JPS5811478B2 - Wool wax refining method - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for purifying wool wax by treating crude wool wax with a cationic ion exchange tree.

Purified wool wax is a useful substance used in pharmaceutical ointment base materials, cosmetic C creams, lotions, shampoos, conditioners, and the like.

The company's wool wax, which is the raw material for this product, is recovered from wool washing waste fluid, and contains impurities such as: ■ Contaminants such as dust, soil, and plant matter ■ Inorganic salts that are thought to be components of sheep sweat ■ Manure, blood, and other oxides Protein-based decomposition products and pigments derived from.

■ Contains a large amount of free fatty acids and free alcohol, which are decomposition products of the main component, wax ester.

For this reason, it has a significant coloration and animal odor, and has low utility value as it is, so it needs to be purified.

Conventionally, this crude wool wax is purified by (1) mixing it with hot water and centrifuging to remove impurities, spindles,
Remove water-soluble impurities.

(2) Add warm water containing acids such as phosphoric acid and sulfuric acid, and bleaching agents such as sodium hypochlorite, heat and mix, and remove the aqueous layer by centrifugation.

(3) Add warm water containing alkalis such as caustic soda and soda carbonate, and bleaching agents such as hydrogen peroxide, heat and mix, and remove the aqueous layer by centrifugation.

(4) Wash with warm water to remove excess alkali, bleach, etc.

(5) After that, perform white clay treatment as necessary.

This was done through a series of operations.

In general, when refining wool wax, coloring and reducing the acid value are the most important.Especially, with the conventional refining methods such as those mentioned above, (1) the degree of purification of the product is greatly influenced by the quality of the crude wool wax that is the raw material; Ru.

(2) The operation is extremely complicated and takes a lot of time.

(3) Impurities with large molecular weights such as proteins are difficult to remove.

(4) The yield of wool wax is low at about 70 cm.

(5) A large amount of contaminated wastewater is produced.

(6) Difficult to remove animal odor.

There are drawbacks such as.

In addition, as a method to improve the conventional general law,
6-10475 describes a method for purifying fats and oils using a strongly basic ion exchange resin.

However, although this method using a strongly basic ion exchange resin is effective in reducing the acid value of wool wax, it is less effective in improving the hue.

In addition, strongly basic ion exchange resins have drawbacks such as their exchange groups are chemically weak, have a short lifespan, and are difficult to regenerate.

The present inventors have finally arrived at the method of the present invention as a result of detailed research on improving the hue of wool wax.

That is, the present invention provides a method for refining wool wax, which is characterized in that, in refining wool wax, the wool wax is made into a solution of a non-polar organic solvent, and the solution is passed through a cation exchange resin to adsorb and remove impurities in the wool layer. It is a purification method.

The invention is generally carried out as follows.

Wool wax is made into a solution of an organic solvent, and insoluble matter is removed, and the wool wax is passed through a cation exchange resin layer that has been regenerated into H type.

The treatment temperature is in the range of 20 to 100°C, preferably 30 to 4
In the range of 0°C, the concentration of the solution is in the range of 5 to 50 wt%, preferably 10 to 30 wt%.

Also, the liquid passing rate is 0.5 to 2 (l/l-exchanged resin/hr)
A range of is desirable.

After treatment, the solvent is distilled off to obtain a refined wool taste.

If necessary, further remove trace amounts of residual solvent and odor by steam distillation, etc.

The cation exchange resin used in the present invention is a strong acid type resin (for example, Amberlyst 15, Amberlyst
N1004, Amberlite 2000, etc., all manufactured by Nippon Organo) 1. Especially durable against organic solvents.
MR type (Macro-Retic) in terms of ion exchange rate.
ular) exchange resin is desirable.

The solvent used in the present invention is preferably a non-polar organic solvent that can dissolve wool wax such as benzene or hexane. Good results are not always obtained, perhaps because impurities that have been adsorbed are easily eluted due to the polarity of .

Regeneration of the cation exchange resin used in the present invention includes:
It is preferable to use a lower alcohol such as methanol or ethanol, and more preferably a lower alcohol containing an acid such as hydrogen chloride or sulfuric acid.

After replacing the non-polar organic solvent with methanol etc., it is possible to regenerate with a basic aqueous solution such as caustic soda or caustic potash, but the regeneration ability is lower than that of lower alcohols containing basic substances, and wastewater treatment is difficult. It becomes necessary.

