Vacuum Distillation

Vacuum Distillation

Contents
1. Introduction 2. Reduced Crude Flashing 3. Vacuum Fractionator 4. Steam Jet Ejectors 5. Vacuum Tower Control System 6. Startup 7. Troubleshooting
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Vacuum Distillation

1. Introduction

Vacuum Distillation

In order to maximize the production of gas oil and lighter components from the bottoms material of an atmospheric distillation unit, these bottoms (reduced crude) can be further distilled in a vacuum distillation unit. Vacuum distillation of an oil means that the pressure on the oil being distilled is lower than the atmospheric pressure It does not mean that there is a perfect vacuum above the liquid
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Vacuum Distillation

The distillation of heavy oils is conducted at a low pressure in order to avoid thermal decomposition or cracking at high temperature. A stock which boils at 400 C at 50 mm. would not boil until about 500 C at atmospheric pressure, at which temperature most hydrocarbons crack.

Vacuum Distillation

For distillation to take place, the vapor pressure of the liquid being distilled must be a little greater than the pressure above it.
The molecules that comprise a liquid are held together by two forces:

Natural cohesion, and The weight of the atmosphere pressing

down.

This pressure is equal to 14.7 psi. at sea level and will support a column of water 34 ft. high.
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Vacuum Distillation

Now if boiling will begin when the vapor pressure of the liquid has become a little greater than the pressure holding down, it is clear that by removing some of the holding down force the liquid will start boiling at a lower temperature.

Vacuum Distillation

The vacuum unit differs from the atmospheric type in that it has a fractionating column of larger diameter with bubble trays farther apart.

This is necessary because much larger volumes of vapors have to be handled because of the lower pressure.
Any sudden increase in vacuum will expand the volume of the vapor rapidly and possibly result in puking the tower.
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Vacuum Distillation

In the vacuum unit, almost no attempt is made to fractionate the products. It is only desired to :

Remove the entrained pitch, Vaporize the gas oil , and Condense the liquid product.
as efficiently as possible.

Vacuum Distillation

Bottoms from the crude tower contain material that can be charged to:

Catalytic cracking unit, or Be used for lube oil stocks .

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Vacuum Distillation

Distilling this material at atmospheric pressure would require high temperatures that would cause thermal cracking. Thermal cracking is undesirable because :

It would cause a loss of valuable product, Degradation of valuable product, and Shortened run time due to coke formation
in pipes and vessels.

For these reasons we conduct the distillation of the heavy reduced crude under vacuum in the vacuum tower.
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Vacuum Distillation

To achieve a deep vacuum,

Pressure drop through the column must be kept low. Instead of the type trays we use random packing and demister pads to keep the vapor velocities low a large diameter tower is used.

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Vacuum Distillation

An actual operating vacuum tower as shown

The side draws from the vacuum tower may be: lube oil stocks or charge to the Cat Cracker The bottoms (vacuum residual) may be : heavy fuel oil or asphalt.
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Vacuum Distillation

2. Reduced Crude Flashing

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Vacuum Distillation

2.1 Vacuum Bottoms Handling

2.2 Entrainment Control

2.3 Product Condensation

2.4 Vacuum Pressure

Measurement

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Vacuum Distillation

The reduced crude is charged through a heater into the vacuum column in the same manner as whole crude is charged to an atmospheric distillation unit.

However, whereas the flash zone of an atmospheric column may be at 11.3 kg cm2,
the pressure in a vacuum column is very much lower

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Vacuum Distillation

The heater transfer and flash zone temperature are generally varied to meet the vacuum bottoms specification, which is probably either:

Gravity or viscosity for fuel oil or Penetration specification for asphalt.

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Vacuum Distillation

The penetration of an asphalt is: The depth in 1/100 cm, which a needle carrying a 100g weight sinks into a sample at 77F in 5 seconds. So that the lower the penetration the heavier the pitch. Very heavy pitches are called asphalts.

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Vacuum Distillation

If the flash zone temperature is too high

The crude can start to crack and produce gases which overload the ejectors and break the vacuum.

When this occurs,

it is necessary to lower the temperature. And if a heavier bottoms product is still required, an attempt should be made to obtain a better vacuum instead.
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Vacuum Distillation

Slight cracking may occur without breaking the vacuum. This is sometimes indicated by a positive result from the Oliensis Spot Test.

