CN106631648B - A method of efficiently preparing compound amino acid - Google Patents
A method of efficiently preparing compound amino acid Download PDFInfo
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- CN106631648B CN106631648B CN201611022450.6A CN201611022450A CN106631648B CN 106631648 B CN106631648 B CN 106631648B CN 201611022450 A CN201611022450 A CN 201611022450A CN 106631648 B CN106631648 B CN 106631648B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B43/00—Formation or introduction of functional groups containing nitrogen
- C07B43/04—Formation or introduction of functional groups containing nitrogen of amino groups
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C11/00—Other nitrogenous fertilisers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
- C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
- C07C227/20—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters by hydrolysis of N-acylated amino-acids or derivatives thereof, e.g. hydrolysis of carbamates
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C277/00—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
- C07C277/08—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups of substituted guanidines
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/22—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of hydropolysulfides or polysulfides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/04—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members
- C07D207/10—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/16—Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/54—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
- C07D233/64—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms, e.g. histidine
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Processing Of Solid Wastes (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The present invention discloses a kind of method for efficiently preparing compound amino acid, comprising: takes feather, was crushed to 40-60 mesh, uses60Co- gamma-rays irradiates it;Step (1) be irradiated to treated that feather meal is hydrolyzed, obtains the first hydrolyzate;Ionic liquid is added in the first hydrolyzate that step (2) obtains, and under conditions of microwave heating, the reaction was continued 5-20min, filtering obtains the second hydrolyzate;The pH of the second hydrolyzate is adjusted to neutrality to get to compound amino acid;The method for efficiently preparing compound amino acid of the invention integrates irradiation technique, microwave heating technique and Ionic liquids technologies, molecule activation is made to the ionization excitation of feather first with the ray of irradiation, on the other hand using ionic liquid to the higher absorbability of microwave and to the good dissolubility of molecular substance, greatly accelerate the speed of reaction, effectively improve percent hydrolysis, it is a kind of method for hydrolysis of new and effective green, there is huge application prospect.
Description
Technical field
The present invention relates to amino acid preparation technical fields, and in particular to a method of efficiently prepare compound amino acid.
Background technique
China is the most country of world population, consumes the birds such as a large amount of chicken and duck goose every year;The fowl generated in 2015
Class feather reaches 800,000 tons or more, but these feather wastes, is only made into pillow on a small quantity, by pad, feather fan, shuttlecock
Deng, be largely simply discarded, not only cause water pollution, generate unpleasant or even pernicious gas, be also easy to cause mosquito, bacterium,
Virus is bred, and is caused damages to human health.
According to surveying and determination, the crude protein content of feather keratin is about 80% or more, and amino acid content is 70% or more, also containing normal
Secondary element, microelement, vitamin and some unknown growth factor;Therefore feather keratin waste passes through processing appropriate
With very extensive purposes, a kind of effective method is found, the higher product of value is converted by wastes such as chicken feathers, has
Major and immediate significance.
Feather hydrolysis industrialization generallys use acid and alkali hydrolysis method, but the time that this method expends is longer, consumes energy higher, and water
A large amount of waste liquids are generated after solution, it is difficult, easily cause secondary pollution.In view of the deficiency of this method, it is badly in need of one in the market in protection ring
Waste feathers are effectively hydrolyzed into the new method of amino acid by border in the case where economizing on resources, for the utilization of people's deep development, become
Waste be changed into values.
Summary of the invention
It is an object of the present invention to provide a kind of method for efficiently preparing compound amino acid, this method collection radiation treatment,
On the one hand the method for microwave heating and ionic liquid three make molecule activation to the ionization excitation of substance using ray in one,
On the other hand using ionic liquid to the higher absorbability of microwave and to the good solubility of macromolecular substances, greatly
The fast speed of reaction, and then form a kind of method for hydrolysis of new efficient green.
