CEBU INSTITUTE OF TECHNOLOGY – UNIVERSITY

College of Engineering and Architecture

Chemical Engineering Department

PRODUCTION OF TARTARIC ACID

In partial fulfilment of the course

CHE 522 ● Plant Design

Submitted by:

Baliguat, Christian Yves E.

De La Rosa, Brian Vincent P.
Genares, Mae Bhen N.
Rañada, Roda Gayle
Satura, Kassandra May E.

Submitted to:

Engr. Vera Marie Lanaria

March 2020
 CHAPTER 1
INTRODUCTION
Natural tartaric acid is a white crystalline dicarboxylic acid with a sour taste. It
is naturally found in fruits like grapes and tamarind. It can be manufactured from
natural raw materials but can also be manufactured synthetically. It is formed by
reacting calcium tartrate, sulfuric acid, and water. Tartaric acid has wide range of
uses in the various industries. In food industry, it is used as an acidifier and natural
preservatives for fruit juices, jams, and soft drinks. Aside from that, it can act as an
emulsifier in bread making and as leavening in desserts. In wine-making industry, it
is used to correct acidity of wine. Aside from food, tartaric acid can also be applied in
pharmaceuticals industry for the preparation of specific medicines; and cosmetics
industry as a base compound in body creams. Moreover, tartaric acid also has its
purpose in construction industries. Tartaric acid is used in gypsum and cement
industries as setting retarder or slowing down the setting process in cement.

One of the major factors driving the global tartaric acid market is the growing
construction industry. It is estimated to reach approximately USD 10.3 trillion in
2020. Global tartaric market is expected to grow at a CAGR of around 6% during the
period of 2018 to 2020. Some of the world’s leading economies are from Asia
Pacific (APAC) including Indonesia, China, India, Japan, and Philippines. In addition,
Malaysia and Vietnam are considered as potential emerging markets. In terms of
infrastructure and development, Singapore is one of the growing markets. Moreover,
the demand for tartaric acid is supported by the growing consumption of sports and
protein drinks, as well as the introduction of fruit-flavored beverages. Another driving
factor in the global market is the growth in the overall beverages market. The growth
of wine industries especially in Asia Pacific and South American countries is one of
the factors that contribute to the growth of this market.

Three basis sources were segmented by the market; (1) grapes and sun-dries
raisins, (2) maleic anhydride, and (3) fruits including apricots, tamarind, bananas,
and apple. The grapes and sun-dried raisins segment was accounted for the largest
share in 2016. Most tartaric acid is naturally extracted from grapes and sun-dried
raisins, which is obtained as a by-product of the wine-making processes in crystal
form.
 On the other hand, with the improving research in the Philippines, grape
farming is now rampant in the Philippines. Even with the tropical climate, it is
possible for grapes to grow. In relation to this, wine consumption in the Philippines
expands as restaurants and bars become more popular. The demand for wine
increases so production for wine also increases. With this, the raw material for the
production of tartaric acid which is wine lees also increases.

Figure 1.1 Tartaric Acid Market as expected from year 2015 to 2020 in 4 regions
globally. Retrieved from https://www.marketsandmarkets.com/Market-
Reports/tartaric-acid-market-59894738.html
A patented project authored by Geza Braun pertains to the production of
tartaric acid from calcium tartrate reacted with sulfuric acid. The invented process
consists of 15 unit operations including milling, filtrations, distillation, agitations,
adsorption, centrifugation, crystallization, and drying. In contrast to Braun’s process,
this plant process omits some of the unit processes as they are not necessary.
Braun’s process started with calcium tartrate salts as raw materials which are
dissimilar to this production as wine lees are utilized as raw material.

The main component such as calcium tartrate can be obtained by different

alternative processes and it just so happened that wine lees, a by-product from the
wine industry that contained mainly residual yeast deposits and other substances
after fermentation and aging process, has a large amount of potassium bitartrate that
can be used with concentrated sulfuric acid, another raw material, to convert into a
calcium tartrate to tartaric acid that is on par with Braun’s process in terms of yield.

This plant design offers a variety of benefits with regards to sustainability,

efficiency, cost-effectiveness, reducing environmental impact and simplifying the
burden of unit processes and unit operations without compromising the quality and
quantity of tartaric acid crystals.
 CHAPTER 2
PROCESS OPTION AND SELECTION

Modern industrial plants governing the production of tartaric acid involves

sophisticated and complex combination of unit processes and unit operations in
order to guarantee the quality with quantity of the product. The appropriate process
selection in a tartaric acid plant plays an important role in the acquisition of the
tartaric acid. This process is, as well, practical and yet efficient equipment and
operation to achieve a feasible design. In tartaric acid production, there involves four
main processes that are carried out: dissolution, crystallization, centrifugation and
drying. Each process is further elaborated in the succeeding section of the chapter
regarding the selection of the specific process and equipment.

Different cases of evaluation are taken into account and are described in
terms of equipment and process selection, expected performance and operating
conditions. The selection of the processes and materials is significant to maintain
and ensure the efficiency, cost-effective, high quality standards, work and safety
practices, health - environmental impact and sustainable development. Discussions
on the different options are considered in each major process with determined set of
criteria presented subsequently.

2.1 Equipment Selection and Design

In the selection of the process and specific equipment, different parameters

like capital expenditure, work efficiency, environmental impact, occupational health
and safety, feasibility and sustainability are considered to achieve the desired
specifications of the products and overall objectives of the industrial plant. These
criteria with corresponding description and percentages are show in Table 2.1
Table 2.1 General Criteria for Selection Processes
Criteria Description Percentage

Capital This refers to the mount of possible costs that causes with
Expenditure the use of equipment and operation. This includes fixed
25%
cost, purchase cost, production cost, operating cost,
(CE)
maintenance cost and utility cost.

Health and This refers to the possible adverse effects incurred by the
Environmental development of the industrial equipment or unreasonable
15%
Impact risks and hazards to the health and to the environment.
This includes standardized health protocols, industrial
(HEI)
waste generation and effluent discharge.

