JPS5851523B2 - Collagen fiber manufacturing method - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing collagen fibers.

More specifically, the present invention aims to effectively utilize skin waste, simplify the multi-step process in the conventional collagen fiber manufacturing method, and produce highly pure collagen fibers at a low cost. The present invention relates to a new method that can be used for production.

Collagen is a basic substance that constitutes the connective tissue of vertebrates, and is the main protein that forms skin, locks, membranes, ligaments, bones, etc.

It is also a white collagenous body called gelatin-producing tissue, and always exists in the form of fibers or fiber bundles.

Bed bark waste, which is a raw material for collagen, is used in the production of adhesives such as glue and gelatin, additives for livestock and fish paste products, and raw materials for foods such as edible sausage casing materials.

The skin tissue of bed skin debris is intertwined with substances other than collagen fibers, such as glycoproteins such as mucin and mucoid, hydrolysis products of fats such as glycerides and phospholipids, subcutaneous connective tissue, or collagen fibers. Proteins such as reticulin, which encapsulate elastin fibers and collagen fiber bundles, hair dregs, and insoluble lime are present.

The collagen fiber structure of animal skin intersects with a few percent of yellow elastin fibers, but the collagen fibers or fiber bundles themselves are fibers made up of several tens to hundreds of fibrils (fine fibers) with a thickness of 70 to 180 nm. (fibers) and fiber bundles (fiber bundles) in which several of these fibers are laid flat, and are said to be supported by complicated interlacing connections between the fiber bundles. , entanglement density, etc. differ depending on the type of animal skin, site, age, etc.

The collagen fiber tissue of the bedding skin used as a raw material is well developed in the dermis, but the coarsest part of the so-called network structure, which is generally unsuitable for use in leather products, is used as the raw material bedding skin for producing collagen fibers. is used.

In general, in the production method of collagen fibers, the so-called untanned floor skin is partially cut out after undergoing treatments such as soaking in water, lining, hair removal lime pickling, and splitting, which are conventionally performed in the production of leather products. Use scraps.

This cut-out waste is usually brought into contact with lime or protein-digesting enzymes, etc. to exude or digest foreign materials other than collagen fibers, and then disintegrated or disintegrated by a wet method using water as a medium or a dry method using a grinder or the like. Spread and separate into individual fibers.

Collagen fibers after disintegration or opening are solubilized by partial hydrolysis, so the former has poor water dispersibility, water drainage, and wire slippage, while the latter is accompanied by hardening due to mechanical frictional heat.

Therefore, in order to alleviate the deterioration in workability, repairs are carried out by making water repellent with a solvent, squeezing water with a pressure roller, or tanning.

Furthermore, dehydration with a solvent is also performed when collecting the individually separated fibers.

This method has also been used for fiber regeneration by enzyme and acid extraction or acid extraction alone.

That is, conventional collagen production methods combine various steps such as reliming, fermentation or acidification, degreasing, modification, scraping, loosening, beating or opening, and dehydration of bed skin waste. In the case of such a multi-stage process, it is difficult to improve productivity and labor safety on an industrial scale, and therefore manufacturing costs also increase.

Furthermore, the quality of the obtained collagen fiber itself was not satisfactory, and there were drawbacks such as the fact that it may not be suitable for various uses.

The method of the present invention was obtained as a result of intensive research to eliminate these drawbacks.

In other words, when producing collagen fibers, the raw bedding skin is not subjected to various treatments under various conditions.
This method treats bedding using a single process that combines the effects of conventional treatments.

According to this treatment method, the skin tissue maintains its original shape, but
It is possible to generate entanglements of only purified collagen fibers without solubilized collagen protein.

Also, the product is in such a state that it is easily cleaved and can be easily separated into individual fibers with a handrail.

Therefore, the products related to the method for producing collagen fibers of the present invention have high purity and can be provided to users as they are. , the advantage is that necessary subsequent treatments, such as mixing, combination, dissolution, etc., can be carried out as appropriate.