The technical scheme to solve the above technical problems is that providing a kind of side for efficiently preparing compound amino acid
Method, comprising the following steps:
(1) feather is taken, 40-60 mesh was crushed to, is used60Co- gamma-rays irradiates it;
(2) step (1) be irradiated to treated that feather meal is hydrolyzed, obtains the first hydrolyzate;
(3) ionic liquid is added in the first hydrolyzate that step (2) obtains, and under conditions of microwave heating, continues
5-20min is reacted, filtering obtains the second hydrolyzate;
(4) pH of the second hydrolyzate of adjusting arrives compound amino acid to neutrality.
Based on the above technical solution, the present invention can also be improved as follows.
Further, in step (1), when using irradiation treatment method, irradiation dose 150-250KGy, radiation dose rate is
20-50Gy/min。
Further, the detailed process of step (2) are as follows:
It is irradiated in step (1) and the hydrochloric acid that concentration is 6-8mol/L is added in treated feather meal, be stirred, and added
Heat obtains the first hydrolyzate to 40-70 DEG C of hydrolysis 5-20min;Wherein, the quality volume of feather meal and hydrochloric acid is 1:5-8.
Further, the detailed process of step (3) are as follows:
The first hydrolyzate that step (2) obtains is placed in microwave reactor, and the first hydrolyzate weight is added
The ionic liquid 1-butyl-3-methyl imidazolium bromide of 0.3%-0.7%, under conditions of microwave heating, the reaction was continued 5-20min,
Obtain the second hydrolyzate;Wherein, microwave heating power is 600-700W.
Further, in step (4), be added saturated calcium hydroxide solution adjust the second hydrolyzate pH value to neutrality to get
To compound amino acid.
When further, using irradiation treatment method, irradiation dose 200KGy, radiation dose rate 25Gy/min.
Further, the detailed process of step (2) are as follows:
It is irradiated in step (1) and the hydrochloric acid that concentration is 6mol/L is added in treated feather meal, be stirred, and heat
To 50 DEG C of hydrolysis 8min, the first hydrolyzate is obtained;Wherein, the quality volume of feather meal and hydrochloric acid is 1:5.
The first hydrolyzate that step (2) obtains is placed in microwave reactor, and the first hydrolyzate weight is added
0.5% ionic liquid 1-butyl-3-methyl imidazolium bromide, under conditions of microwave heating, the reaction was continued 8min obtains second
Hydrolyzate;Wherein, microwave heating power is 640W.
Contain 17 kinds of amino acid in the compound amino acid obtained using above-mentioned preparation method.
Wherein, irradiation technique is the effective ways of degradation high polymer, it is to utilize process60Co or37The γ that Cs is generated is penetrated
The ionising radiations actinisms such as the electron beam that line, X-ray and electron accelerator generate make substance that physics occur, change in substance
And biological effect;It is proved to be a kind of cleaning, efficient, free of contamination Physical Processing side by years of researches and application
Method.
Microwave heating technique has obtained extensively because it has many advantages, such as that energy saving and heating treatment time is short in many fields
General research and application;Traditional heating is from outward appearance to inner essence heated by radiation, convection current and conduction;With traditional heating mode phase
Than, microwave heating has the following characteristics that 1. efficiently quick and penetrability is strong: microwave can be directed through into inside material,
Material inside and outside equilibrium is heated, to substantially reduce heating time, saves the energy;2. selectivity heating: different material is micro-
Wave degree of absorption is different;In general, material molecular polarity is stronger, easier absorption microwave;3. heating reaction is fast, convenient for control
System: the time lag of microwave heating is extremely short, and heating and heating are almost synchronous;Microwave source is controlled by power supply, and it is convenient to operate;4. heat source with plus
Hot material is not directly contacted with, less pollution.
