PROCESO DE CRISTALIZACIÓN

CRYSTALLIZATION OF THE SUGAR.

36. The Vacuum-pan. " The eirup obtained in the

concentration of the juice still contains 45 per cent or

more of water. This content of water could have been

largely reduced in the multiple-effect, but to facilitate the

graining of the sugar further evaporation is conducted in

a vacuum-pan, in single-effect.

The modem vacuum-pan is usually a vertical cylindrical

vessel, of cast iron^,with a conical bottom and is fitted with

a number of copper steam-coils and has a large door or

strike-valve at the bottom, for the discharge of the sugar.

The roof or dome of the pan is connected with a save-all

and condenser by a large vapOT-pipe and with a vacuiunpump

directlyby the vapor-pipe or by a small pipe,according

to the type of pump. The vapor-pipe is usually made very

large, that the velocityof the vapors may be comparatively

slow, thus reducing the entrainment of sirup. Hhe pan is

also provided vsritheye-glassesor lunettes through which to

observe the progress of the boiling liquor,and a proof-stick

for the removal of test samples. The apparatus is so

arranged that the panman can vary the temperature of

the boilingliquor by increasingor decreasing the vacuum

which is produced by the pump and condenser. The pump

is said to be of the ''wet system " when all of the condensingwater

and the ctmdensed vapors are passed through it. The

vapors are condensed in a special condenser, when using ,

a pump of the ''dry system," and flow with the condensing-

water through a torricilian tube or "leg-pipe" to a hot

well and thence from the factory. The air is led off in as

separate pipe and removed by the pump..

The pan as described is of the usual form. Various types

of vacuum-pans are used. These vary in the extent and

85

86 CRYSTALLIZATION OF THE SUGAR.

arrangement of the heating Hurfaces,in the relation of the

heightto the diameter of the pan, and in the use or absence of

specialdevices to promote the circulation of the boilingmass.

37. Boiling Sugar to Grain. " In order to facilitate

the descriptionof pan-boilinga,nd to familiarize the chemist

with factory terms, a few expressions used by sugar-boilers

will be first given. These expressionsdiffer somewhat in

the cane, beet, and refiningbranches of the industry. Only

those customary in cane-work will be given:

The concentrated juice is called "sMp'* or "meladura,"

the latter word is Spanish and is used by foreigners in

Cuba and other parts of Spanish-America. The ctoranctednmass

of crystalsand molasses form the ''massecuite,"

or when boiled partly with sirup and partly with molasses,

"mixed massecuite," and each boilingis called a "strike."

When a portion of a strike is removed from the pan and the

remainder is left as a footing or nucleus upon which to boil

another strike,the portion so left is termed a "cut." There

is some confusion in regard to the use of the word "cut," as

many sugar-^boilerusse this Word for the massecuite removed

from the pan. The pirocess is termed "cutting."

Where two or more pans are worked side by side they

are often connected with one another by large pipes, with

suitable valves, for drawing the massecuite from one to

another. These are called "cut-over pipes."

In modem practice,when a grained strike reaches a

certain stage, diluted molasses is drawn into the pan instead

of sirup and it is said to be "boiled in," or "boiled in on

grain-sugar."

When the liquor in the pan has been concentrated to a

certain density and is more or less saturated with sugar, it

fs said to haVe reached " proof." The proof may be ' ' strong "

or "weak" as the liquidis of greater or less density. This

expression is still further modified, as will be explained in

connection with the boiling of molasses-sugars.

The process of boiling sugar is as follows: The pan is

closed, the vacuum pump is started, and when the gauge

shows a vacuum of 15 to 20 inches of mercury, tlie chargevalve

is opened and sufficient sirup is drawn into the pan

td cover the coils. Steam is turned into the coils ahd tlie

BOILING SUGAR TO GRAIN. 87

sirup is rapidlyconcentrated to proof. The quantityof sinip

used depends upon whether the boiler wishes "to grain" high

or low in the pan. In making fine-grainedsugar he will grain

high, as he needs many crystalsand comparatively little

room for their growth; on the contrary, in making cgorairnse-d

sugar he will grain low, and form few crystals.

