Chemical Refining

Muhammad Asif Ali

Factors affecting Alkali refining process

• Following factors play an important part in making the alkali refining

process operate effectively and efficiently.
1. Selection of the NaOH strength
2. Mixing time
3. Mixing energy
4. Temperature
5. The quantity of excess caustic
The conventional caustic-soda continuous system that evolved has the
flexibility to efficiently refine all the crude oils presently utilized in the
United States. The system may be outlined as follow:
• Crude receipts
• Sampling
• Crude oil conditioning
• Caustic treatment
• Caustic-oil mixing
• Soap-oil separation
• Water washing
• Vacuum drying
Crude Receipts

• Crude or degummed oils are received by railcar, truck, or barge

or from onsite extraction or degumming operations.

Sampling
• Receipts are sampled, analyzed, and then transferred to the
appropriate storage tanks.

• For optimum performance, degummed soybean oil should have a

phosphatide content below 0.3%.

• If this level is exceeded, non-degummed oil should be blended with

the degummed oil to attain a 1.0% phosphatide content.
Crude Oil Conditioning

• As needed, the oils are transferred to the appropriate pretreatment

or supply tank.

• Crude oils with high levels of phosphatides, such as soybean and

canola oils, are usually treated with food-grade phosphoric acid for a
minimum of four hours (eight hours preferred) before refining — 300
to 1000 ppm for soybean and 1000 to 3000 ppm for canola.
Purpose of acid pre-treatment
The purpose of the acid pretreatment is to

1. Precipitate phosphatidic materials

2. Precipitate natural calcium and magnesium as insoluble phosphate

salts

3. Inactivate trace metals, such as iron and copper, that may be

present in the oil
Purpose of acid pre-treatment

4. Reduce the neutral oil losses

5. Destabilize and improve the removal of chlorophyll in bleaching

6. Improve the color and flavor stability of the finished deodorized oil
Selection of Caustic Treatment
The degummed or acid-conditioned crude oil is continuously mixed with
a proportioned stream of dilute caustic soda solution and heated to
break the emulsion. Selection of the caustic treatment is determined by:
• The type of crude oil
• FFA content
• Past refining experience with similar oils
• The refining equipment available
Caustic Treatment

• The strength of the caustic solution is measured in terms of specific

gravity, expressed in degrees Baumé (°Bé).

• The caustic treatment selected for the crude oil will vary with the free
fatty acid content, the amount of acid pretreatment, and the level of
caustic “excess” over “theoretical” determined for each oil type from
previous experience.
• The theoretical quantity of caustic is based on the ratio of molecular
weights of sodium hydroxide to oleic fatty acid. This factor is
determined as follows:
• The phosphorus reduction during refining is determined largely by the
amount of water present in the caustic solution.

• Higher excess caustic treatments remove more phosphorus, but the

increase in removal is due more to the increased water than NaOH.
Caustic–Oil Mixing

• The caustic and soft oils are mixed at 30 to 35°C in a dwell mixer with
a 5 to 15-minute residence time.

• High temperatures during the caustic addition must be avoided

because they can increase the neutral oil saponification and reduce
the refined oil yield.
Caustic–Oil Mixing

• After the caustic-mixing phase is complete, the mixture should be

delivered to the centrifuges at a temperature suitable for optimum
separation.

• Most soft oils are heated to 74°C to provide the thermal shock
necessary to break the emulsion.
Soap–Oil Separation

• Refining yield efficiency is dependent on the primary separation step.

• From the caustic–oil mixer, the resultant soap-in-oil suspension is fed

to high-speed centrifuges for separation into light- and heavy-density
phases.

• These separators are designed to divide suspensions of insoluble

liquids and solids in suspension with different specific gravities.
Factors for the improvement of separation
completeness
The major factors to consider for improvement of separation
completeness include:
1. greater differences in the specific gravity of each phase
2. lower viscosities
3. higher temperatures
4. Shorter travel distance for the heavy particles
5. increased centrifugal forces
6. longer centrifugal dwell times
Water Washing

• Refined oil from the primary centrifuge is washed with hot softened
water or recovered steam condensate proportioned into the oil at a
rate of 10 to 20% of the oil flow.

• Softened water must be used to avoid the formation of insoluble

soaps.
Water Washing

• Wash water temperature is important for efficient separation in the

centrifuge.

• The water temperature should be 85°C to 90°C, preferably 05°C to 8°C

warmer than the oil temperature.
Vacuum Drying

• Water-washed oil is usually dried with a vacuum dryer before storage

or bleaching.

• Washed oil at approximately 85°C is passed through nozzles into the

evacuated section of a continuous vacuum dryer that controls the
moisture content of the washed oil to below 0.1%, most often in the
range of 0.05%.
• A typical dryer operates at 70 cm of mercury (Hg) and is equipped
with a high-level alarm and automatic shutdown capability.

• After drying, the refined oil should be cooled to 49°C to 55°C before
storage.

• For extended storage periods, a nitrogen sparge or a nitrogen blanket

applied to the surface of the oil will minimize oxidation before use.