JPS5811480B2 - Advanced purification method for wool wax - Google Patents

Description

Detailed Description of the Invention The present invention relates to a method for highly refining wool wax by treating crude wool wax with a combination of a cationic ion exchange resin and an anionic ion exchange resin. It is a useful substance used in cosmetic creams, lotions, shampoo rinses, etc.

Crude wool wax, which is the raw material, recovered from wool washing waste liquid contains impurities such as: ■ Contaminants such as dust, earth and sand, and vegetable matter ■ Inorganic salts that are thought to be components of sheep sweat ■ Manure, blood, and other oxides Contains a large amount of protein decomposition products derived from, pigments, and free fatty acid free alcohol, which is a decomposition product of wax ester, the main component.

For this reason, the coloring and animal odor are significant, and the value of using it as it is is low, so the refining process of this crude wool wax is as follows:
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, the most important factors are reducing the tarnish and acid value, and in particular, with the conventional refining methods such as those mentioned above, (1) the degree of refinement of the product is inferior to the quality of crude wool wax. Depends on it.

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

(3) Impurities with large molecular weights such as proteins are removed.

(4) The yield of wool wax is as low as about 70%.

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

(6) Difficult to remove animal odor.

The present inventors conducted research to find a method for solving these problems and easily producing highly purified wool wax in a high yield, and as a result, they arrived at the method of the present invention.

That is, in refining wool wax, the present invention converts the wool wax into a solution of a non-polar organic solvent and passes the solution through a cation exchange resin and a weakly basic ion exchange resin to adsorb and remove impurities in the wool layer. 9 advanced refining methods for wool wax.

The invention is generally carried out as follows.

Wool wax is made into a solution of an organic solvent, insoluble matter is removed, and the solution is reconstituted to H type and passed through a resin layer consisting of a combination of an existing cation exchange resin and an OHH type regenerated anion exchange resin.

The treatment temperature during liquid passage is in the range of 20 to 100°C, preferably 30 to 40°C, and 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 (1/l-exchanged resin/hr)
A range of is desirable.

What is the combination of cation exchange resin and anion exchange resin?
(1) Double-bed type in which the liquid to be treated is passed through a cation exchange resin layer and then an anion exchange resin layer.

(2) A double bed type in which the liquid to be treated is passed through an anion exchange resin layer and then a cation exchange resin layer.

(3) A mixed bed type in which the liquid to be treated is passed through a resin layer made of a mixture of cation exchange resin and anion exchange resin.

φ means a combination of three types.

No matter which combination of the three types is used, there is no significant difference in the quality (hue, acid value, ash content, peroxide value) and yield of the wool wax obtained, and the gist of the present invention is satisfied.

Wool wax can be purified using cation exchange resins alone or anion exchange resins alone, but cation exchange resins cannot significantly reduce the acid value, while anion exchange resins cannot highly reduce the ash content and color. There are some processing steps required to achieve this.

The present invention uses a combination of a cation exchange resin and an anion exchange resin to treat the wool to remove negative phase, acid value, ash content, peroxide, etc.! Not only can many of the qualities required for be improved by simple operations, but also the processing efficiency is dramatically increased compared to when a cation exchange resin and an anion exchange resin are used alone.

The iodine exchange resin used in the present invention is preferably a strongly acidic MR type resin such as Amberlyst 15, Amberlyst N1004, Amberlyte 200C (all manufactured by Nippon Organo) as a cation exchange resin, and as an anion exchange resin. is preferably a weakly basic MR type resin such as Amberlyte IRA94, Amberlyte IRA93, Amberlyst A-21 (all manufactured by Nippon Organo).

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 once adsorbed are easily eluted due to the polarity of the solvent.

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 and sulfuric acid.

Further, the anion exchange resin is preferably regenerated using a lower alcohol such as methanol or ethanol, and more preferably using a lower alcohol containing a base such as caustic soda or caustic potash.

For both cation exchange resins and anion exchange resins, non-polar organic solvents are replaced with methanol, etc. For cation exchange resins, aqueous acids such as hydrochloric acid and sulfuric acid are used, and for anion exchange resins, aqueous bases such as caustic soda and caustic potash are used. Although it is possible to regenerate it, the regeneration ability is lower than that of lower alcohols containing acids or bases, and wastewater treatment is required.

According to the method of the present invention, wool wax with a highly excellent hue and low acid value and ash content can be obtained in high yield by simultaneous or continuous operations.