As the liquor boils down, the steam-valves of the upper

coils are successivelyclosed,anii as it becomes more and

more concentrated, the portions projected against the eglyae-sses

flow more and more slowly and the panman increases

or decreases the quantity of water injected into the cdeon-ser

until the liquor boils at the desired teftiperature.

At this stage there are two methods of procedure: (1)

The concentration is continued until the liquor is csiueffnit-ly

supersaturated with sugar, as is indicated by a

sample drawn by the proof-stick. The watet of injection

into the condenser is now increased and the steam-pressure

on the coils reduced, thus coolingth^ boilingmass, increasing

the degree of saturation,and forcing minute crystalsof

sugar to form. These manipulations vary somewhat aicncgordto

the vacuum-pan itself and the qualityof the sirup,

but in general are as described. (2) The second method

of graining is that usually employed in the United States.

The concentration of the liquor is continued until crystals

of sugar separate, and when the panman consider^ that

there are sufficient crystalshe raises the temperature of

the pan and injectsmore sirup. The first method produces

a sugar of more uniform grain than the second, since all ol

the crystalsrequired are formed at once.

After the crystals are formed, sirup is drawn into the.

pan from time to time as the water evaporates. This

charging of the pan with sirup,and Judging just when to

charge, requiresmuch skill and practiceon the part of the

boiler in order to secure the best results. If he injects

sirup when the mass is too concentrated, with the liquor

surrounding the crystals too rich in sugar, fresh crystals

will be formed and must be remelted. Th^se crystalsare

termed -'false grain," and where formed at a late stage

through carelessness of the sugar-boilerand are not removed,

they impede or even prevent the curing of the sugar in

88 CRYSTALLIZATION OF THE SUGAR.

the centrifugals.False grain may be formed by charging

the pan too freelywith sirup,or by coolingthe massecuite

while the sirupsurroundingthe crystalsis rich in sugar and

of such densitythat it is supersaturatedat a lower teumrep.era-

Also,if a sufficient number of crystalshave not been

formed when grainingthe strike,there is great risk of the

formation of false grain,after the crystalshave grown to

largesize. If the false grainis formed and not removed at

this stage of the boiling,the sugar cannot be purged of

molasses. False grain is gotten rid of by raisingthe ptemr-ature

of the pan and drawing in additional sirupto melt

the fme crystals.

As alreadystated, as the water is evaporated, sirup is

drawn into the pan from time to time until the strike is

finished. The massecuite is kept very free,t.e., of c""nparativelylow

density,until the crystalsare largeor the pan is

about two-thirds filled. At this stage it is graduallyboiled

dryer ioid dryer until near the end of the operation,thus

impoverishingthe molasses surrounding the crystals,and

finallythe massecuite is evaporated to an apparent degree

Brix of about 93, and is then discharged from the pan.

The massecuite should be as cold as possibleat this stage.

There are various methods of estimatingthe proper moment

for strikingthe massecuite, i.e.,dischargingit from the pan.

This is usually determined by withdrawing a sample with

the proof-stickand forming it into a conical heap upon the

thumb with the finger. The consistencyof this massecuite,

as shown by its appearance, rate of flattening, etc.

are noted

by the sugar-boiler,and a practicedman can in this way

judge within narrow limits when to drop the strike.

During the boiling,care must be observed after each

charge of sirup to concentrate the mass sufficientltoy force

the sugar to deposititselfupon the crystalsalready present

and not to form new ones, Unnecessfiryconcentration

causes a waste of time and steam.