Work This refers to the chance to pose risk and injuries towards
Operation and the users upon handling the equipment. This includes
Safety operational work assessment, risk reduction management
and equipment specification safety guidelines. 15%
(WOS)

Feasibility and This refers to the plausible degree of continuity and

Sustainability convenience of the industrial plant. This includes the
longevity of the equipment used in the production with
(FS)
ease of control throughout the functional operating time. 10%

Plant Work This refers to the expected performance of the equipment

Efficiency in which it doesn’t compromise the overall quality of the
35%
final product. This includes time and effort reduction.
(PWE)

2.2 Modes of Operation

The processing of tartaric acid anhydrous crystals can be done by batch or

continuous process. Using each processes has its own advantages and
disadvantages and it depends on the scale of production and what kind of product to
be processed.

Both batch and continuous processes are vital in the production of materials
or products.
Table 2.2 General Criteria for Modes of Operation
Criteria BATCH PROCESS CONTINUOUS PROCESS

Quantity Ideal for production of small Ideal for large quantity and scale
Production quantities of specific materials production of specific materials
are planned and produced. are planned and produced.
(30 %)
(25 %) (20 %)

Operational Ideal for the same equipment Ideal to be established but

Flexibility to be utilized for multiple sometimes lead to inefficient use
industrial operations. (10 %) of capital. (5 %)
(15 %)

Variety of Ideal when the industrial plant Ideal when the industrial plant
Product and produces a wide variety of produces a centralized and
Diversity materials and the product can permanent product of the same
be subjected to change every reactor. (5 %)
(5 %)
now and then while using the
same reactor. (0 %)

Controllability Ideal when complicated yet Ideal and easier to control and
and Stability proper scheduling to control stabilize for the same equipment
the manufacture of different is used for the same unit
(15 %)
products as same equipment is operation in manufacturing the
used for different unit product thus reducing operational
operations. (10 %) burden. (10 %)

Product Ideal when the process is Ideal after the finalization of all the
Development relatively new and stages of overall calculation
Stage revolutionary. In its preliminary revenues, costs and economic
stage, the case for initial feasibility tests.
(15 %)
investment is in a smaller scale
(10 %)
of batch reactor and the
economic risk is also smaller.

(10 %)
Criteria BATCH PROCESS CONTINUOUS PROCESS

Maintenance Ideal if the operating labor cost Ideal if the operating labor cost is
and Labor is higher due to equipment lower due to the continuous
Operation maintenance at higher process of the same product
frequency due to different being manufactured. This reduces
(20 %)
products manufactured. This the amount of time and effort for
includes production start-ups, equipment maintenance, reducing
production end-runs, cleaning its frequency.
and preparation time.
(10 %)
(15 %)

TOTAL: 70 % 60 %

The production of tartaric acid crystals from wine lees has a simple process
and the feedstock availability is regular. Since the raw materials are regular, the
scale of its production can range from small to large. Patented feasibility, although
few such as Braun’s industrial study and process of tartaric acid, studies have shown
an appropriate amount of data that solidifies its product development. The amount of
operational flexibility is crucial in the production. Moreover, huge manpower is
required to do the whole operation from maintenance to start-ups and end-runs of
the production. Thus, Batch process is utilized.

2.3 General Processes

In the production of the tartaric acid crystals, different methodologies have

various impacts on the quality of crystals produced. The required technology
refinement vastly depends on the method for production used, the amount and rate
of conversion of raw materials to final product and the efficiency and sustainability of
the equipment and methods that varies from industrial plant to industrial plant. With
that being said, an immense classification and selection is considered and executed
to reach the most economical and feasible option.

The selection on the process and/or equipment is used for the agitator,
screening, crystallizer, centrifuge and drying is hereby conducted.
2.3.1. Batch Reactor

Batch reactors are enclosed vessel where chemical reaction takes place in a
fixed volume to ensure high conversion towards desired product output and
producing highest yield while requiring the least amount of money to purchase and
operate. The batch reactor is crucial in the conversion of the wine lees and other raw
materials into the final product. Types of batch reactors are considered in attaining
the desired amount to carry out the particular chemical reaction are shown and
compared below.

Table 2.3.1.1 Comparison of Batch Reactors

Batch Reactors per Semi Batch Reactor Stirred BatchReactor
Criterion

Capital Expenditure (+10%) Considerable cost (+10%) Simple

for the equipment construction and
25%
construction. fabrication costs.

(+15%) Low installation (+15%) Requires no

cost of semi-batch reactor. auxiliary or specific
equipment for installation.

(-3%) Requires high labor (-3%) Requires high labor

costs per unit product. costs per unit product.

(-3%) Operating cost may (-9%) High operating cost.

be relatively high.

(-6%) Installation of may

require specific piping and
valves.

Health and Environmental (+15%) Secured reactor (+15%) Secured reactor

Impact that allows no chemical to that allows no chemical to
cause adverse effects cause adverse effects
15%
during and after operation. during and after operation.
 Batch Reactors per Semi Batch Reactor Stirred Batch Reactor
Criterion

(-6%) High exothermal (-3%) Industrial risk and

reaction risks are further health hazard is observed
observed especially every for every batch reaction.
after increment of
materials to the reactor

Work Operations and (+10%) Promotes flexibility (+10%) Promotes flexible

on complicated operation. operation.
Safety
(+5%) Intrinsically permits (+5%) Easy to conduct an
15%
stable and safer operation equipment maintenance.
than normal batch
operation.

(-6%) Specific reactor (-6%) Operation is affected

operations can be difficult due to down time
to analyze. maintenance like emptying
and filling delays.

Feasibility and (+5%) Can additionally (+10%) Data is easily

Sustainability simulate continuous collected if under
production for small scale. isothermal reactions are
10%
carried under constant
volume condition.

(-6%) Semi- batch reactors (-3%) Large area and

not used often as other dedicated facilities are
reactors. needed.