The Oliensis Spot Test

Is a simple laboratory test which purports to indicate the presence of cracked components by the separation of these components when a 20% solution of asphalt in naphtha is dropped on a filter paper.
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Vacuum Distillation

Some crudes always yield a positive Oliensis asphalt, regardless of process conditions. If a negative Oliensis is demanded, operation at the highest vacuum and lowest temperature should be attempted. Since the degree of cracking depends on both The temperature, and The time during which the oil is exposed to that temperature.
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Vacuum Distillation

The level of pitch in the bottom of the tower should be held at a minimum, and its temperature reduced by recalculating some pitch from the outlet of the pitch crude exchanger to the bottom of the column. It will often be observed that : When the pitch level rises the column, vacuum falls because of cracking due to increased residence time.
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Vacuum Distillation

The flash zone temperature will vary widely depending upon: The crude source pitch specifications, The quantity of product taken overhead, and The flash zone temperatures from below 315 to even 425 C have been used in commercial operations.

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Vacuum Distillation

Some vacuum units are provided with facilities to:

Strip the pitch with steam,

This will tend to lower the temperature necessary to meet an asphalt specification, but an excessive quantity of steam will overload the jets.

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Vacuum Distillation

2.1 Vacuum Bottoms Handling

Pitch must be handled more carefully than most refinery products.
The pitch pumps which handle Very hot, Heavy material Have a tendency to lose suction.

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Vacuum Distillation

This problem can be minimized by: Recycling some cooled pitch to the column bottom and so reducing the tendency of vapor to form in the suction line. The pitch pump glands be sealed in such a manner so as to prevent the entry of air.

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Vacuum Distillation

Since most pitches are sold at atmosphere temperatures. All pitch handling equipment must either be: Kept active, or

Flushed out with gas oil when it is shut down.

Steam tracing alone is sometimes inadequate to keep the pitch fluid, but where this is done, the highest pressure steam available should be used.
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Vacuum Distillation

It is often desirable to send pitch to storage at high temperature to facilitate blending.

It is sometimes cooled in open box units, while shell and tube units are not efficient in this service.

If it is desired to increases the temperature of the pitch:

It is better to do so by lowering the level

of water in the open box, and not by lowering the water temperature.
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Vacuum Distillation

If the water in the box is too cold:

Pitch can solidify on the inside wall of the

tube and insulate the hot pitch in the central core from the cooling water. Lowering the water temperature can actually result in a hotter product. When pitch is sent to storage at over 100 C, insure that the tank is absolutely free from water.
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Vacuum Distillation

Pitch coolers should always be flushed out with gas oil immediately once the pitch flow stops, since melting contents of a cooler is a slow job.

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Vacuum Distillation

2.1 Entrainment Control

The vapor rising above the flash zone will entrain pitch, which cannot be tolerated in cranking unit charge. The vapor is generally washed with gas oil product, sprayed into the slop wax section.

Slop Wax
The mixture of gas oil and entrained pitch. it is often circulated over the decks to improve contact.
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Vacuum Distillation

slop wax can also be re-circulated through the heater to the flash zone and re-flashed, if the plant has the capacity to do so.
If, however, a crude contains volatile material compounds, these will be recycled with the slop wax and can finally rise into the gas oil .

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Vacuum Distillation

Where volatile metals are a problem, it is necessary either: To yield slop wax as a product, or To make a lighter asphalt.
which will contain the metal returned with the slop wax. compounds

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Vacuum Distillation

Some slop wax must be;

Yielded in order entrainment..

to

reject

the

captured

The final stage of entrainment removal is obtained by:

Passing the rising vapors through a metallic

mesh demister blanket through which the fresh gas oil is sprayed..

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Vacuum Distillation

Most of the gas oil spray is re-vaporized by the hot rising vapors and returned up the column. The amount of spray to the demister blanket is generally varied so that the yield of slop wax necessary to maintain the level in the slop wax pan is about 5% of the charge .

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Vacuum Distillation

If the carbon residue or the metals content of the heavy vacuum gas oil is high: A greater percentage of slop wax must be withdrawn or circulated. Variation in the color of the gas oil product is a valuable indication of the effectiveness of entrainment control.