Ionic liquid has many good qualities as novel green solvent: 1. steam forces down, is non-volatile, is nonflammable;2. liquid
Range is wide, good electric conductivity and wider potential window;3. good dissolubility energy;Room-temperature ion liquid physical efficiency selectivity it is molten
Many inorganic matters, organo-metallic compound, high molecular material, protein and enzyme etc. are solved, is the good solvent of many substances;④
Toxicity is low, recoverable;Relative to traditional organic solvent, there is lower environmental toxicity and influence, be easier to be recovered benefit
With it is latent that these properties make ionic liquid at room temperature have a wide range of applications in the fields such as electrochemistry, organic synthesis, catalysis reaction
Power is 21st century ideal green solvent.
Of the invention efficiently prepares in the method for compound amino acid, handles first with irradiation technique feather, spoke
According to the process for being an energy transmission, it makes its molecule activation to feather ionization excitation using ray, and then feather is made to occur one
Physics, the chemical change of series, destroy its original macromolecular structure, finally make mass degradation in feather, polymerization, crosslinking or
Denaturation;After the radiation treatment, feather can quickly absorb microwave energy, preferably dissolve in ionic liquid, so that whole
A reaction time shortens, and percent hydrolysis greatly improves.
The present invention heats the feather meal after radiation treatment using microwave heating technique, is passing through radiation treatment
So that on the basis of feather meal molecule activation is to be easy to absorb heat, microwave heating technique is more efficiently fast to the heating of substance
Speed and penetrability is strong: microwave can be directed through into inside material, be heated to material inside and outside equilibrium, in radiation treatment and micro-
On the basis of Wave heating technology combines, heating time is substantially reduced, saves the energy.
The present invention carries out substance using ionic liquid on the basis of using radiation treatment and microwave heating, also molten
Solution, because ionic liquid has good dissolubility energy;The many inorganic matters of dissolution, the You Jijin of room-temperature ion liquid physical efficiency selectivity
Belong to compound, high molecular material, protein and enzyme etc., and still a kind of toxicity is low, green solvent of recoverable, it should be from
The addition of sub- liquid substantially increases the solution rate of solute, to further improve reaction speed.
Method collection irradiation technique, microwave heating technique and the Ionic liquids technologies for efficiently preparing compound amino acid of the invention
In one, molecule activation is made to the ionization excitation of feather first with the ray of irradiation, on the other hand using ionic liquid to micro-
The higher absorbability of wave and good dissolubility to molecular substance, greatly accelerate the speed of reaction, effectively mention
High percent hydrolysis, is a kind of method for hydrolysis of new and effective green, with huge application prospect.
The present invention is established for the first time using radiation treatment feather, microwave heating coupled ion liquid as microwave absorption medium
Waste feathers efficiently prepare amino acid hydrolyticsolution innovative technology, (the conversion ratio compared with the widely used sulfuric acid process of current industry
60%), this technology conversion ratio has been obviously improved 20% or more;Radiation treatment is added, so that the whole flow process reaction time greatly shortens,
Effectively overcoming conventional hydrolysis feather, existing hydrolysis effect is bad in the process, hydrolysis rate is slow, causes secondary environmental pollution
The deficiencies of;This research can be widely used in the industrial production of amino acid and the preparation of amino acid fertilizer.
Specific embodiment
The present invention will be described in detail below, and the given examples are served only to explain the present invention, is not intended to limit the present invention
Range.