(-3%) Design is
complicated because of
small increment of
reactant or removing of
product during operation.
 Batch Reactors per Semi Batch Reactor Stirred Batch Reactor
Criterion

Plant Work Efficiency (+15%) Unwanted side- (+25%) Generally has high
reactions are minimized. yield and product
35%
conversion per unit
(+10%) Promotes high
volume.
conversion.
(+10%) Product can be
(+10%) Good temperature
easily traced.
and pressure control
equipment.

%) Large scale production (-3%) Large scale

difficult to achieve production difficult to
(Preferably pilot scale). achieve.

(-3%) Variable quality of (-6%) Long idle time

the product is observed. (charging and discharging)
leads to period of no
(-3%) The production rate
production.
may be limited due to the
cyclic nature of the
operation.

TOTAL: 55% 70%

It can be seen from the Table 2.3.1.1 that the stirred batch reactor is superior
when it comes down to the different criteria for process selection. This batch reactor
is not only efficient for working food grade and medium scale production like tartaric
acid crystals but also cost effective when it boils down to fabrication costs, operation
costs and maintenance costs.

2.3.1.a Agitators

After the selection of batch reactors, different agitators are presented that is
appropriate for the reaction in the batch reactor to get the desired amount and quality
of the product. Axial flow impellers are recommended for utilizing chemical reactions,
suspension solid and miscible liquid mixing. But the type of axial flow agitators to be
used is placed into process selection criteria. The following agitators are taken into
consideration.

Table 2.3.1.a Comparison of Agitators

Axial-Flow Agitators per Hydrofoil Impeller Pitched Turbine Impeller
Criterion

Capital Expenditure (+25%) Low Maintenance (+15%) Low Maintenance

Costs Costs
25%
(+10%)Simple installation
costs

(-3%)Relatively High (-3%) Relatively High

Purchase Cost Purchase Cost

(-6%) Power consumption

cost is high

Health and Environmental (+15%) No unwanted (+15%) No unwanted

Impact waste generated waste generated

15% (0%) Considerably (0%) Considerably

Negligible Negligible

Work Operations and (+10%) Works for slow (+10%) Can operate at
operation and dissolution high axial flow
Safety
(+5%) Relatively have high (+5%) Excellent for
15%
shear properties. dispersion operations

(-3%) Sensitive in (-6%) Not Preferred with

operation. solvents of relatively high
viscosity

(-3%) Sensitive in
operation.
Axial-Flow Agitators per Hydrofoil Impeller Pitched Turbine Impeller
Criterion

Feasibility and (+5%) Low Space (+10%) Very large flow

Sustainability Requirement inside the rate is required
reactor
10%
(+5%) High Throughput

and no vortex formation

(-3%) Sensitive to use in (-3%) Sensitive to use in

the operation as the operation as
maintenance is necessary maintenance is necessary

Plant Work Efficiency (+10%) Low Power (+15%) High efficiency

Requirement
35% (+10%) Greater shearing
(+10%) High suspension forces than other impellers
mixing efficiency
(+10%) Provides excellent
(+15%) Heavy Duty circulation of the fluid in
Performance. the vessel.

(-3%) High Power (-3%) High Power

Requirement. Requirement.

TOTAL: 88% 76%

Based on Table 2.3.1.a above, it showed that hydrofoil impeller is superior to

the process selection for impeller suited in the batch reactor for the production of
tartaric acid. It showed that hydrofoil impeller works well with chemical processes
and reaction such as dissolution of materials.

After choosing the equipment, the next process involves the utilization to
decolorize the solution through the process of adsorption. Choosing adsorption with
different adsorbents as method has different criteria in order to achieve the desirable
results of the production of tartaric acid crystals.
 2.3.2 Adsorption

For the efficiency and compatibility of the food grade production, the selection
of different batch adsorption is utilized. Ignoring this process allows to produce the
product with distinct characteristic and standard in the market. To have an optimum
performance, it was speculated that Multi-Layered Filter (MLF) and Fluidized Bed
(FB) gave the majority of positive response but the specifications for the production
of tartaric acid is shown below.

Table 2.3.2.1 Comparison of Adsorbers

Adosrption per Criterion Multi-Layered Filters Fluidized Bed System
System

Capital Expenditure (+10%) Low purchase cost (+10%) Economical due to

25% (+15%) Economical due to
its promising performance
and efficiency with respect
to usage.
its recycle system.
(+5%) Specific design with
appropriate adsorbent can
pose cost-effectiveness.

(+10%) Energy
consumption and
consumer costs are
effectively reduced.

(-6%) High operation costs (-6%) High operation

costs
(-3%) High maintenance
cost. (-3%) High maintenance
costs.
(-3%) High Installation
costs

Health and Environmental (+15%) Different (+10%) Adsorbs

Impact adsorbents can be used
and installed in the filter
15%
that can’t pose harm to
health and environment.
hazardous and toxic
substances that can pose
harm to the environment.
Adosrption per Criterion Multi-Layered Filters Fluidized Bed System
System

(+5%) Uses small amounts

of adsorbents in fluidized
system.

(-6%) Materials used in (-3%) Escape particles are

manufacturing this system likely to be noticed if not
can pose environmental operated properly.
problems if not handled
properly.

Work Operations and (+10%) Can be modified (+10%) Provides with a

with cationic polymer or single deposit for the
Safety
anionic polymer. fluidized liquid.
15%
(+5%) Work operations (+5%) It is much easier to
blends well with manage compared to
membrane separations. other adsorbers.

(-3%) It has specific (-6%) Due to optimization

criteria to follow such as fo recycling, monitored
controlled modes of regeneration is taken into
constant pressure and flow account.
rate.

Feasibility and (+5%) Contains depth (+5%) Commonly used for

Sustainability filters that are composed purification and treatment
of cellulose and inorganic of industrial production.
10%
adsorbents.
(+5%) Designed to prevent
(+5%) Porous filtering losses of adsorbent.
mediums perfect for
adsorption.