Next, the present invention will be explained in more detail with reference to Examples, which are not intended to limit the present invention, and may be modified without changing the properties of the present invention.

All references in the following examples and comparative examples refer to baking soda, and Gardner chromaticity, acid value, and peroxide value were measured using the methods described in Standard Oil and Fat Analysis Test Methods (edited by Japan Oil Chemists' Association). .

Comparative Example l 160g of strongly acidic MR type ion exchange resin (Amberlyst 15) was slurried with methanol and the inner diameter was 22mmφ.
It was filled with a rem with a jacket attached.

The height of the resin layer was approximately 110 cm.

After washing the resin by passing Medinol through it, about 3 volumes of a methanol solution of IN chloride water A was passed through it to regenerate the resin into H4.

Thereafter, Q hydrogen chloride in the resin layer was removed with methanol, and finally, methanol was replaced with hexane 4 times.

In this ion exchange resin layer, 80g of crude wool wax was added to%n-
A hexane solution was passed through at a rate of 200 cc/stone.

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

Pour the entire amount of to% n-hexane solution of wool wax through the hole diameter,
All remaining two wool waxes are washed out into the resin layer using 500cc of n-hexane.

The entire effluent was collected and the n-hexane was distilled off.

Table 1 shows the Gardner chromaticity, acid value, ash content, and yield of the raw material crude wool wax and the purified wool wax obtained by the above-mentioned literature.

Comparative Example 2 210g of weak salt resistant MR type ion exchange resin (Amberlite IRA94) instead of strongly acidic MR type ion exchange resin
A crude wool wax was treated in the same manner as in Comparative Example 1, except that a methanol solution of IN caustic soda was used instead of a methanol solution of IN hydrogen chloride.

Table 1 shows the Gardner color, acid value, ash content, and yield of the wool wax obtained by this treatment.

Example 80 g of a strong acidic MR type ion exchange resin (Amberlyst 15) was prepared in the same manner as in Comparative Example 1, and 80 g of a weak salt-resistant ion exchange resin (Amberlyte IRA94) was prepared in the same manner as in Comparative Example 2. did.

A 10% o-hexane solution of crude wool wax 809 was first passed through a strongly acidic ion exchange resin, and then passed through a weakly basic ion exchange resin.

During liquid passage, the temperature of the resin layer was kept at 30°C, and the liquid passage rate was 20°C.
It was carried out at 0cc/hr.

After pouring out the entire amount of coarse wool wax, add approximately 500 cc of n-hexane.
The wool wax in the resin layer was caused to flow out.

The entire effluent was collected and the n-hexane was distilled off.

The Gardner color, acid value, ash content, and yield of the purified wool wax obtained are shown in Table 1.

It can be seen that a high-quality wool wax with a much better hue, lower acid value, and lower ash content than Comparative Examples 1 and 2 can be obtained.

Example 2 The performance of three combinations of ion exchange resins was compared.

Combination (1) is a solution of 10.9 of crude wool wax in 10% n-hexane and 25 of strong acidic ion exchange resin (Amberlyst 915) regenerated into H type in the same manner as in Comparative Example 1.
After passing the liquid through the solution, a weakly basic ion exchange resin (Amberlite IRA94
259 of ).

Combination (2) is a weakly basic ion exchange resin (Amberlite IRA94) regenerated into an OH type in the same manner as in Comparative Example 2 using a 10% n-hexane solution of the log of crude wool wax.
) and then regenerated into H-type in the same manner as in Comparative Example 1 (Amberlyst 15).
The liquid was passed through 259.

Combination (3) is a 10% hexane solution of the log of crude wool wax, 25 g of a strongly acidic ion exchange resin (Amberlyst 15) regenerated into H type in the same manner as in Comparative Example 1, and OH in the same manner as in Comparative Example 2. 25 g of a weakly basic ion exchange resin (Amberlite IRA94) regenerated into a mold was passed through the mixed resin layer.

Table 2 shows the Gardner color, acid value, and yield of wool wax obtained by each combination treatment.

In all combinations, wool layers with a high degree of purification and low hue and acid value were obtained.

Among the three combinations, combination (3) was particularly excellent.

Claims (1)

[Claims] 1. When refining wool wax, the wool wax is made into a solution of a non-polar organic solvent, and the impurities in the wool layer are adsorbed and removed by passing the solution through a cation exchange resin and a weakly basic ion exchange resin. An advanced refining method for wool wax characterized by: