KR101686474B1 - Pearl proteins solubilization manufacturing method for using alkali solubilisated and clathrate hydrate - Google Patents

Abstract

The present invention relates to a method for manufacturing a pearl protein solubilized material using alkali solubilization and clathrate hydrolysis. More specifically, the method for manufacturing a pearl protein solubilized material comprises performing alkali hydrolysis of pearl protein, which is poorly water soluble or insoluble, solubilizing pearl protein in water, and concentrating a solubilized material by using clathrate hydrolysis in a high pressure reactor. Accordingly, volatile basic nitrogen that ammonia smells remain can be conveniently removed and concentrated to form a hydrate with pure water from the pearl protein solubilized material; only the concentrated pearl protein solubilized material can be separated and obtained; processing yield of pearl protein, which is poorly water soluble or insoluble, i.e. difficult to be dissolved in water, is increased; and productivity and economic feasibility can be improved.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a pearl protein solubilization method for alkali solubilization and clathrate hydrate,

The present invention relates to a process for preparing a pearl protein solubilization using alkali solubilization and clathrate hydration. More particularly, the present invention relates to a method for purifying an insoluble pearl protein by alkali hydrolysis and solubilizing the same in a water phase, and concentrating the solubilized product using a clathrate hydrate in a high-pressure reactor to remove ammonia from the pearl protein- Volatile basic nitrogen can be conveniently removed and formed by forming a hydrate with pure water to separate and concentrate the concentrated pearl protein soluble solids so that the processing yield of the insoluble pearl protein which is difficult to dissolve in conventional water can be increased, The present invention relates to a method for producing pearl protein-soluble carbohydrate using alkali solubilization and clathrate hydration, which can improve economical efficiency, commercialize low-priced poultry protein at low price and actively utilize insoluble pearl protein as a cosmetic material.

Pearls have been used as ornaments for the past 6,000 years, and there is evidence that a considerable amount of pearls have been commerce in China around 2,500 years ago. Pearls have been popular because they produce elegant shine and light without having to process them separately.

When calcium carbonate is the main component and foreign matter enters the shell, calcium carbonate surrounds it, and the small particles of calcium carbonate crystals form a layer of material called 'Conchiolin', which is superimposed to form a layer of nacre.

Conchiolin (Conchiolin) is a type of light protein in the shell of shellfish, and has excellent effects on skin moisturizing and is used in cosmetics or external skin applications. Conchiolin, however, is an insoluble protein and needs to be dissolved to be used in cosmetics.

However, the prior art level of pearl protein solubilization is performed at the physical or mechanical decomposition level, and the processing yield is very low, about 4% of the dry raw material weight, resulting in very poor productivity and economical efficiency, and the final consumer price is very high. It was not easy.

In addition, conventional pearl powder is insoluble in water and is difficult to dissolve in water. To dissolve the pearl powder, it is necessary to perform hydrolysis by controlling the pH. Volatile basic nitrogen generated during the protein hydrolysis process is strongly retained in ammonia, It is extremely difficult to utilize the pearl protein and thus the function of the pearl protein can not be efficiently maximized.

Prior Art Document: Korean Patent Registration No. 0549399 (Registered on Feb. 17, 2006)

DISCLOSURE OF THE INVENTION The present invention has been conceived in order to solve the above-mentioned problems, and it is an object of the present invention to improve the productivity and economical efficiency by increasing the processing yield in the technique of solubilizing the pearl protein, commercialize the high- The present invention provides a method for producing pearl protein-soluble carbohydrate using alkali solubilization and clathrate hydration which can be actively utilized.

In order to accomplish the above object, the present invention provides a method for preparing a pearl protein soluble product using alkali solubilization and clathrate hydration, comprising the steps of: preparing a pearl powder; An alkali which performs a complete solubilization in which the pearl powder prepared in the preparation step is mixed with an alkali agent having a mass ratio of 20% or more of the protein content in the pearl powder and heated and stirred at a temperature of 100 ° C or higher for 2 hours or more to hydrolyze to the constituent unit of the peptide and amino acid Solubilization step; And an acidic aqueous solution containing hydrochloric acid, sulfuric acid, acetic acid, and citric acid to the solubilized product that has been reacted in the alkali solubilization step to neutralize the solution in the range of pH 8 to pH 9 to prevent precipitation of oligomeric or higher polymeric peptides .

