DD287273A5 - METHOD FOR THE PRODUCTION OF SULFATAR PROTEIN HYDROLYSATES BY ENZYMATIC WAYS - Google Patents

Abstract

The invention relates to a process for the preparation of low-sulfate enzymatic protein hydrolysates for cosmetic preparations. The aim of the invention is to produce in the enzymatic hydrolysis of sulfate-containing substrates protein hydrolyzates having a sulfate content of not more than 0.7% at 40% dry matter. According to the invention, this is achieved by the use of calcium oxide or calcium hydroxide in the staining of an operating in the range of alkaline enzyme used p H value during the enzymatic reaction and by heating the reaction mixture to 110 to 120C for reaction termination and filtration of the solids at temperatures around 100C. {low-sulfate protein hydrolysates; enzymatic hydrolysis; chrome-tanned leather waste; p H-stating; calcium hydroxide; Termination of the reaction; Heat; Druckgefaesz}

Description

Characteristic of the known state of the art It is known that for the production of protein hydrolysates from collagen-containing raw materials bacterial, animal and

herbal proteases are used. Proteases of various Bacillusarten are described (DE-OS 2252281,

DE-OS 2643012, DE-OS 2705671, DE-OS 2709035), which are suitable for the hydrolysis of collagen-containing raw materials. The The aim of these methods is both in the complete and rapid elimination of waste products, in particular the Leather industry, as well as in the further use of hydrolysates to commercially useful products to see, but without

that further explanations are made for further use. The methods do not deal with the workup of the

Hydrolysates to useful low-mineral starting materials for the cosmetic or detergent industry. In DD-WP 212983 and DD-WP 243715, the enzymatic recovery of protein hydrolysates from chromium tanned Abft'lleder proposed here, however, with the aim of processing the hydrolysates to cosmetically usable

Produften.

The preparation of the serine protease used in DD-WP 243715 is the subject of DD-WP 241533, in which also already

the aforementioned use is pointed out.

For the problem-free further processing of these enzymatically obtained protein hydrolysates on an industrial scale as well as for

the recovery of qualitatively flawless cosmetic products, it is necessary that the protein hydrolysates are largely free of calcium t'.id sulfate ions.

This requirement is not considered in DD-WP 212983 and DD-WP 243715. According to their teachings one becomes ProteinhydrC'lysat obtained with high levels of calcium and sulfate ions, leading to considerable difficulties in the

technological processing and inferior cosmetic products.

ZIoI the invention

The aim of the invention is a process for the preparation of an enzymatic way from sulphate substrates, such as. As chrome shavings or chrome split leather, won protein hydrolyzate with a minimum content of calcium and sulfate ions, without the need for additional cleaning or precipitation operations are necessary.

Explanation of the essence of invention The invention is based on the object, while maintaining the working range of each alkaline enzyme used

(Temperature, pH, time, amount of enzyme) for the production of protein hydrolysates with the properties required for high-quality cosmetics conditions to find that during the technological regime of enzymatic hydrolysis, the elimination of the sulfate to a maximum residual content of 0.7% and Production of a virtually calgiumionenfreien free product allow.

According to the invention, this is achieved by using an aqueous calcium oxide or hydroxide slurry for stationing a

reached in the working range of the alkali-active enzyme used pH during the enzymatic reaction and by the reaction termination at 110 to 12O ⁰ C and by a temperature around 100 ⁰ C in the filtration.

The conventional pH-stating with alkalis, such. As sodium hydroxide, however, is inappropriate, the desired goal. 'U

to reach.

The conditions according to the invention change in their entirety in the present multicomponent system the chemical Balance between calcium ions and sulfate ions in favor of the formation of insoluble calcium sulfate completely surprising

so much that after the subsequent calcium separation with sodium carbonate, the concentrate of virtually calcium ion-free hydrolyzate has a sulfate content of 0.7% at most.

Calcium ions are no longer detectable by oxalate precipitation. The method is suitable for protein hydrolysis by means of alkaline enzymes whose pH ranges in one Area to pH 10.7. The amount of enzyme used depends on its activity and the desired hydrolysis effect.

The activity of the enzyme and the hydrolysis of the protein are not impaired by the agents according to the invention. The Cr ⁺⁺⁺ liberated by the enzymatic hydrolysis is precipitated as chromium hydroxide which, after termination of the enzymatic reaction, can be separated off together with excess calcium hydroxide and calcium sulphate in easily filterable form.

The choice of the conditions of the enzymatic reaction to achieve a certain molecular mass spectrum or a desired degree of degradation is subject in the inventive method no changes compared to the conventional enzymatic processes.

Ausfuhrungsbelsplele example 1

100 g of chrome cuttings are boiled with the addition of 12 g of calcium oxide in 1180 ml of distilled water with stirring for 20 minutes. To

Cooling the mixture to 5O ⁰ C and adjusting the pH to 9.3 with HCI, the addition of 1.2 ml of alkaline protease

Activity 1000 TE _Hb / ml.

The pH of the batch is adjusted to 9 during the enzymatic reaction by adding calcium hydroxide in portions

held.

The temperature of the reaction is thermostated at 5O ⁰ C. After a reaction time of 3 hours, the reaction mixture is inactivated for the purpose of inactivating the enzyme and precipitating the largest portion of Sulfate ions as calcium sulfate in a pressure vessel at 110 to 120 ⁰ C heated. After 20 to 30 minutes, the vapor pressure

relaxed and the solids were rapidly separated while maintaining a temperature around 100 ⁰ C.

The klara filtrate is freed from calcium ions with existing sodium carbonate and further to a neutral pH

reconditioned concentrated hydrolyzate.

The result is a product with 0.34% sulfate content at 40% dry matter. Calcium ions are not detectable as oxalate. Example 2

85g chrome split leather are boiled with the addition of 10g calcium oxide in 1000ml tap water with stirring for 30min. To

Cooling the mixture to 5O ⁰ C and adjusting the pH to 9.8 with HCI, the addition of 1.0 ml of alkaline protease

of activity1300TE _Hb / ml.

The pH of the batch is increased during the enzymatic reaction by adding calcium hydroxide in portions

der.i optimal value 9.0 of the enzyme kept. The temperature of the reaction is to 5O ⁰ C, the optimum "Vtrt of the enzyme statiert.

After 2.5 h reaction time, the reaction mixture to inactivate the enzyme and precipitate the largest proportion of Sulfate ions as calcium sulfate in a pressure vessel at 110 to 120 ° C heated. After 20 to 30 minutes, the vapor pressure

relaxed and the solids are separated quickly while maintaining a temperature around 100 ° C. The others

Work-up is carried out according to Example 1. The result is a product with 0.54% sulfate content at 40% dry matter. Calcium ions are not detectable as oxalate.

Claims (1)

Process for the preparation of sulfatarme.ι protein hydrolyzates by enzymatic means, characterized in that during the enzymatic hydrolysis of sulfate-rich protein-containing raw materials a lying for each used alkaline active enzyme in the working range of the enzyme liegenderpH value by addition of calcium oxide or calcium hydroxide suspension and the Reaction termination by heating the reaction mixture in a pressure vessel to 110 to 120 ⁰ C, whereupon the solids are separated at a temperature between 98 and 100 ⁰ C. Field of application of the invention The invention relates to a process for the preparation of low-sulfate enzyme-produced protein hydrolysates from sulfate-rich proteinaceous raw materials for cosmetic preparations.