(-3%) It has intricate and (-3%) Incomplete

complicated design layers. fluidization of the
Adosrption per Criterion Multi-Layered Filters Fluidized Bed System
System

(-6%) Lack of experimental adsorbent can happen.

studies.

Plant Work Efficiency (+15%) Works better than (+20%) Integrated

surface adsorption. technology that combines
35%
clarification, concentration
(+20%) High selective
and purification in single
adsorption.
step.

(+15%) Increased
adsorbent capacity.

(-6%) Filter fouling or (-6%) Suspended solid

clogging must be clogging can affect the
assessed with adsorption efficiency.
consistency.
(-3%) Incomplete
. fluidization of the
adsorbent can weaken
efficiency.

TOTAL: 64% 70%

It is observed that the fluidized bed adsorber pose a promising result upon
carefully observed on different equipment selection criteria in terms of capital
expenditure, work operations and safety, plant work efficiency, feasibility and
sustainability.

After carefully selecting the equipment design, the specific adsorbent is yet to
be considered. This adsorbent design must coincide well with the type of adsorbent
being utilized.
2.3.2.a Adsorbents

In this part of the adsorption design selection, the most important part of
determining the adsorber’s, capacity, efficiency and selectivity is the type and
amount of adsorbents used. In most food production industry, adsorbents are used
to remove different physical parameters such as odor, taste and color. Failure to
remove this causes the tartaric acid product to produce a purple shade of color with
a peculiar wine alcoholic smell of the tartaric acid crystals.

The Table 2.3.2.a shows two of the most promising adsorbents, the activated
carbon and resin that can be classified into the selected criteria.

Table 2.3.2.a Comparison of Adsorbents

Adsorbers per Criterion Activated Carbon Polymer Resin

Capital Expenditure (+10%) Low purchase (+15%) Not exothermic, no

costs catalytic reaction that
25%
causes spontaneous
(+5%) Economical
combustion that destroys
operation costs.
the bed overtime.
(+10%) One of the least
(+10%) High return of
expensive adsorbents
investment index.
used in the industry.

(-3%) Relatively high (-6%) Relatively High

operating costs. operation costs.

(-6%) Increased expenses (-3%) Mandatory royalty

for regenerative or expenses and
treatment costs. regeneration costs.

Health and Environmental (+15%) Natural adsorber (+10%) Used to adsorb

Impact made from wood and harmful substances in food
coconut shells. industry.
15%
Adsorbers per Criterion Activated Carbon Polymer Resin

(+5%) Interference of
aldehydes, ketone, esters
and sugars of certain
amount in different
products for quality control
standards.

(-3%) Can harbor (-3%) It can cause

pathogens which can lead secondary pollution if not
to microbial growth inside taken care appropriately.
the media.
(-6%) Some adsorbent
resins lack medicinal and
technological quality
control standards in resin
materials, therefore
hazardous.

Work Operations and (+5%) Simple and natural (+10%) Chemical and
adsorption and filtration physical adsorbent resins
Safety
process. characteristics can be
15% controlled artificially.
(+5%) Simple and robust
technology. (+5%) Long service life

(+5%) Easy and

convenient to maintain.

(-6%) Short service life, (-3%) A synthetic material

needs to be replaced which needs care as its
when filled with component isn’t easily
contaminants easily. removed when having
maintenance.
Adsorbers per Criterion Activated Carbon Polymer Resin

Feasibility and (+5%) Suitable for (+5%) High adsorbility

Sustainability discontinuous or batch because of strong van der
processes. Waals forces and
10%
hydrogen bonds.
(+5%) Good contaminant
removal capacity. (+5%) Great screening
properties.

(-9%) Adsorption process (-6%) Has weak rigidity

is exothermic, too much thus easy to break.
local heating destroys the
adsorbent layer.

Plant Work Efficiency (+25%) High adsorbing (+15%) High adsorption

efficiency. selectivity for organic and
35%
inorganic compounds.
(+10%) Right
concentrations enable to (+20%) Used repeatedly
effectively deal with and regenerated without
contaminants like volatile compromising the quality
organic compounds of the adsorbent.
(VOC).

(-6%) Not good at (-3%) Lower loading

removing chemicals that capacity.
are not attracted to
(-6%) Specific resins
carbon, including metals,
require a corresponding
anions, cations and heavy
regenerative medium.
metals.

(-3%) Effectiveness can be

determined by amount of
activated carbon and its
residence time.
 Adsorbers per Criterion Activated Carbon Polymer Resin

(-6%) Not effective with

pathogenic bacteria and
viruses.

TOTAL: 58% 64%

It can be concluded that from the Table 2.3.2.a the adsorbent used would be
the polymer resins. Given the different criteria as equipment and process selection,
the resins pose a positive advantage especially its high regenerative and adsorbent
properties when coupled with fluidized bed adsorber system.

2.3.3 Filtration

After successful reaction on the dissolution of wine lees with sulfuric acid and
water of the needed tartaric acid crystals in the process, all the other ingredients
subjected to this process to separate the slurry-containing used resins, suspended
particles and remaining substances of wine lees that are not yet converted from the
filtrate containing impure tartaric acid solution. The special type of filtration such as
separation membranes needed are presented and compared below.

Table 2.3.3 Comparison of Filter Equipment

Filters per Criterion Horizontal Pressure Shell Plate-and-Frame Press
and Leaf Filter

Capital Expenditure (+15%) Low labor charges (+10%) Low capital cost

25% (+10%) Low initial cost (+15%) Low operation

costs

(-3%) Operating costs may be (-3%) High labor

high due to controlled maintenance costs
operations
 Filters per Criterion Horizontal Pressure Shell Plate-and-Frame Press
and Leaf Filter

Health and (+10%) Filter medium does (+5%) No unwanted waste

Environmental Impact not require frequent change generated.
thus less waste.
15% (+10%) Low power and
(+5%) No spillage due to close energy consumption.
and compact operations.