In addition, the solubles and mineral water, which have been carried out in the stabilization step, are introduced into a high-pressure reactor having an atmosphere of carbon dioxide and concentrated under conditions of 30 atm and 0 ° C to 4 ° C to form a mixture of soluble and mineral water in a lattice structure The gas containing carbon dioxide is captured, so that the hydrate of the gas composed of carbon dioxide and volatile basic nitrogen introduced into the high-pressure reactor is removed by the hydration of the solubilized material, and the base nitrogen is removed, Concentration of cargo; A filtration and separation step of separating the hydrate forming the clay hydrate and the remaining soluble matter by transferring the base oil-removed soluble matter to the separator in the concentration step of the solubilization using the clathrate hydrate; And obtaining the separated concentrated solvate in the filtration and separation steps.

In addition, the concentration step of the solubilized product using the crystal hydrate is characterized by being concentrated to 30 minutes or more and 1 hour or less.

According to the present invention, the pearl protein, which is insoluble in nature, is subjected to alkali hydrolysis to be solubilized in the aqueous phase, and the pale protein is allowed to be concentrated in the high pressure reactor using the clathrate hydrate, Volatile basic nitrogen can be separated and removed conveniently by forming a hydrate with pure water to separate and concentrate only the concentrated pearl protein soluble solids, thereby increasing the processing yield of the insoluble pearl protein, which is difficult to dissolve in conventional water, It is effective in improving economic efficiency, lowering the price of high-priced consumers, commercializing them, and making the insoluble pearl protein actively used as a cosmetic material.

In addition, since conventional pearl proteins are insoluble in water, it is difficult to dissolve them in water. For solubilization, hydrolysis should be performed by adjusting the pH, and volatile basic nitrogen generated during protein hydrolysis is strongly retained in ammonia This difficulty is solved by performing the crystal hydration in the present invention to exclude volatile basic nitrogen and concentrate and recover only the choline protein-soluble substance. Therefore, it is possible to maximize the preservation of the physiological activity of the material and the application range of the material, This is effective in securing technological advancement in the market for cosmetics (cosmetics).

FIG. 1 is a flowchart of a method for preparing a pearl protein-soluble product using alkali solubilization and clathrate hydrate according to a preferred embodiment of the present invention.
FIG. 2 is a photograph showing that the gas hydrate is produced in the step of concentrating the solubilized material using the clathrate hydrate in the method of producing the pearl protein solubilization using the alkali solubilization and the clathrate hydrate according to the preferred embodiment of the present invention, and
FIG. 3 is a graph showing the separation and transfer of the excipient excluded in the gas hydrate reaction to the separator in the filtration and separation steps of the process for preparing the pearl protein solubilization using the alkali solubilization and the clathrate hydrate according to the preferred embodiment of the present invention to be.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the drawings, the same reference numerals are used to designate the same or similar components throughout the drawings. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear. In addition, the preferred embodiments of the present invention will be described below, but it is needless to say that the technical idea of the present invention is not limited thereto and can be variously modified by those skilled in the art.

FIG. 1 is a flowchart of a method 100 for preparing a pearl protein-soluble product using alkali solubilization and clathrate hydration according to a preferred embodiment of the present invention, and FIG. 2 is a flow chart of a method for preparing an alkali- FIG. 3 is a photograph showing the production of gas hydrate in the step (S40) of concentrating the solubilized product by using the crystallization hydrate of the process for producing the pearl protein-soluble product using the alkali solubilizing and clustering method according to the preferred embodiment of the present invention. FIG. 12 is a photograph showing that the solvate excluded from the gas hydrate reaction is transferred to a separator and separated in the filtration and separation step (S50) of the process for producing a pearl protein-soluble product using a hydrate of a slate.

The present invention relates to a process for preparing a pearl protein solubilization using alkali solubilization and clathrate hydration. More particularly, the present invention relates to a method for purifying an insoluble pearl protein by alkali hydrolysis and solubilizing the same in a water phase, and concentrating the solubilized product using a clathrate hydrate in a high-pressure reactor to remove ammonia from the pearl protein- Volatile basic nitrogen can be conveniently removed and formed by forming a hydrate with pure water to separate and concentrate the concentrated pearl protein soluble solids so that the processing yield of the insoluble pearl protein which is difficult to dissolve in conventional water can be increased, The present invention relates to a method for producing pearl protein-soluble carbohydrate using alkali solubilization and clathrate hydration, which can improve economical efficiency, commercialize low-priced poultry protein at low price and actively utilize insoluble pearl protein as a cosmetic material.

In addition, since conventional pearl proteins are insoluble in water, it is difficult to dissolve them in water. For solubilization, hydrolysis should be performed by adjusting the pH, and volatile basic nitrogen generated during protein hydrolysis is strongly retained in ammonia This difficulty is solved by performing the crystal hydration in the present invention to exclude volatile basic nitrogen and concentrate and recover only the choline protein-soluble substance. Therefore, it is possible to maximize the preservation of the physiological activity of the material and the application range of the material, This is effective in securing technological advancement in the market for cosmetics (cosmetics).