Embodiment 1:
A method of efficiently preparing compound amino acid, comprising the following steps:
(1) feather is taken, dry, pulverize to 40 meshes are crossed, use60Co- gamma-rays irradiates it, and irradiation dose is
200KGy, radiation dose rate 25Gy/min;
(2) it is irradiated in step (1) and the hydrochloric acid that concentration is 6mol/L is added in treated feather meal, be stirred, and
50 DEG C of hydrolysis 10min are heated to, the first hydrolyzate is obtained;Wherein, the quality volume of feather meal and hydrochloric acid is 1:5;
(3) the first hydrolyzate that step (2) obtains is placed in microwave reactor, and the first hydrolyzate weight 0.5% is added
Ionic liquid 1-butyl-3-methyl imidazolium bromide, under conditions of microwave heating, the reaction was continued 10min, after cooling, warp
Filtering, obtains the second hydrolyzate;Wherein, microwave heating power is 640W;
(4) saturated calcium hydroxide solution is added in the second obtained hydrolyzate, adjusts the pH value of the second hydrolyzate to 7,
Filtering, obtains compounded amino acid hydrolysis liquid;
Part compounded amino acid hydrolysis liquid sample is taken to measure total nitrogen content in sample through Kjeldahl's method, through formol titration
Amino acid nitrogen content in test sample, obtaining compound amino acid conversion ratio made from the present embodiment is 82.97%;The compound ammonia
Contain 17 kinds of amino acid in base acid, measure its concrete composition ingredient through automatic amino acid analyzer analysis and be shown in Table 1:
1 compound amino acid of table forms (g/L)
Embodiment 2:
A method of efficiently preparing compound amino acid, comprising the following steps:
(1) feather is taken, dry, pulverize to 60 meshes are crossed, use60Co- gamma-rays irradiates it, and irradiation dose is
250KGy, radiation dose rate 20Gy/min;
(2) it is irradiated in step (1) and the hydrochloric acid that concentration is 8mol/L is added in treated feather meal, be stirred, and
40 DEG C of hydrolysis 5min are heated to, the first hydrolyzate is obtained;Wherein, the quality volume of feather meal and hydrochloric acid is 1:6;
(3) the first hydrolyzate that step (2) obtains is placed in microwave reactor, and the first hydrolyzate weight 0.3% is added
Ionic liquid 1-butyl-3-methyl imidazolium bromide, under conditions of microwave heating, the reaction was continued 5min passes through after cooling
Filter, obtains the second hydrolyzate;Wherein, microwave heating power is 700W;
(4) saturated calcium hydroxide solution is added in the second obtained hydrolyzate, adjusts the pH value of the second hydrolyzate to 7,
Filtering, obtains compounded amino acid hydrolysis liquid;
Part compounded amino acid hydrolysis liquid sample is taken to measure total nitrogen content in sample through Kjeldahl's method, through formol titration
Amino acid nitrogen content in test sample, obtaining compound amino acid conversion ratio made from the present embodiment is 85.3%;The compounded amino
Contain 17 kinds of amino acid in acid, measure its concrete composition ingredient through automatic amino acid analyzer analysis and be shown in Table 2:
2 compound amino acid of table forms (g/L)
Amino acid composition | Irradiation collaboration microwave-ionic liquid | Sulfuric acid process |
Aspartic acid | 4.97 | 3.86 |
Threonine | 3.64 | 2.41 |
Serine | 8.05 | 5.82 |
Glutamic acid | 6.56 | 6.51 |
Proline | 7.12 | 4.31 |
Glycine | 6.32 | 3.44 |
Alanine | 6.97 | 4.07 |
Cysteine | 2.03 | 1.16 |
Valine | 3.64 | 2.54 |
Methionine | 1.52 | 0.08 |
Isoleucine | 2.26 | 2.17 |
Leucine | 3.86 | 3.46 |
Tyrosine | 1.56 | 1.34 |
Phenylalanine | 2.65 | 2.24 |
Lysine | 1.97 | 0.66 |
Histidine | 1.65 | 0.06 |
Arginine | 1.45 | 1.58 |
Total amino acid content | 66.22 | 45.71 |
Embodiment 3:
A method of efficiently preparing compound amino acid, comprising the following steps:
(1) feather is taken, dry, pulverize to 50 meshes are crossed, use60Co- gamma-rays irradiates it, and irradiation dose is