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Vacuum Distillation

2.3 Product Condensation

The scrubbed vapor rising above the demister blanket is the product, and no further fractionation is required. It is only desired to condense these vapors as efficiently as possibly. This could be done in a shell and tube condenser.

But these are inefficient at low pressures, and the high pressure drop through such a condenser would raise the flash zone pressure.
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Vacuum Distillation

The most efficient method is to contact the hot vapors with liquid product which has been cooled by pumping through heat exchangers.

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Vacuum Distillation

It is further desired to usefully recover the heat of the rising vapors by heat exchange against crude oil, So we must arrange to have the circulating liquid at a high enough temperature to permit efficient heat exchange.

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Vacuum Distillation

We therefore have to compromise. If the gas oil circulation is high enough to condense all the vapors:

The gas oil pan temperature will be so low

that we will have inefficient heat exchange.

In order to obtain a suitable high pan temperature we are forced to reduce the circulation rate until some of the vapors escape uncondensed.
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Vacuum Distillation

The problem of uncondensed vapors is easily solved by: Adding a small circulating LVGO section to catch these vapors by condensation against LVGO from a water cooler.

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Vacuum Distillation

HVGO circulation rate

The HVGO circulation rate is chosen to maximize crude heat exchange .
The best way of doing this on an operating unit is To observe the temperature of the crude leaving the crude / HVGO exchanger, Then lower the HVGO circulation rate by 10% .
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Vacuum Distillation

If the crude temperature rises The effect of the higher HVGO pan temperature has been greater than the effect reduced circulation, and we should try some more of the same %age . If the crude temperature is lower We should try a 10 percent change in the opposite direction.

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Vacuum Distillation

Sometimes it is impossible to remove enough heat with crude exchange alone, and some HVGO from the outlet of the HVGO cooler is returned to the circulating line.

This should only be done when necessary, since both heat and cooling water are wasted.

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Vacuum Distillation

The HVGO product is cooled and pumped to storage on HVGO pan level control. The LVGO section is a final contact condenser.

Normally the circulation rate should be adequate to keep the vapor to the jets within about 5C of cooling water temperature. A high circulation rate will provide a cushion against upsets.
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Vacuum Distillation

2.4 Vacuum Pressure Measurement

Confusion often arises because of the different scales used to measure vacuum.
Positive pressures are commonly measured as: kilograms per square-centimeter above atmospheric pressure. Atmospheric pressure is: gauge

1.035 kg/cm2 760 millimeters of mercury absolute.

While a perfect absolute. vacuum is 0 millimeters
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Vacuum Distillation

3.Vacuum Fractionator

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Vacuum Distillation

The function of a vacuum tower:

Is to fractionate hydrocarbons that boil above 700F (370C) in the crude tower.

Vacuum Column Pressure

The pressure can be reduced to around 1.0 psia, below the slop wax tray. This is a total reduction in absolute pressure of perhaps 28.7 psi from the bottom of the crude tower.
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Vacuum Distillation

This large difference in pressure: Enables a great deal of hydrocarbon to flash overhead in the vacuum tower.

While maintaining a bottoms temperature not exceeding, for example, 730 780F (388 415C) depending on the crude source.

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Vacuum Distillation

Stripping Steam
Can be injected into the bottom boot of the column to:

o Further aid in removal of o Help produce proper

penetration asphalt, and

usable products from the bottoms material,

o Decrease the partial

pressure of the bottoms liquid.
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Vacuum Distillation

The bottom of the vacuum tower is swaged down: To decrease the time that the bottoms liquid spends at the elevated bottoms temperature.

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Vacuum Distillation

Quench oil
A quench oil inlet line is also provided to protect the bottoms pumps.

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Vacuum Distillation

Feed Line
The feed line to a vacuum column is very large in comparison to the feed lines of most fractionators. This is because of the low pressure which causes almost all the vacuum column feed to be vapor.

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Vacuum Distillation

Tangential distributor
Also requires a special distributor called a tangential distributor that: Imparts a swirling direction to the feed and Prevents damage to equipment above the distributor.
Due to the rapid expansion of the feed as it enters the low pressure of the vacuum tower.

