DD287274A5 - 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 both for the staging of a p H value in the working range of the alkaline enzyme used during the enzymatic reaction and before the termination of the reaction to p H elevation to p H 10.7 and a temperature of 98 reaches up to 100C during filtration. {Low-Sulfate Protein Hydrolyzates; enzymatic hydrolysis; chrome-tanned leather waste; p H-stating; calcium hydroxide; Termination of the reaction; Calciumhydroxidueberschusz}

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 kc'lagenhaltigen 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 executions are made for further use. The methods do not deal with the workup of the

Hydrolysates to useful low-mineral raw materials for the cosmetic or WaschmiUelinciustrle. DD-WP 212983 and DD-WP 243715 describe the enzymatic recovery of protein hydrolysates from chromium tanned Abfalleder proposed, but here with the aim of processing the hydrolysates to cosmetically usable

Products.

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 and sulfate ions.

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

technological processing and inferior cosmetic products.

Object of 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 the 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 free of calcium ion product allow.

According to the invention, this is achieved by using an aqueous calcium oxide or hydroxide slurry in both Control of a lying in the working range of the alkaline-active enzyme pH value during the enzymatic Reaction as well as before the reaction termination for pH increase to pH 10.5 to 10.7 and by an inactivation period of

reached at least 20min and a temperature of 98 to 100 ⁰ C in the inactivation and subsequent filtration.

The conventional pH-stating with alkalis, such. As sodium hydroxide, however, is unsuitable to achieve the desired goal. 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 the virtually calcium-free hydrolyzate has a maximum sulfate content of 0.7%.

Calcium ions are no longer detectable as oxalate. 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 method according to the invention no changes compared to the conventional enzymatic methods.

embodiments example 1

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

Cooling the mixture to 5O ⁰ C and adjusting the pH-value 9.8 with HCI, the addition of 1.0 ml of alkaline protease of Activity 1000 _Hb / ml. The pH of the batch is during the enzymatic reaction by adding portions of Calcium hydroxide suspension kept at 9. The temperature of the reaction is thermostated to 50 ° C. After a reaction time of 3 hours, calcium hydroxide suspension is added to pH 10.7, danr. ods reaction mixture in order Inactivation of the enzyme heated to 100 ⁰ C and 'left JO at this temperature. After that, quickly submerge Maintaining the temperature, the solids separated. The clear filtrate is freed at pH 10.7 with sodium carbonate of calcium ionone and further to a

worked up a neutral concentrated hydrolyzate. The result is a product with a content of 0.65% sulfate at 40%

Dry matter. There are no calcium ions as oxalate detectable. Example 2

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

Cooling the mixture to 50 ⁰ C and adjusting the pH to 9.8 using HCI, the addition of 1.0 ml of alkaline Protease of activity 1300TE _H b / ml. The pH of the batch is increased during the enzymatic reaction by adding calcium hydroxide in portions

kept the optimal value 9.0 of the enzyme. The temperature of the reaction is at 50 ⁰ C, the optimal value of the enzyme statiort.

After 2.5 h reaction time, calcium hydroxide is added to pH 10.5, then the reaction mixture in order to inactivate the Enzyme heated to 100 ⁰ C and left for 30 min at this temperature. Thereafter, the solids are rapidly separated while maintaining the temperature. The further work-up takes place after Example 1. The result is a product with 0.7% sulfate at 40% dry matter. There are no Claciumionen detectable as oxalate.

Claims (1)

Process for the preparation of low-protein protein hydrolysates !! enzymatically, characterized in that during the onzymatischen hydrolysis of sulfate-rich protein-containing raw materials a lying in the working range of each alkaline active enzyme pH by addition of calcium oxide or calcium hydroxide suspension and before the R; action discontinuation of the pH by re-addition of calcium oxide or calcium hydroxide suspension is increased to 10.5 to 10.7, after which the enzyme inactivation takes place over a period of at least 20 minutes at 98 to 100 ⁰ C and then the solids are removed while maintaining the aforementioned temperature. 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, protein-containing raw materials for cosmetic preparations.