(0%) Considerably negligible (-3%) Exposure to cake

filters can cause health risk
and hazards.

Work Operations and (+10%) Simple design can (+5%) Filter presses are
have easy cleaning of filter easily cleaned.
Safety
cake.
(+5%) Filter medium is
15%
(+5%) The equipment is user easily replaced.
friendly.
(+5%) Most operations are
automated.

(-6%) Needs strict and (-3%) Imperfect washing

intelligent supervision. due to cake density.

(-3%) Physical hazards may (-3%) Housekeeping

be observed when operations problems.
are going on.

Feasibility and (+5%) Adaptable to (+5%) Floor-space and

Sustainability displacement washing. headroom needs per unit of
filter area is small
10% (+5%) Filtered cloth is
optional. (+5%) Can easily be
modified and adjusted.

(+5%) Rapid
disassembling as well as
 Filters per Criterion Horizontal Pressure Shell Plate-and-Frame Press
and Leaf Filter

reusing of filter medium is

possible

(-6%) Restriction of operating (-6%) Filter cloth have

pressure. short service life.

(-3%) Not suitable for high

throughput.

Plant Work Efficiency (+20%) High productivity due
to high filtration rate.
35%
(+15%) Uniform production of
the product.
(+20%) Ability to operate at
high pressure
(+15%) High percent solid
capture.

(-3%) Inability to produce dry (-3%) Plant presses leak

cake. and drip easily.

TOTAL: 79% 76%

From Table 2.3.3, the horizontal pressure leaf filter is the best option between
the two options. Although it needs strict supervision, it is also considerably flexible as
it permits maximum and various thicknesses of cake filters. It has low labor costs
because the cake can be cleaned by blowback. The simplicity of its design makes it
adaptable and easy for displacement washing.

2.3.4 Crystallizer

Crystallizers are unit operations used in the industry to achieve liquid-solid

separation. Food industries such as manufacturing of tartaric acid utilize this
purification technique because it’s capable of generating high purity products with a
 relatively low energy input. Crystallizers that are prominently used in the industry are
Draft Tube Baffle (DTB) Crystallizers and Batch Vacuum Cooling (BVC)
Crystallizers. Their specialization and utilities are showcased with the table below.
Table 2.3.4 Comparison of Crystallizers
Crystallizer per Criterion Draft Tube Baffle
Capital Expenditure (+15%) Economical due to
recyclability of fines
25%
(+10%) Lower operating
costs.
(-6%) Baffle Installation
Cost
(-3%) Increased labor cost
(-3%) Maintenance cost
greatly increased.
Health and Environmental (+10%) Minimum space
Impact requirement with single
support elevation
15%
(+5%) Adaptable to most
corrosion resistant
materials of construction.
(0%) Considerably
Negligible
Work Operations and (+10%) Simplicity of
operation such as start-
Safety
ups and shutdowns.
15%
Batch Vacuum Cooling
(+15%) Least expensive
type of crystallizer
(+10%) Simple Installation
Cost
(-3%) Increased labor cost
(-3%) Maintenance cost
greatly increased.
(+10%) Minimum space
requirement for batch
crystallizer.
(+5%) Volatile materials
are kept tightly inside to
secure batch integrity.
(0%) Considerably
Negligible
(+15%) Generates
supersaturated solution
when very low
temperatures are needed.
Crystallizer per Criterion Draft Tube Baffle Batch Vacuum Cooling

(+5%) Can be easily

instrument controlled.

(-3%) Frequent flushing of (-6%) Crystal size is

the equipment to minimize difficult to control.
the crystallizer wall.

Feasibility and (+5%) Baffles allow slurry (+10%) Ranges of sizes

Sustainability density control in the baffle are available.
zone.
10%
(+5%) Baffles permit
separation of unwanted
fine crystals from the
suspension of growing
crystals, thereby affecting
control of product size.

(-3%) Can’t handle (-6%) First cooling and

effectively high density seeding must be at a very
slurry slow rate.

Plant Work Efficiency (+15%) More efficient than (+25%) High rate of
most forced circulation circulation reduces particle
35%
crystallizers deposits on vessel wall.

(+10%) Capable of (+10%) Optimal for

producing large singular controlled crystal sizing.
crystals.

(+10%) Produces narrow

crystal size distribution for
easier drying and less
caking.
Crystallizer per Criterion Draft Tube Baffle Batch Vacuum Cooling

(-3%) Auxiliary equipment (-9%) Simple installation

are also purchased and leads to poor quality.
installed to increase its
efficiency.

TOTAL: 79% 73%

It is clearly shown at Table 2.3.4 that the different criteria for the production of
tartaric acid crystals gives more positive response to Draft Tube Baffle (DTB)
Crystallizer than Batch Vacuum Cooling (BVC) Crystallizer. The DTB showed a
promising characteristics and quality output when it comes to crystal size control and
equipment efficiency despite its considerable economical costs.

2.3.5 Centrifuge Equipment

The impure tartaric acid solution together with the formed crystals from the
crystallizer is fed to the centrifuge for further separation if liquid and solids. The
separated solids (tartaric acid crystals) will be collected. The mother liquor contains
polyphenolic compounds. The use of the centrifugal filter is chosen since it is more
compact than the centrifugal sedimentation since the solids in the sedimentation are
not normally deposited or settled out. Two centrifugal equipment are compared and
shown in Table 2.3.5

Table 2.3.5 Comparison of Centrifuge Equipment

Centrifuge per Criterion Vertical Basket Horizontal Peeler
Centrifuge Centrifuge

Capital Expenditure (+15%) Less expensive (+15%) Less labor cost

compared among the
25% (+15%) Relatively high
centrifuge equipment.
return of investment index.
(+15%) Economical due to
no crystal breakage.
Centrifuge per Criterion Vertical Basket Horizontal Peeler
Centrifuge Centrifuge

(-3%) High labor cost (-6%) High capital costs.