A method of charging a pan with sirup,employed with

many vacuum-pans, but not applicablewith all,is by means

of a "set feed." After the formation of the grainthe charge*

valve is opened and so adjusted that the flow of sirupinto

the pan justcompensates for the evaporation. The opening

BOILING SUGAR TO GRAIN. 89

of the valve is adjusted from time to time as the ctorancteino-n

varies, with variations in the steam-pres""ure, the

density of the sirup,etc. This method of charging, with

the first method of graining,produce a very uniform quality

of sugar, and a very good yieldfrom the massecuite. An

irregulargrain,with many minute crystals,from false grain

that has not been melted, results in a low yield of sugar

from the massecuite.

In boilinga massecuite so as to obtain the maximum

yield of sugar from it,the full number of crystalsrequired

should be formed at graining,and the crystalsshould be of

moderate and very regular size. Of course, false grain at

any stage of the operation must be avoided. The formation

of too few crystalsresults in rich molasses, since there is not

sufficient crystal-surfaceto take up the sugar, and besides

increases the risk of the formation of false grain. When

boiling a strike on a very small nucleus of massecuite or on

a small cut, there is also risk of false grain or of a partially

exhausted molasses.

The temperature to be maintained in the massecuite

during boilingvaries with the desired grade of sugar, whether,

hard or soft,white or raw. American practice also differs

somewhat from that of Java in respect to temperatures.

The Java superintendentprefersrelativelylow temperatures.

As will be noted in the chapter on sugar-refining,page 119,

hard sugars are boiled at 180" F. in the American refineries,

with no inversion. Similar but lower temperatures are

customary in the white-sugar factories of Louisiana.

Hard sugars, as stated,are boiled at high temperatures, but

they may also be produced at moderate temperatures from

sirups of low densities. High-test raw sugars should be

grained at temperatures approximating 160" F., and the

high temperature should be continued until the grain is

well developed. The temperature may be lowered in the

latter part of the strike to promote reduction of the purity

of the molasses surrounding the crystals. Massecuites that

are to be further crystallizedeither in motion (crystallizer

massecuite) or at rest in tanks should be boiled at as low

temperature as possible.
In making a very soft sugar, after graining,the tempera90

CRYSTALLIZATION OP THE SUGAR.

ture of the boilingmassecuite should be maintained as low

as possible. Low-pressure pans, i.e., pans having large

heating-surfaceand utilizingsteam of below 10 lbs. pressure,

are usually preferredfor soft-sugars.

38. Methods of Sugar-boiling. " Pan-room Dteifoinns.i-

" Raw sugar manufacturers often designate their

vacuum-pans by the letters "A," "B" and "C," as in frei-neries,

or number them, to distinguishthe grade of cmauissteand

not the pans themselves. A pan is usuallyalways

employed in boilingthe same grade of sugar in a refineryon

account of fts proximity to a certain mixer and set of cueganltrs,ifbut

this is not usuallytrue in a factory.

With the complications introduced into pan practice by

boiling-inmolasses, it is simpler to designate massecuites

by n"Un"3 rather than numbers. Formerly when only

"straight-sugars"were boiled, the strikes were numbered

"first,""second" and "third." The first strike of cmauisstewas

boiled' with pure cane-sirup,the second with first

molasses and the third with second molasses. At present

all the pahs may be boiled in part with molasses, hence

thfere is some confusion in the nomenclature. When three

massecuites are boiled with return of molasses, the writer

prefersthe followingdesignation for each: (1) First cmauisste,-

containing only sirup or sirup and a very little first

molasses. This is therefore a massecuite of high coefficient

of purity. (2) Mixed massecuite, containing a footing of

massecuite from a first pan and a large proportion of first

molasses. This is of medium purity,approximately 75** to

80**. The first and mixed massecuites will produce the same

grade of raw sugar. (3) Second or crystallizermassecuite.

This massecuite is of low purity,usually of 60" and upward.

In many factories but two massecuites are boiled,in which

case that of the second boilingis termed "mixed" or 'o'nds.e"c-

The first massecuite in this method is reduced to

about 75" puritywith firstmolasses.

Utilizingthese definitions,the methods of pan-boiling

applicablewith rich tropicalcane in raw-sugar worl^ will be

described. These methods are rapidly extending in Cuba

and possiblyelsewhere.