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Vacuum Distillation

Internals
Are designed for a minimum amount of pressure drop. The only internals that extend completely across the entire column are:

The slop wax

accumulator,

The grid pad, and Demister pad.

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Vacuum Distillation

The grid and demister pads provide coalescing mediums: To remove entrained liquid particles from the rapidly rising vapors.

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Vacuum Distillation

Spray distributors
Spray distributors are used to aid the grid and demisters in coalescing.

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Vacuum Distillation

Side by Side Pans

There are no of trays in this vacuum tower.
But what appears to be trays are side-by-side pans. Their outer edges Perforated by holes, and Stiffened by metal lattice.
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Vacuum Distillation

The side-by-side pans:

Overlap and Provide a cascading effect to the condensed liquid.

Hot vapors pass through the cascade to re-vaporize the lower boiling components of the liquid.
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Vacuum Distillation

Accumulator trays are designed to provide a vapor-free liquid to the suction of side draw pumps. Pump vents are returned to the column to allow removal of non-condensable from the pump during startup.

This helps a great deal in getting the pump started.

After the pump is pumping properly, the vent should be closed.
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Vacuum Distillation

Top section
The top section of the vacuum column is swaged down because the traffic of material through the top of the column is much less than at the side draws.

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Vacuum Distillation

In fact, too many light ends in the feed or light ends formed by thermal decomposition of the bottoms would place an undue burden on the vacuum ejectors that have created and are maintaining the low pressure on the vacuum column
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Vacuum Distillation

Vacuum columns are generally designed to withstand an internal pressure of 50 psi (3.5 Kg/cm2 gauge), and an external pressure of 14.7 psia (760 mm absolute)
To strengthen the vessel walls to work between these two pressures

stiffeners are used

These are merely rings welded around the column and spaced a few feet apart.
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Vacuum Distillation

Materials of construction
The materials of construction used in the design of a vacuum tower are: The vessel with killed carbon steel. The lower section clad with an 11-13% Cr S.S. The slop wax accumulator is made of a

12% Cr S.S.
The wall of the accumulator is lined with concrete.
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Vacuum Distillation

The grid is constructed of 304 stainless steel.

The upper demister pad is constructed of monel. Side-by-side pans are constructed of 12% Cr S.S. The remainder are constructed of carbon steel.

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Vacuum Distillation

4. Steam Jet Ejector

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Vacuum Distillation

4.1 Introduction
4.2 Operating Principle

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Vacuum Distillation

4.1 Introduction
Vacuum is methods: maintained by two general

Vacuum Jets, and Vacuum pumps Jets.

Vacuum jets are used extensively in yard

equipment, whereas

Vacuum pumps are widely used in the

laboratories. The vacuum system is used to remove vapors from the system which cannot be condensed.
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Vacuum Distillation

Steam jet ejectors are commonly used in distillation units and can be employed:
Singly, or In stages. To create a wide range of vacuum conditions. Their wide acceptance is based upon:

Their having no moving parts, and Requiring very little maintenance.

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Vacuum Distillation

Vacuum jets pull gases from the tower by using air, steam, or water in the jet.

The jets generally use

steam as the motivating material.

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Vacuum Distillation

A series of jets (normally three) is used to boost the gases from the pressure of the vacuum tower to atmospheric pressure.
The steam used to pull the gases and is condensed in each stage and removed as water.
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Vacuum Distillation

Water is removed from the jet stages by a pump or gravity flow from a water column. If the jets are 34 ft. above ground level the water flows out by gravity. At any height lower than 34 ft. the water must be pulled off with a pump.
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Vacuum Distillation

Barometric systems are generally controlled by: Changing the water flow to the condenser for the first-stage jet. Varying steam to the jet. Varying steam is normally not as effective as varying the condenser water.

Every vacuum system has a definite capacity.

This capacity is measured as to the quantity of non-condensable removed at a definite vacuum.
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Vacuum Distillation

As the quantity of non-condensable exceeds the capacity of the jets, the vacuum begins to fail off Therefore as the cooling water to the first stage jets is reduced the quantity of non-condensed gases exceeds the capacity of the jet and causes the vacuum to fail off.