(-6%) Additional (-3%) High maintenance

installation costs. costs.

Health and Environmental (+5%) Explosion-proof (5%)Explosion-proof

Impact equipment. equipment.

15% (+10%) Installments such (+10%) Intricate system

as pressurized pneumatic and equipment installed.
shaft seal and cake
detection device.

(-6%) Depending on cake (-6%) High power

discharge can pose consumption.
unreasonable risk to
health or environment.

Work Operations and (+5%) Can be easily (+5%) Filter cloth

controlled with sensors exchange does not require
Safety
and probes. entry
15%
(+10%) Simple and robust (+5%) Can be manual or
technological design. automated.

(+5%) Long maintenance

free and smooth
operational life.

(-9%) Labor intensive on (-3%) Damaged by

operation. abrasion can happen as
sharp peeler isn’t kept
away from innermost
surface of separation.
Centrifuge per Criterion Vertical Basket
Centrifuge
Feasibility and (+5%) Can be manual or
Sustainability automated.
10% (+5%) Functions further as
clarifier.
(-3%) Requires larger
space for construction.
Plant Work Efficiency (+15%) Conventional
design
35%
(+20%) Employs gravity
and feed controlled
through distribution funnel
for optimization.
(-6%) Uneven filtration
resistance, affecting wash
pattern and efficiency of
the wash.
(-6%) Works well with
small batches of
production.
TOTAL: 61%
From Table 2.3.5, the horizontal peeler centrifuge is the best option among
the equipment. The higher capital cost of the horizontal peeler centrifuge is offset by
the numerous process and mechanical advantages it has over vertical centrifuge
Horizontal Peeler
Centrifuge
(+5%) Designed to have
high throughput.
(+5%) Suitable also for
low concentration slurries.
(-3%) Relative requires
large space.
(+10%) High output duties
where strong crystalline
materials are recovered.
(+10%) Less dead cycle
time
(+15%) Provides higher
rotation speed means
higher centrifugal force.
(-6%) Layer of solid cake
forms on the wall that
serves as extra separation
step.
(-3%) Filtration time is
increment with solid layer.
70%
basket. The peeler centrifuge can provide higher centrifugal forces than can vertical
baskets for increased performance and flexibility. Its ability to discharge at high
speed eliminates or at least minimizes the dead cycle time for higher capacity, lower
power consumption, and lower wear and tear. Moreover, it distributes the solids
more evenly compared to vertical basket centrifuge.

2.3.6. Dryers

There are several varieties of techniques when it comes to solids drying.

Adjustment and moisture level control in solid materials are critical process in
manufacturing especially in food industry. Dryers are practically used in every
chemical process industries. In production of tartaric acid crystals, the selections for
dryers are selected with regards to the different criteria shown below.

Table 2.3.6 Comparison of Dryers

Dryers per Criterion Vacuum Tray Dryers Vacuum Freeze Dryer

Capital Expenditure (+10%) Considerably (+15%) Relatively low

affordable among the installation costs.
25%
dryers.
(+10%) Low maintenance
(+10%) Low installation costs.
costs.

(+5%) Low maintenance

costs.

(-3%) High operating costs (-6%) High purchase costs

(-6%) High labor costs. (-6%) High operation

costs.

Health and Environmental (+10%) Enclosed (+5%) No additives are

Impact equipment so that noise
produced is minimized.
15%
(+5%) Significant energy
savings.
added on the food.
(+10%) Nutrients and
flavors are retained when
freeze dried.
 Dryers per Criterion Vacuum Tray Dryers Vacuum Freeze Dryer

(-3%) Volatile organic (-3%) Cryoprotectants are

compounds can be carried required.
out by the exit air.
(-6%) Energy consuming
(-3%) Unsterilized air can drying process.
bring possible particles
and pathogens.

Work Operations and (+10%) Limited amount of (+15%) Packaging

control makes it user- requires specifications like
Safety
friendly. condition and attention.
15%
(+5%) Manual loading and
unloading is
advantageous.

(-3%) Develops electric (-3%) Complex process is

charges observed in the dryer.

(-3%) Mechanical attritions (-3%) Skilled operator is

may occur. required.

Feasibility and (+10%) Suitable for food (+10%) Texture of the

Sustainability and pharmaceutical product is well-maintained;
production. no shrinkage and case
10%
hardening.

(-3%) Lacks great (-6%) Dehydration process

controlling methods. is a lot common compared
to freeze dryers.

Plant Work Efficiency (+20%) High drying and (+15%) Removal of

thermal efficiency. moisture content is high.
35%
(+15%) Prevents (+10%) Product has long
significant material losses shelf life.
 Dryers per Criterion Vacuum Tray Dryers Vacuum Freeze Dryer

(+10%) High and rapid

drying efficiency.

(-3%) Useful when (-3%) Air tight and

production is relatively moisture control is
small and has long drying necessary to ensure
time. quality.

TOTAL: 73% 61%

From the Table 2.3.6, it can be shown that batch tray dryer has numerous
advantages when it comes to drying food grade products despite its limitations found
on the mentioned criteria. The simplicity and user-friendly of the equipment allows
the process to proceed to smooth operation and less trouble shoot of technical
problems. Moreover, this also gives efficient and purposeful result when drying.
 CHAPTER 3
BASIS OF DESIGN

3.1 Purpose

Tartaric acid is an important food additive that is commonly combined with

baking soda to function as a leavening agent in recipes. It can be used in all kinds of
foods except untreated foods. It is popularly used to enhance the quality of the food,
at the same time helps preserve it. Significant growth in demand of Tartaric Acid is
expected as the increasing demand for processed food and ready-to-drink
beverages, making the production of Tartaric acid contribute economic benefits to
the residents, in the form of employment and community support.

This design aims to provide a safe, energy and cost-effective process by

selecting the most appropriate and practical process operations, equipment and
materials along with a definite project evaluation. Moreover, the proposed plant is
also designed with minimum environmental impact.