Furthermore, as mentioned above, the method of the present invention is simple and has the characteristics of high product purity. In addition, the residual fat percentage of collagen is extremely low, and it can be tanned well by conventional appropriate tanning methods. It also has many features such as being able to make paper without adding a binder to the collagen fibers.

Specifically, in the method of the present invention, bed rawhide that has been soaked in water, lined, and dehaired with lime is immersed in a deflocculating solution having the following composition at room temperature, and then subjected to wet defibration or dry opening. The peptizing solution has the following composition based on the dry weight of the rawhide.

Alkali metal or alkali 0.01-1% earth metal carbonate hypochlorite or chlorite 3-15% acid salt polyhydric alcohol 10-30% acid
0.01-0.5% water
15 to 30 times Examples of carbonates of alkali metals or alkaline earth metals include sodium carbonate, potassium carbonate, soda ash, calcium carbonate, etc. Examples of hypochlorites or chlorites include bleaching powder,
Highly bleached powder, calcium hypochlorite, hypochlorous acid) I
Examples of polyhydric alcohols include polyethylene glycol, polypropylene glycol, ethylene glycol, propylene glycol, and glycerin.

As the acid, mineral acids, particularly hydrochloric acid, are preferred.

In the method of the present invention, bed rawhide is immersed in the above-mentioned peptizing solution composition to exude or digest foreign substances other than collagen.

The temperature of the immersion treatment may be room temperature, and there is no particular need to heat it, but in cold seasons it may be heated to such an extent that the collagen does not become gelatinized.

Further, the higher the immersion temperature, the shorter the treatment time, and although the treatment time varies depending on the component concentration of the peptizer composition, it is generally in the range of 20 hours to 5 days.

When bed rawhide is treated with the above-mentioned deflocculating solution, proteins, mucoids, lipids, etc. other than collagen in the bed rawhide are decomposed or made solubilized. Collagen fibers can be isolated individually by opening them using a dry method.

This disintegration or opening process may be carried out using conventionally known devices such as a disintegrator, various types of pulverizers, and the like.

The method of the present invention will be explained in more detail below with reference to Examples.

Example Pickling, lining, hair removal Lime pickling uses 400 kg of treated cowhide dermis (75% moisture) as raw material, and uses a meat chopper (3rd plate) to make 10100 x 200 pieces. After roughly cutting into pieces of
A net-type drum washer was used to remove hair slag, etc. attached to the debris.

A peptizing solution shown in Table 1 was prepared in a chest (vertical paddle type).

Calcium hypochlorite in the table was diluted with water and stirred according to a conventional method, and then the supernatant liquid was used.

When the washed bed skin fragments were put into the peptizing solution and the pH of the peptizing solution immediately after was measured, it was 8.3, and the solution temperature was 13°C.
Met.

Afterwards, a peptizing solution containing ground skin fragments was applied continuously for 3 days.
The mixture was stirred at 3 times/hr.

The peptized state of the bed skin fragments is not sufficient to the touch; for example, solubilized colloid protein, which is a product of the peptizing reaction, is attached only to the surface associated with the subcutaneous connective tissue, which contains a large amount of lipids. When the surface was further scratched by hand, a peptized reaction product with low viscosity oozed out, but it did not reach a peptized state where it could be easily cleaved by hand.

Therefore, when the peptizing treatment was continued for two more days, the peptized skin tissue retained its original shape, had a smooth texture after washing with water, and became spongy with good water absorption and desorption properties.

The product was also easily disintegrated by hand, allowing it to be separated into individual fibers using a handrail.

Subsequently, the skin was washed with water, and the pH of the washing solution for soaking the skin was measured and found to be 5.4, which is equal to the isoelectric point of rawhide.

Next, it was disintegrated using a pulper (dry loaf type) and separated into individual collagen fibers.

There are no tangles or agglomerations of fibers in the slurry in the aqueous medium.
Water dispersibility was good.

The collagen fibers after disintegration were further washed using a cylinder press (wire 80 mesh), dehydrated, and collagen fibers with a water retention of 15% were collected.

