CN106631648A - Method for efficiently preparing compound amino acids - Google Patents
Method for efficiently preparing compound amino acids Download PDFInfo
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- CN106631648A CN106631648A CN201611022450.6A CN201611022450A CN106631648A CN 106631648 A CN106631648 A CN 106631648A CN 201611022450 A CN201611022450 A CN 201611022450A CN 106631648 A CN106631648 A CN 106631648A
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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 invention discloses a method for efficiently preparing compound amino acids. The method for efficiently preparing the compound amino acids comprises the following steps: taking feathers, grinding until sieving with a 40-60 mesh sieve, and using <60>Co-gamma rays to carry out irradiation on sieved feather powder; hydrolyzing the feather powder which is subjected to irradiation in the step (1) to obtain first hydrolysate; adding ionic liquid to the first hydrolysate obtained in the step (2), and continuously reacting for 5 to 20min under the conditions of microwave heating, and filtering to obtain second hydrolysate; adjusting the pH of the second hydrolysate to be neutral, thus obtaining the compound amino acids; the method for efficiently preparing the compound amino acids disclosed by the invention integrates irradiation technologies, microwave heating technologies and ionic liquid technologies, firstly, the irradiation rays are used for carrying out ionization excitation on the feathers to activate molecules, on the other hand, the ionic liquid has a higher absorptive capacity for microwave and good solubility for molecular substances to greatly accelerate the reaction rate, and effectively improve the hydrolysis rate, so that the method for efficiently preparing the compound amino acids is a novel high-efficiency and green hydrolysis method and has great application prospects.
Description
Technical field
The present invention relates to amino acid preparing technical field, and in particular to a kind of method for efficiently preparing compound amino acid.
Background technology
China is the most country of world population, and the birds such as substantial amounts of chicken and duck goose are consumed every year；The fowl for producing for 2015
Class feather reaches more than 800,000 tons, but these feather wastes, be only made on a small quantity pillow, padded, feather fan, shuttlecock
Deng, major part is simply discarded, and not only causes water pollution, produces unpleasant or even pernicious gas, be also easy to cause mosquito, bacterium,
Virus is grown, and is worked the mischief to human health.
According to surveying and determination, the crude protein content of feather keratin is about more than 80%, amino acid content more than 70%, also containing normal
Secondary element, trace element, vitamin and some UGFs；Therefore feather keratin discarded object is through appropriate process
With quite varied purposes, a kind of effective method is found, chicken feather the like waste is converted into the higher product of value, had
Major and immediate significance.
Feather hydrolysis industrialization generally adopts acid and alkali hydrolysis method, but the time that the method expends is longer, consumes energy higher, and water
A large amount of waste liquids are produced after solution, it is difficult, easily cause secondary pollution.In view of the deficiency of the method, is badly in need of one in protection ring on market
Border, waste feathers are effectively hydrolyzed into the new method of amino acid in the case of economizing on resources, and for the utilization of people's deep development, are become
Waste be changed into values.
The content of the invention
It is an object of the present invention to provide a kind of method for efficiently preparing compound amino acid, the method collection radiation treatment, microwave
The method of heating and ionic liquid three is in one, and on the one hand the ionization using ray to material is excited makes molecule activation, another
Aspect utilizes higher absorbability and good solubility to macromolecular substances of the ionic liquid to microwave, greatly accelerates
The speed of reaction, and then form a kind of method for hydrolysis of new efficient green.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：A kind of side for efficiently preparing compound amino acid is provided
Method, comprises the following steps：
（1）Feather is taken, 40-60 mesh sieves were crushed to, is adopted60Co- gamma-rays carries out irradiation to it；
（2）By step（1）Feather meal after irradiated process is hydrolyzed, and obtains the first hydrolyzate；
（3）In step（2）Ionic liquid is added in the first hydrolyzate for obtaining, and under conditions of heating using microwave, continues to react
5-20min, filters, and obtains the second hydrolyzate；
（4）The pH of the second hydrolyzate is adjusted to neutrality, that is, obtains compound amino acid.