150KGy, radiation dose rate 50Gy/min;
(2) it is irradiated in step (1) and the hydrochloric acid that concentration is 7mol/L is added in treated feather meal, be stirred, and
60 DEG C of hydrolysis 8min are heated to, the first hydrolyzate is obtained;Wherein, the quality volume of feather meal and hydrochloric acid is 1:8;
(3) the first hydrolyzate that step (2) obtains is placed in microwave reactor, and hydrolysate weight 0.7% is added
Ionic liquid 1-butyl-3-methyl imidazolium bromide, under conditions of microwave heating, the reaction was continued, and 8min passes through after cooling
Filter, obtains the second hydrolyzate;Wherein, microwave heating power is 600W;
(4) saturated calcium hydroxide solution is added in the second obtained hydrolyzate, adjusts the pH value of the second hydrolyzate to 7,
Filtering, obtains compounded amino acid hydrolysis liquid;
Part compounded amino acid hydrolysis liquid sample is taken to measure total nitrogen content in sample through Kjeldahl's method, through formol titration
Amino acid nitrogen content in test sample, obtaining compound amino acid conversion ratio made from the present embodiment is 83.49%;The compound ammonia
Contain 17 kinds of amino acid in base acid, measure its concrete composition ingredient through automatic amino acid analyzer analysis and be shown in Table 3:
3 compound amino acid of table forms (g/L)
Amino acid composition | Irradiation collaboration microwave-ionic liquid | Sulfuric acid process |
Aspartic acid | 5.01 | 3.86 |
Threonine | 4.61 | 2.41 |
Serine | 6.94 | 5.82 |
Glutamic acid | 6.35 | 6.51 |
Proline | 6.58 | 4.31 |
Glycine | 6.07 | 3.44 |
Alanine | 6.84 | 4.07 |
Cysteine | 3.02 | 1.16 |
Valine | 3.54 | 2.54 |
Methionine | 0.98 | 0.08 |
Isoleucine | 1.45 | 2.17 |
Leucine | 3.81 | 3.46 |
Tyrosine | 1.07 | 1.34 |
Phenylalanine | 1.85 | 2.24 |
Lysine | 1.53 | 0.66 |
Histidine | 1.78 | 0.06 |
Arginine | 1.34 | 1.58 |
Total amino acid content | 62.77 | 45.71 |
Embodiment 4:
A method of efficiently preparing compound amino acid, comprising the following steps:
(1) feather is taken, dry, pulverize to 60 meshes are crossed, use60Co- gamma-rays irradiates it, and irradiation dose is
180KGy, radiation dose rate 40Gy/min;
(2) it is irradiated in step (1) and the hydrochloric acid that concentration is 8mol/L is added in treated feather meal, be stirred, and
70 DEG C of hydrolysis 20min are heated to, the first hydrolyzate is obtained;Wherein, the quality volume of feather meal and hydrochloric acid is 1:8;
(3) the first hydrolyzate that step (2) obtains is placed in microwave reactor, and the first hydrolyzate weight 0.6% is added
Ionic liquid 1-butyl-3-methyl imidazolium bromide, under conditions of microwave heating, the reaction was continued 20min, after cooling, warp
Filtering, obtains the second hydrolyzate;Wherein, microwave heating power is 680W;
(4) saturated calcium hydroxide solution is added in the second obtained hydrolyzate, adjusts the pH value of the second hydrolyzate to 7,
Filtering, obtains compounded amino acid hydrolysis liquid;
Part compounded amino acid hydrolysis liquid sample is taken to measure total nitrogen content in sample through Kjeldahl's method, through formol titration
Amino acid nitrogen content in test sample, obtaining compound amino acid conversion ratio made from the present embodiment is 84.61%;The compound ammonia
Contain 17 kinds of amino acid in base acid, measure its concrete composition ingredient through automatic amino acid analyzer analysis and be shown in Table 4:
4 compound amino acid of table forms (g/L)
Amino acid composition | Irradiation collaboration microwave-ionic liquid | Sulfuric acid process |
Aspartic acid | 5.36 | 3.86 |
Threonine | 3.54 | 2.41 |
Serine | 5.84 | 5.82 |
Glutamic acid | 6.78 | 6.51 |
Proline | 5.95 | 4.31 |
Glycine | 6.51 | 3.44 |
Alanine | 6.74 | 4.07 |
Cysteine | 4.16 | 1.16 |
Valine | 4.08 | 2.54 |
Methionine | 1.32 | 0.08 |
Isoleucine | 1.46 | 2.17 |
Leucine | 3.92 | 3.46 |