Referring to FIG. 1, a method for preparing a pearl protein solubilized product using alkali solubilization and clathrate hydration includes a preparation step (S10), an alkali solubilization step (S20), a stabilization step (S30), a solubilization using a crystallite hydrate A concentration step (S40), a filtration and separation step (S50), and an obtaining step (S60).

Hereinafter, the preparation step (S10) will be described.

The preparing step S10 is a step of preparing the pearl powder.

The pearl contains an ingredient such as amino acids and other organic substances, and has an excellent effect of whitening whitish pigment such as stain. In addition, eating and applying pearls will moisturize and moisturize the skin, prevent aging of the skin, and contain ingredients such as age-old spots, freckles, rashes, acne and skin boils.

These pearls are crushed and prepared into powder.

In the alkali solubilization step S20, an alkali agent having a mass ratio of the protein content of the pearlescent powder and the pearl powder prepared in the preparation step S10 is mixed and heated and stirred at a temperature of 100 ° C or more for 2 hours or longer to prepare a peptide, Lt; RTI ID = 0.0 > solubilization < / RTI >

More specifically, the alkali agent to be mixed in the alkali solubilization step (S20) is characterized by using a weak alkali or strong alkali comprising calcium carbonate, sodium carbonate, sodium bicarbonate, sodium hydroxide, potassium hydroxide.

In addition, if less than 20% of the alkaline agent of the protein content contained in the pearl powder is used in the alkali solubilization step (S20), incomplete solubilization leads to complete solubilization.

Here, complete solubilization means that the protein is hydrolyzed to the peptide and amino acid building block, and the incomplete solubilization is not hydrolyzed to the peptide and amino acid building block.

In the alkali solubilization step (S20), the reaction is preferably carried out at a temperature of at least 80 DEG C, mainly 100 DEG C, and the minimum reaction temperature required for complete hydrolysis of the protein is 80 DEG C, and the reaction is carried out at a temperature of 100 DEG C or lower Since oligomeric or higher polymeric peptides are mainly formed, it is difficult to complete solubilization. Therefore, it is preferable to carry out the reaction at a temperature of 100 캜 or higher.

Further, it is preferable to stir the solution at a temperature of 100 DEG C or more for 2 hours or more in the alkali solubilization step (S20) because it is the minimum reaction time required for complete hydrolysis of the protein.

In the stabilization step (S30), an acidic aqueous solution containing hydrochloric acid, sulfuric acid, acetic acid, and citric acid is added to the reacted solubilized product in the alkali solubilization step (S20) to neutralize the solution to a pH range of 8 or more to a pH of 9 or less to precipitate the oligomeric or higher oligomeric peptide .

In this case, in the stabilization step (S30), the acidic aqueous solution is added to neutralize the solution to a pH of from 8 to less than pH 9, whereby the polymeric peptides of oligomeric or higher oligomeric or higher than the unreacted ones in the neutral or acidic range below pH 7 may be precipitated in the aqueous solution, It can not be used as a cosmetic material (cosmetics) when the pH exceeds 9.

Referring to FIG. 2, in step S40 of concentrating solubles by using the crystallization hydrate, the solubilized material and mineral water in the stabilization step (S30) are introduced into a high-pressure reactor having an atmosphere of carbon dioxide, ° C, the gas containing carbon dioxide is trapped in the lattice structure of the mixture of the soluble and mineral water, so that the degree of hydration of the gas composed of carbon dioxide and volatile basic nitrogen introduced into the high-pressure reactor is available As moisture in the cargo is removed, the base nitrogen in which the ammonia odor remains is removed.

The hydrate is trapped in the space where the water molecules are formed by the hydrogen bonding, so that the gas containing carbon dioxide is trapped.

In addition, the concentration by the use of the clathrate hydration is controlled by controlling the composition of a specific gas and liquid, so that water as a subject molecule surrounds a gas, which is an object molecule, to form a crystal of a hydrate. Therefore, Since only pure water is consumed to combine with gas molecules to form a hydrate, it is possible to separate it from the solution including the gaseous substance present in the raw material solution, and the amount of water consumed to form the hydrate The concentration of the solution can be controlled by adjusting the amount of water consumed so that the concentration of the solution increases.

In the present invention, since hydrate is formed by the combination of base nitrogen remaining in ammonia odor generated by hydrolysis of pearl protein and mineral water which is pure water by using pure water hydration, pure water is consumed, It is possible to separate and concentrate the concentrated high-concentration pearl protein-soluble carbohydrate by easily removing ammonia from the base nitrogen due to the hydrolysis of the pearl protein, which is a conventional problem by improving the productivity and economical efficiency Of course.