3.2Conceptual Process Design

3.2.1 Design Description

Several unit operations are involved in processing tartaric acid. The design uses
batch type process as the overall mode of the production. The process involve are
dissolution and agitation, adsorption, screening, crystallization, centrifugation,drying
and packaging.

3.2.2 Process Concept

Dissolution and Agitation. The wine lees are subjected to agitation and dissolution
with sulfuric acid

Screening. This separates the slurry, suspended particles and remaining

substances of wine lees from the filtrate containing impure tartaric acid solution.

Crystallization. Impure tartaric solution will be then crystallized

Drying. Tartaric acid concentrates will be then subjected to drying.

Packaging.This is the last step to produce tartaric acid from wine lees. After drying
the tartaric crystals, it will proceed into packaging.

Figure 3.2.2 Process Scheme for Production of Tartaric Acid from Wine Lees
3.3 Basic Assumptions

3.3.1 Plant Capacity

The plant produces tartaric acid as the main product and the targeted plant will
produce 30,303 kg of tartaric acidper day. The previous capacity coincides with the
production capacity of most of the tartaric acid producing plants across the world.

Figure 3.3.1.1 Satellite View of the Plant Site (Google Map)

This proposed plant is located at Barangay Sangat, Carcar City, Cebu.This

location is chosen according to the following factors and specifications: topography,
climate, utilities and accessibility. It is equipped with enough utilities such as water
and electricity to maintain the operations that take place in the plant, and the Cebu
Straight is situated behind the plant for the treated wastewater discharge. In addition,
the plant has a neighboring shipyard and directly on the highway road. The total lot
area covers 10,000 square meters with an estimated cost value of 500 pesos per
square meter, which when purchased, will have a total calculated price of 5,000,000
pesos. Figures shown below are the site and floor plans of the plant.
Figure 3.3.1.2 Site Plan of the Plant
 Figure 3.3.1.3 Floor Plan of the Plant

3.4 Battery Limits

This plant aims to produce tartaric acid from wine lees. The activities involved in
the transformation and production of this product is determined, regardless of
whether or not it is involved inside or outside the plant and its operation. The
selection of which process activity is built within the plant depends exclusively on the
extent to which the system designers can reach and what they cannot reach. Table
3.4.1 below presents the scope and limitations of the entire project.
Table 3.4.1 Battery Limits of the Design Project
Inside Battery Limit
 Perform overall material balances
around the process and material
balance on each equipment.
 Calculate overall energy balance
over the production of tartaric
acid.
 Develop the following:
 Process flow sheet
 Final process block flow
diagram
 Material and energy
processes stream
summaries of the design
project.
 Chemical engineering
design of the operation
involved in the production
of tartaric acid from wine
lees.
 Carry out mechanical design of
the operations involved in the
production of tartaric acid from
wine lees.
 Provide equipment specifications
and supports of the operations in
the production of tartaric acid from
wine lees.
 Prepare a list of materials of
construction and present the
selection process.
Outside Battery Limit
 Develop chemical engineering
design of the upstream processes
i.e. raw material storage and
treatment process.
 Prepare specification sheet for the
remaining upstream processes
 Develop a plan for product
packaging.
 Plan a waste treatment
management process for the
generated waste.
 Specifications of the following:
 Electrical system used to
run the design equipment.
 Recovery units
 Design of quality control
laboratories, process control
centers, etc.
 Transportation and delivery of
products
 Inside Battery Limit Outside Battery Limit

 Specify the following:

 Safety features of the
design equipment for the
production of tartaric acid
from wine lees.
 Process control and
instrumentation of the
design equipment in the
production.
 Prepare the final equipment
specification sheet for design
equipment.
Carry out economic analysis on
the costing categories and
determine economic criteria.

3.5 Economic Margin

୔୰୭ୢ୳ୡ୲ୗୟ୪ୣିେ୭ୱ୲୭୤ୖୟ୵ ୑ ୟ୲ୣ୰୧ୟ୪ୱ
%Margin= x100%
୔୰୭ୢ୳ୡ୲ୗୟ୪ୣୱ

Table 3.5.1 Input variables with their respective quantity and price
Feed Quantity Price Total Amount
(Php)

Wine lees 21,901.52 kg/day Php 7.60/kg Php

166,451.55/day

Sulfuric acid 14,601.01 kg/day Php 20.32/kg Php

solution 296,692.52/day

Calcium hydroxide 3000 kg/day Php 12.7/kg Php 38,100/day

Total cost of Feedstock: Php

501,244.07/day
Table 3.5.2 Output variables with their respective quantity and price
Feed Quantity Price Total Amount
(Php)

Tartaric acid 30,303.03 kg/day Php 475/kg Php

(anhydrous) 14,393,939.25/day
Potassium 3000 kg/day Php 101.6/kg Php 304,800/day
hydroxide
Polyphenolic 10,000 kg/day Php 10/kg Php 100,000/day
compunds
Total income from Sales: Php
14,798,739.25/day
*Prices are from alibaba.com and some of it is converted to Philippine Peso.

୔୰୭ୢ୳ୡ୲ୗୟ୪ୣିେ୭ୱ୲୭୤ୖୟ୵ ୑ ୟ୲ୣ୰୧ୟ୪ୱ
%Margin= x100%
୔୰୭ୢ୳ୡ୲ୗୟ୪ୣୱ

14,798,739.25 − 501,224.07
= x100
14,798,739.25
= 96.61%
 CHAPTER 4
THERMODYNAMIC PROPERTIES

In the proposed plant, the thermodynamic and physical properties of wine lees,
which has the components of tartaric acid, and yeast, sulfuric acid, and water that
was used the production of the product are presented in this chapter. The
thermodynamic properties of saturated liquid water at various temperatures are also
present in this chapter.