Tyrosine | 2.16 | 1.34 |
Phenylalanine | 1.22 | 2.24 |
Lysine | 1.69 | 0.66 |
Histidine | 1.62 | 0.06 |
Arginine | 1.47 | 1.58 |
Total amino acid content | 63.82 | 45.71 |
Contained it can be seen from the data in above table using the amino acid in the compound amino acid of the method for the present invention preparation
Amount is greatly enhanced relative to existing sulfuric acid law technology, therefore, is greatly improved using method percent hydrolysis of the invention, so that
Effective component in feather can be extracted farthest, simultaneously as the first time in a creative way use radiation treatment,
The technology that microwave heating and ionic liquid combine, so that the reaction time greatly shortens, extraction efficiency is significantly improved, because
This, method of the invention has huge application prospect.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of method for efficiently preparing compound amino acid, characterized in that the following steps are included:
(1) feather is taken, 40-60 mesh was crushed to, is used60Co- gamma-rays irradiates it;Irradiation dose is 150-
250KGy, radiation dose rate 20-50Gy/min;
(2) step (1) be irradiated to treated that feather meal is hydrolyzed, obtains the first hydrolyzate;Place is irradiated in step (1)
The hydrochloric acid that concentration is 6-8mol/L is added in feather meal after reason, is stirred, and be heated to 40-70 DEG C of hydrolysis 5-
20min obtains the first hydrolyzate;Wherein, the quality volume of feather meal and hydrochloric acid is 1:5-8;
(3) ionic liquid is added in the first hydrolyzate that step (2) obtains, and under conditions of microwave heating, the reaction was continued
5-20min, filtering, obtains the second hydrolyzate;The first hydrolyzate that step (2) obtains is placed in microwave reactor, and is added
The ionic liquid 1-butyl-3-methyl imidazolium bromide of the first hydrolyzate weight 0.3%-0.7%, in microwave heating
Under the conditions of, the reaction was continued 5-20min obtains the second hydrolyzate;Wherein, microwave heating power is 600-700W;
(4) pH of the second hydrolyzate of adjusting arrives compound amino acid to neutrality.
2. the method according to claim 1 for efficiently preparing compound amino acid, characterized in that in step (4), saturation is added
The pH value of calcium hydroxide solution the second hydrolyzate of adjusting arrives compound amino acid to neutrality.
3. the method according to claim 1 for efficiently preparing compound amino acid, characterized in that use irradiation treatment method
When, irradiation dose 200KGy, radiation dose rate 25Gy/min.
4. the method according to claim 1 for efficiently preparing compound amino acid, characterized in that the detailed process of step (2)
Are as follows:
It is irradiated in step (1) and the hydrochloric acid that concentration is 6mol/L is added in treated feather meal, be stirred, and be heated to 50
DEG C hydrolysis 8min, obtain the first hydrolyzate;Wherein, the quality volume of feather meal and hydrochloric acid is 1:5.
5. the method according to claim 1 for efficiently preparing compound amino acid, characterized in that the detailed process of step (3)
Are as follows:
The first hydrolyzate that step (2) obtains is placed in microwave reactor, and the first hydrolyzate weight 0.5% is added
Ionic liquid 1-butyl-3-methyl imidazolium bromide, under conditions of microwave heating, the reaction was continued 8min obtains the second hydrolysis
Liquid;Wherein, microwave heating power is 640W.
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CN110484429A (en) * | 2019-09-19 | 2019-11-22 | 安徽小溪生态科技发展有限公司 | Microwave hydrolysis waste plant protein resource prepares compound amino acid syrup technique and equipment |
CN111587761A (en) * | 2020-04-15 | 2020-08-28 | 安徽小溪生态科技发展有限公司 | Method for preparing crop culture medium by utilizing microwave hydrolysis of livestock waste resources |
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