Particularly, the reaction conditions for performing hydration such that carbon dioxide-containing gas is trapped in a mixture of the soluble substance and the mineral water put into the high-pressure reactor in the concentration step (S40) of the solubilization using the clathrate hydration is 30 atm Or more and 4 DEG C or less.

This is because, as the phase equilibrium condition for forming the hydrate, hydrate formation does not occur when the pressure is 30 atmospheres and the temperature is higher than 4 DEG C, and when the pressure is 30 atmospheres, especially below 0 DEG C, all of the reactants form hydrate and the exclusion of volatile basic nitrogen It is difficult to separate the interface for concentration.

In addition, it is preferable that the reaction time of the carbon dioxide hydrate in the concentration step (S40) of the solubilized material using the clathrate hydration is generally 30 minutes or more and 1 hour or less.

This is the induction time, which is determined by the phase equilibrium arrival time of the gas hydrate. If the reaction time is less than 30 minutes and the reaction time is more than 1 hour, it is not suitable for the phase equilibrium reaching time. It is difficult to remove the nitrogen and to separate the interface for concentration of the solute.

Referring to FIG. 3, the filtration and separation step (S50) includes a step of concentrating the solubilized material using the clathrate hydrate (S40). The solubilized material from which the base nitrogen has been removed is passed through a filter including a microfilter in a high- To separate the hydrate forming the clathrate hydrate and the remaining soluble matter from which the base nitrogen has been removed.

The step of obtaining (S60) is a step of obtaining a volatile basic nitrogen-removed solvate through the filter and the separator in the filtration and separation step (S50).

The thus-obtained concentrated soluble substance is used as a flame-retardant material (cosmetic material).

According to the present invention, in the technology for solubilizing the pearl protein, the processing yield is increased to improve the productivity and economical efficiency, commercialization of the pearl protein is lowered by lowering the consumer price, and active use of the pearl protein which is insoluble is made possible.

Further, according to the present invention, it is possible to preserve physiological activity inherent to the material and to maximize the application range of the material, thereby contributing to securing technological advancement in the market of the coconut material (cosmetics).

It will be apparent to those skilled in the art that various modifications, substitutions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims. will be. Therefore, the embodiments disclosed in the present invention and the accompanying drawings are intended to illustrate and not to limit the technical spirit of the present invention, and the scope of the technical idea of the present invention is not limited by these embodiments and the accompanying drawings . The scope of protection of the present invention should be construed according to the following claims, and all technical ideas within the scope of equivalents should be construed as falling within the scope of the present invention.

S10 - Preparatory phase
S20 - Alkali Solubilization Step
S30 - Stabilization step
S40 - Concentration of Soluble Compounds by Clathrate Hydration
S50 - Filtration and Separation Step
S60 - obtaining step
100 - Method for the preparation of pearl protein solubles by alkali solubilization and clathrate hydration

Claims (3)

A preparation step for preparing pearl powder;
Mixing the pearl powder prepared in the preparation step with an alkali agent having a mass ratio of 20% or more of the protein content in the pearl powder, heating and stirring the mixture at a temperature of 100 ° C or higher for 2 hours or more to complete the solubilization, An alkaline solubilization step in which base nitrogen is generated during the hydrolysis;
Adding an acidic aqueous solution containing hydrochloric acid, sulfuric acid, acetic acid, and citric acid to the solubilized product that has been reacted in the alkali solubilization step to neutralize the solution to a pH of 8 or more to a pH of 9 or less to prevent precipitation of oligomeric or higher polymeric peptides;
In order to remove the base nitrogen generated from the solubilized product after the stabilization step, the soluble material and water are put into a high-pressure reactor having an atmosphere of carbon dioxide and concentrated under conditions of 30 atm and 0 ° C to 4 ° C. Hydrate in which water forms a lattice structure and gas containing carbon dioxide in a lattice structure is carried out and water forms a hydrate by surrounding gas containing carbon dioxide and base nitrogen so that the base nitrogen contained in the solute is separated A step of concentrating the solubles using the clathrate hydrate;
A filtration and separation step of separating the hydrate forming the clathrate hydrate and the remaining soluble matter from which the base nitrogen has been removed by transferring the concentrated soluble matter to the separator in the concentration step of the solubilization using the clathrate hydration; And
The step of obtaining the concentrated solvate separated in the filtration and separation steps
Wherein the alkali soluble solubilizing and clathrate hydrate is selected from the group consisting of alkali solubilization and clathrate hydrate. delete The method according to claim 1,
The concentration step of the solvated cargo using the hydrate of the clathrate
Wherein the concentrate is concentrated from 30 minutes to 1 hour or less.

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