As a comparison with the above-mentioned wet disintegration, dry fiber opening was performed using a cutter mill type pulverizer (screen pore size: 5 wg).

The deflocculating raw material used for fiber opening was prepared in the same manner as the raw material used for the wet deflocculating process, but the final water content was adjusted to 40% to prevent powdering.

Next, the collagen fibers obtained in the above step were selected using a paper pulp flat screen.

The seminal yield was as shown in Table 2 below.

Note that the above-mentioned selected collagen fibers had good properties with a smooth texture.

The following tests were conducted on the above collagen fibers.

(a) Using a single fiber index paper pulp TAPPI type sieving tester, JIS
The test was conducted in accordance with the method of P8207.

The results are shown in Table 3 below.

The single fiber length varies depending on the tanning method and temperature when collagen fibers are tanned later, but it is shown as a guideline.

(b) Freeness (C, S, F,) Using Canadian standard freeness tester for paper pulp, J
Freeness was tested according to IS P8121.

As a result, the collagen fiber obtained by the wet method had an average value of 760d, and the collagen fiber obtained by the dry method had an average value of 630rILl.

From the above, it can be seen that both have a freeness equal to or higher than that of wood pulp.

←) Preparation of paper sheets (unmodified collagen fibers) The collagen fibers were beaten in a ball mill and made into TAPPI for paper pulp.
After forming the paper sheets into sheets using a standard sheet machine, various physical properties of the paper sheets were measured.

The measurement conditions were 22°C, 65°C RH.

The results are shown in Table 4 below.

(→ Preparation of paper sheets (modified collagen fiber paper sheets) Wet fibers were beaten with a modified beater, modified with a synthetic tanning agent made of naphthalene thread wire hardware, and then made into sheets using a TAPPI standard sheet machine for final valves. .

The paper sheets were tested at 22° C. and 65% RH.

For comparison, a similar test was conducted on paper.

The results are shown in Table 5 below.

As can be seen from the above test results, the collagen fibers prepared by the method of the present invention have high purity and have extremely good physical properties as a fiber. It is superior to products made using other methods.

The collagen fibers produced by the method of the present invention may have a slight brownish tinge due to changes in raw materials, peptizer composition, concentration, and other processing conditions; By this, white discoloration can be improved by 80% or more.

Transparency can also be increased by moving the pH away from the isocenter of collagen by treatment with dilute acids or alkalis.

Claims (1)

[Scope of Claims] 1. Pickling, lining, and hair removal lime pickling are performed by treating the treated floor hide with 0.01 to 1% of alkali metal or alkaline earth metal carbonate based on the dry weight of the floor hide. salt, 3-15% hypochlorite or chlorite, 10-30% polyhydric alcohol, 0. A method for producing collagen fibers, which comprises immersing the collagen fibers in a peptizing solution consisting of 1 to 0.5% O acid and 15 to 30 times water, followed by wet defibration or dry opening. 2. The method for producing collagen fibers according to claim 1, wherein the immersion treatment is performed at room temperature for 20 hours or more. 3. The method for producing collagen fibers according to claim 1 or 2, wherein the alkali metal or alkaline earth metal carbonate is at least one of sodium carbonate, potassium carbonate, soda ash, and calcium carbonate. . 4. Claim 1, wherein the hypochlorite or chlorite is at least one of bleached powder, highly bleached powder, sodium hypochlorite, calcium hypochlorite, and sodium chlorite. 3. The method for producing collagen fibers according to any one of Item 3. 5. Collagen fibers according to any one of claims 1 to 4, wherein the polyhydric alcohol comprises at least one of polyethylene glycol, polypropylene gellicol, ethylene glycol, globylene glycol, and glycerin. manufacturing method. 6. The alkali metal carbonate is sodium carbonate,
6. The method for producing collagen fibers according to claim 5, wherein the hypochlorite is calcium hypochlorite, the polyhydric alcohol is polyethylene glycol, and the acid is hydrochloric acid.