According to the method of the present invention, the obtained wool wax has a much better hue, has less animal odor and ash content, and is of superior quality than those made by conventional methods or the one disclosed in Japanese Patent Publication No. 36-10475. It is.

Furthermore, the processing operation is simple, the yield of wool wax is high, and the process can be carried out without producing waste water.

Next, the present invention will be explained in more detail with reference to Examples, which are not intended to limit the present invention, but may be modified within a range that does not change the nature of the present invention.

In the following examples, all numbers indicate weight, and Gardner chromaticity was measured by the method described in Standard Oil and Fat Analysis Test Methods (edited by Japan Oil Chemists' Association).

The methanol and n-hexane used were reagent grade.

Example 1 160 g of a strongly acidic MR type ion exchange resin (Amberlyst 15) was slurried in methanol, and the inner diameter was 22 mm.
It was packed into a V jacketed column.

The height of the resin layer was approximately 110 cm.

After washing the resin by passing methanol through this, 4N
-HCl aqueous solution was passed through the tube for regeneration.

Thereafter, it was washed with purified water, the water was replaced with methanol, and finally the water was replaced with n-hexane.

A 10 $ n-hexane solution of crude wool wax was passed through this ion exchange resin layer at a rate of 200 cc/hr.

During the liquid flow, hot water was passed through the column jacket to maintain the temperature of the resin layer at 30°C.

Approximately 1300 g of 10 n-hexane solution was passed through the resin layer, the liquid that had passed through the resin layer was collected, and n-hexane was distilled off.
A refined wool taste of g was obtained.

The Gardner chromaticity of the raw wool wax at this time was 17, but the purified wool wax had a Gardner chromaticity of 12, and its odor and ash content were significantly lower than that of the raw wool wax.

The recovery rate of wool wax was 95 cm.

Example 2 According to Example 1, approximately 500 ml of methanol was passed through the ion exchange resin layer through which the wool wax had been passed, and then INHcl-
Approximately 3 liters of methanol solution was passed through the tube to regenerate the ion exchange resin.

After that, methanol was passed through it to wash out HCl, and then
- Methanol was replaced by hexane.

13 of the same crude wool wax as in Example 1 was applied to this ion exchange resin layer.
0p as a 10% n-hexane solution, 200cc/h
The liquid was passed at a rate of r.

The wool wax obtained by collecting the liquid passed through the ion exchange resin layer and distilling off n-hexane has a Gardner chromaticity of 12 as in Example 1, and the ion exchange resin was sufficiently absorbed by the above method. Indicates that it is being played.

On the other hand, when an ion exchange resin regenerated with a 4N-Hcl aqueous solution was used instead of the above-mentioned INHCl methanol solution, the Gardner color of the obtained wool wax was 15, indicating that the ion exchange resin was not sufficiently regenerated. do not have.

Example 3 Approximately 4 (l) of each of the resins listed in the table below was regenerated into the H form with a 4N-HCl aqueous solution, washed with purified water until the washing solution became neutral, replaced the water with methanol, and finally A column having an inner diameter of 174 mm was filled with hexane.

A 10% solution of 30 g of crude wool wax (Gardner chromaticity 18) in n-hexane is passed through the resin layer, and after the entire amount has passed, about 50 cc of n-hexane is further passed through.

All of the effluent was collected and the Gardner color after hexane was distilled off is shown in the table below.

Improvements in Gardner chromaticity were observed in all cases, but the improvement in hue was particularly remarkable in those using strongly acidic, and even more strongly acidic MR type ion exchange resins.

Example 4 40 g of each Amberlyst 15 was regenerated into H-form with a 4N HCl aqueous solution, washed with purified water until the washing liquid became neutral, and the water was replaced with methanol.

This resin was packed into a column with an inner diameter of 17y, and replaced with each solvent shown in the table below.

30 g of each crude wool wax (Gardner chromaticity 18) was taken, diluted to 10 parts with each solvent listed in the table, and passed through a resin layer substituted with the same solvent.

The filtered liquid was collected and the solvent was distilled off, and the Gardner chromaticity of the purified wool wax obtained was compared.

Improvement in hue was observed in all cases, but the improvement in hue was particularly remarkable when non-polar organic solvents such as hexane and benzene were used.

Claims (1)

[Claims] 1. A method for purifying wool wax, which is characterized in that the wool wax is made into a solution of a non-polar slave solvent, and the solution is passed through a cation exchange resin to adsorb and remove impurities in the wool layer.