4.1 Thermophysical Properties of Wine Lees

Lees are composed mainly of yeasts, tartaric acid, polysaccharides,

and protein-tannin complexes. Lees contribute to colloidal macromolecules in wine
which are derived from three general sources, polysaccharides, glucans and
mannoproteins. Mannoproteins are proteins with a high carbohydrate content
including mannose sugars, hence the term.

4.1.1 Thermophysical Properties of Yeast

Yeasts are eukaryotic single-celled microorganisms classified as

members of the fungus kingdom. The first yeast originated hundreds of millions of
years ago, and 1,500 species are currently identified. They are estimated to
constitute 1% of all described fungal species. Yeasts are unicellular organisms that
evolved from multicellular ancestors, with some species having the ability to develop
multicellular characteristics by forming strings of connected budding cells known as
pseudohyphae or false hyphae.

Yeast sizes vary greatly, depending on species and environment, typically

measuring 3–4 µm in diameter, although some yeasts can grow to 40 µm in size.
Most yeasts reproduce asexually by mitosis, and many do so by the asymmetric
division process known as budding
 Table 4.1.1 Physical Properties of Yeast

Property Yeast

Aspect Pellets/Powder

Moisture Content (%) 12

Viscosity 50 (1.5% Solution at 75C)

pH 9.5 (1.5% Solution at 60C)

Water Gel Strength 700

Color Beige

Mesh >90% Pass 150 Mesh

4.1.2 Thermophysical Properties of Tartaric Acid

Tartaric acid is an important carboxylic acid, which is also called as

dihydroxybutanedioic acid. The chemical formula of tartaric acid can be written as
HO2C-CH(OH)-CH(OH)-CO2H or (CH(OH)COOH)2. It is a dihydroxy (having two OH
groups) and dicarboxylic (having two COOH groups) acid.

Tartaric acid is a muscle toxin, which works by inhibiting the production of

malic acid, and in high doses causes paralysis and death. The minimum recorded
fatal dose for a human is about 12 grams. In spite of that, it is included in many
foods, especially sour-tasting sweets. Tartaric acid plays an important role
chemically, lowering the pH of fermenting "must" to a level where many undesirable
spoilage bacteria cannot live, and acting as a preservative after fermentation.
 Table 4.1.2 Properties of Tartaric Acid

Property Value/Unit

Acidity 3.22

Appearance White Powder

Boiling Point 399.3°C

CAS Number 526-83-0

ChEBI 15674

Density 1.79 g/mL

Acidity 3.22

Melting Point 146-148 °C

Molar Mass 150.08 g/mol

4.1.3 Thermophysical Properties of Protein-Tannin

Tannins (or tannoids) are a class of astringent, polyphenolic biomolecules that

bind to and precipitate proteins and various other organic compounds including
amino acids and alkaloids.

Tannins are defined as water-soluble phenolic compounds with molecular

weights ranging from 500 to 3000 that have the property of combining with proteins,
cellulose, gelatin, and pectin to form an insoluble complex. Tannins are an important
group of secondary plant metabolites that were originally used in the leather
production industry in the tanning of animal hides. The varied chemical structures
and stability evidenced among the tannin group result in their classification as
hydrolyzable, complex, and proanthocyanidins.
 Table 4.1.3 Properties of Protein-Tannin
Property Value/Unit

Molecular Formula C76H52O46

Color Light Yellow to Tan Solid

Boiling Point 399.3°C

Flash Point 197 °C

Solubility 1g dissolves in 0.35ml water

Density 1.2 g/mL

Odor Faint odor

Melting Point 200 °C

Molar Mass 1701.2 g/mol

4.2 Thermophysical Properties of Sulfuric Acid

Sulfuric acid is one of the most important mineral acids with a wide range of
applications. The chemical formula of sulfuric acid is H2SO4 and its molecular
weight is 98.079 g/mol. Its chemical structure is shown below. The sulfur atom is
bound to two oxygen atoms through double bonds, and two hydroxyl groups (OH)
through single bonds. It is a diprotic acid, as it can release two protons.

Sulfuric acid is formed naturally by oxidation of sulfide minerals in rocks.

Dilute sulfuric acid is also formed in the atmosphere by oxidation of sulfur dioxide
(from burning of fuels) in the presence of moisture, eventually precipitating as 'acid
rain'.
Table 4.2 Properties of Sulfuric Acid

Property Value/Unit

Molecular Formula H2SO4

Color Colorless

Boiling Point 337°C

Flash Point 197 °C

Solubility Miscible in water

Density 1.84 g/mL

Odor Pungent

Melting Point 10.36 °C

Molar Mass 98.079 g/mol

Heat of Formation -909.3 kJ/mol at 25 °C

Gibbs Energy of Formation -744.5 kJ/mol at 25°C

Heat Capacity -293.0 J/mol-K at 25 °C

Entropy 20.1 J/mol-K at 25°C

Henry’s Law Constant 9.9x10-15 atm cu.m/mol

Heat of Fusion 10.71 kJ/mol

Table 4.3 Thermodynamic Properties of Saturated Liquid Water

1 1000 4226 0.001655 0.569 656

5 1000 4216 0.001484 0.576 872

10 1000 4206 0.001302 0.584 1227

15 999 4198 0.001150 0.592 1705

20 998 4191 0.001021 0.599 2339

25 997 4186 0.000913 0.607 3170

30 996 4182 0.000820 0.613 4248

35 994 4180 0.000740 0.620 5630

40 992 4178 0.000671 0.626 7386

45 990 4178 0.000611 0.632 9596

50 988 4178 0.000560 0.638 12352

60 985 4182 0.000474 0.648 19940

70 983 4188 0.000408 0.657 31181

80 980 4197 0.000355 0.665 47368

90 977 4208 0.000313 0.671 70092

100 973 4221 0.000279 0.677 101261

110 970 4235 0.000252 0.681 143124

120 967 4251 0.000229 0.684 198285

130 963 4269 0.0.00209 0.686 269713

140 960 4289 0.000193 0.686 360745

150 956 4312 0.000179 0.686 475089