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Vacuum Distillation

4.2 Operating Principle

For two-stage ejector system. The steam is injected at high velocity through a specially designed nozzle (next Figure) and transfers sufficient energy to the gases from the suction header to entrain them through the diffuser into the first-stage discharge header.
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Vacuum Distillation

The pressure in the first stage discharge header is, of course, higher than the pressure in the suction header.

But if the velocity of the steam through the diffuser throat is high enough, gas cannot back into the suction header.
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Vacuum Distillation

If a single ejector is incapable of raising the gases to atmospheric pressure at which they can be vented, the steam is condensed and a second ejector taking suction of the noncondensable gases raises them to a higher pressure.

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Vacuum Distillation

The effect of changes in operating conditions can be summarized as follows:

Steam Pressure,
Discharge Pressure, Load, and Cooling Water Temperature.

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Vacuum Distillation

Steam Pressure
If the steam pressure greatly exceeds that for which the nozzle was designed:

The quantity of steam discharging into the

diffuser will be greater than can pass through the diffuser, and

Steam will back into the suction header.

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Vacuum Distillation

NOTES

Too low a steam pressure will mean, a drastic loss in performance of the ejector.

Wet steam will cause:

Random fluctuations in ejector

performance, and

Will erode the nozzle and diffuser.

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Vacuum Distillation

Discharge Pressure
If the discharge pressure rises above design in single stage ejector, there is an increasing probability of reverse flow. But in multi-stage units an increase in interstage pressure due to high condensate temperatures or failure of a second or thirdstage ejector will immediately affect the performance of the first-stage unit.
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Vacuum Distillation

Load
A decrease in load (kgs/hour of vapor to ejector) will result in a somewhat Higher vacuum being obtained

But if the load is increased above design

The vacuum obtained will suddenly and dramatically. fall off quite

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Vacuum Distillation

Cooling Water Temperature

The temperature at which the steam is condensed in the inter and final condensers will have a relatively minor effect on the vacuum obtained.
But will substantially reduce the load at which the ejector system breaks down. Since an increase in condensate temperature increases the inter-stage pressure.
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Vacuum Distillation

In order to insure flexibility a refinery ejector system for a vacuum unit will generally be constructed using two parallel sets. The minimum combination of equipment which will achieve a satisfactory vacuum is normally used.

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Vacuum Distillation

The vapors drawn from the top of a typical vacuum unit to the jets consists of: Air from leaks, Steam entrained from the bottom of the crude distillation tower, Light hydrocarbons, Sulfur and nitrogen compounds from thermal decomposition in the heater, and Any hydrocarbons lighter than gasoline which have not been stripped from the charge.
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Vacuum Distillation

The steam and light hydrocarbons will condense in the inter-condenser so that:
The first-stage ejectors can be heavily loaded, and Lightly load the second-stage ejectors. Any actual cracking in the furnace: will produce light gases which will very rapidly overload the second-stage ejectors.
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Vacuum Distillation

Both the condensable and non-condensable vapors handled by a typical vacuum unit ejector set are highly odiferous so that: The condensate must be stripped, and The non-condensable vapors incinerated.

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Vacuum Distillation

5. Tower Vacuum Control System

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Vacuum Distillation

Steam pressure below a critical value of a jet will cause:

The ejector operation to be unstable.

Therefore,
It is recommended to install a pressure controller on the steam to keep it at the optimum pressure required by the ejector.

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Vacuum Distillation

Air or gas is bled into the vacuum line just a head of the ejector . This makes the maximum capacity of the ejector available to handle any surges or upsets.

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Vacuum Distillation

A pressure control valve regulate the amount of bleed air used to maintain the pressure on the reflux drum. The liquid overhead product shall always be subcooled: To avoid excessive loss of product vapor to the evacuating equipment.

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Vacuum Distillation

6. Startup

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Vacuum Distillation

When starting a vacuum unit it is common practice to

S team out the heater and tower and then Pressure test the tower with steam at about 50 psig It will be assumed that this has been done and that all valves around the ejectors are closed.

a. Shut off steam to the tower.

b. Vent steam from top of tower until the

pressure is about 0.2 Kg/cm2, then close end plug the top vent.
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Vacuum Distillation

c. Open the inlet and outlet valves of one of the second-stage ejectors.

d.Open the inlet and outlet valves of one of the first-stage ejectors.
e. Open water through both condensers. f. Open steam to both first and secondstage ejectors.

g. Check that the steam is dry and adjust the steam pressure to that given on the equipment name plate.
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Vacuum Distillation

As soon as a level appears in the intercondenser, start the condensate pump and place the level on control. h. Set the ejectors run until a constant vacuum is obtained even though the presence of water in the tower may result in a poor initial vacuum. i. Charge the vacuum unit and proceed with normal operations.

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Vacuum Distillation

Adding Additional Ejectors

The operators: Should observe, and Get to know the interstage pressure. which gives: The most stable operation on a given ejector set. On most two-stage units, this is about 260 130 mm Hg. absolute vacuum.

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Vacuum Distillation

When the tower vacuum: Either decreases, or Becomes sensitive to process conditions. Additional ejector capacity should be added.

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Vacuum Distillation

If the interstage pressure has risen (the vacuum as measured in mm Hg. has increased) An additional second-stage jet should be added..

If the interstage pressure is unchanged

but the lower pressure has risen An additional first-stage jet should be added and this may render the addition of another secondstage jet necessary.
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Vacuum Distillation

a. Open the ejector discharge valve.

b. Open the steam to the nozzle. c. Check that the nozzle steam pressure is
under good control.

d. Open the ejector suction valve.

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7. Troubleshooting

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Vacuum Distillation

Occasionally, Ejectors

Will fail to pull an adequate vacuum, or Will perform erratically.

This can be the result of a large number of troubles, a few of which are listed below for checking:

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Vacuum Distillation

1. Air Leaking Into the System:

Hot bolt all flanges and manways on the vacuum tower and on the overhead line. Tighten and oil all valve packing glands. Plug all vent and drain valves and tighten any screwed connection.

Check that pump gland flushing is adjusted to maintain a positive pressure on the gland.
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Vacuum Distillation

2. Air Leaking Into Interstage:

This will be confirmed by a rise in interstage pressure.
Tighten all flanges, pump glands and screwed connections, Check that the condensate drain trap is not stuck, and Bleeding air back from the second stage.

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3. Leaking Behind Nozzle:

Certain styles of ejectors can readily leak: air or steam through a leak in the point where the nozzle is attached to the body.

4. Wrong Steam Pressure :

Check ejector name plate data and Change pressure controller setting

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Vacuum Distillation

5. Wet Steam:
Causes erratic performance. Check performance of steam traps.

6. Worn Nozzles and Diffusers:

The result of using wet steam.

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Vacuum Distillation

7. Clogged Steam Filters :

There is generally A main filter ahead of the steam pressure controller, and A filter in the nozzle of each ejector.

8. High Condensate Temperatures:

The result of: Insufficient cooling water flow, or Fouling of either the tube or the shell side of the condensers.
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9. Flooded Condensers:
The result of malfunctions of: The level controller, or The condensate drain trap, or Pump failure. If the pump will not hold suction:

Check that air is not leaking in at the gland.

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10. Faulty Installation :

Failure to properly: Align gaskets, and Similar details. which are normally insignificant: Can trap condensate pockets, or Cause turbulence. which can affect the performance of vacuum equipment.
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If an ejector set has been dismantle: Each nozzle must of course be reinstalled in the correct diffuser.

11. Back Pressure :

Due to:
Deposits in the condensers, Plugged flame arrester in the vent, Condensate pocket or other obstruction.

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12. Impossible Operation:

Such as
Attempting to obtain an absolute pressure

Lower than the vapor pressure of a liquid in the system.

If a very little vacuum gas oil is produced: It may be so light that it will be impossible to pull a vacuum on the tower.
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13. High Tower Bottom Level:

If the level in the tower is permitted to rise:
Some cracking will occur Because the pitch is being held at a high temperature for too long.

14. Steam Entering System :

Check:
Steam-out connections on the tower, Heater, Exchangers, etc.
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15. Cracking in Furnace:

Experienced at very high transfer temperatures and can be checked by: Running an Oliensis on the pitch, or A bromine number on the light vacuum gas oil. Where a leak is elusive A special meter can be installed to measure the non-condensable being vented and These vent gases can be analyzed in the laboratory.
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