On the basis of above-mentioned technical proposal, the present invention can also do following improvement.
Further, step（1）In, during using irradiation treatment method, irradiation dose is 150-250KGy, and radiation dose rate is
20-50Gy/min。
Further, step（2）Detailed process be：
In step（1）Concentration is added in feather meal after irradiated process for the hydrochloric acid of 6-8mol/L, stirring mixing, and be heated to
40-70 DEG C of hydrolysis 5-20min, obtains the first hydrolyzate；Wherein, feather meal and the quality volume of hydrochloric acid are 1：5-8.
Further, step（3）Detailed process be：
By step（2）The first hydrolyzate for obtaining is placed in microwave reactor, and adds the first hydrolyzate weight 0.3%-
0.7% ionic liquid 1-butyl-3-methyl imidazolium bromide, under conditions of heating using microwave, continues to react 5-20min, obtains the
Two hydrolyzates；Wherein, heating using microwave power is 600-700W.
Further, step（4）In, add saturated calcium hydroxide solution to adjust the pH value of the second hydrolyzate to neutrality, obtain final product
To compound amino acid.
When further, using irradiation treatment method, irradiation dose is 200KGy, and radiation dose rate is 25Gy/min.
Further, step（2）Detailed process be：
In step（1）Concentration is added in feather meal after irradiated process for the hydrochloric acid of 6mol/L, stirring mixing, and it is heated to 50
DEG C hydrolysis 8min, obtain the first hydrolyzate；Wherein, feather meal and the quality volume of hydrochloric acid are 1：5.
By step（2）The first hydrolyzate for obtaining is placed in microwave reactor, and adds the first hydrolyzate weight
0.5% ionic liquid 1-butyl-3-methyl imidazolium bromide, under conditions of heating using microwave, continues to react 8min, obtains second
Hydrolyzate；Wherein, heating using microwave power is 640W.
Using in the compound amino acid that above-mentioned preparation method is obtained contain 17 kinds of amino acid.
Wherein, irradiation technique is the effective ways of degraded high polymer, and it is using process60Co or37The γ that Cs is produced is penetrated
The ionising radiation actinisms such as the electron beam that line, X-ray and electron accelerator are produced make material physics occur, change in material
Learn and biological effect；It is proved to be a kind of cleaning, efficient, free of contamination Physical Processing side through years of researches and application
Method.
Microwave heating technique has the advantages that energy saving and heating treatment time is short has obtained extensively in many fields because of it
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 heating using microwave has the characteristics that：1. it is efficiently quick and penetrability is strong：Microwave can be directed through entering inside material,
It is balanced to material inside and outside to heat, so as to substantially reduce the heat time, save the energy；2. selective heating：Different material is micro-
Ripple degree of absorption is different；In general, material molecular polarity is stronger, easier absorption microwave；3. heating response is fast, is easy to control
System：The time lag of heating using microwave is extremely short, heats almost synchronous with intensification；Microwave source is by power supply, simple operation；4. thermal source with plus
Hot material is not directly contacted with, less pollution.
Ionic liquid has many good qualities as novel green solvent：1. steam force down, it is non-volatile, nonflammable；2. liquid
Wide ranges, good electric conductivity and wider potential window；3. good dissolubility energy；Room-temperature ion liquid physical efficiency is selectively molten
Many inorganic matters, organo-metallic compound, macromolecular material, protein and enzyme etc. are solved, is the good solvent of many materials；④
Toxicity is low, recoverable；Relative to traditional organic solvent, with lower environmental toxicity and impact, it is more easy to be recovered profit
With it is latent that these properties cause ionic liquid at room temperature to have a wide range of applications in the fields such as electrochemistry, organic synthesis, catalytic reaction
Power, is 21st century preferable green solvent.
In the method for efficiently preparing compound amino acid of the present invention, feather is processed first with irradiation technique, spoke
According to the process for being an energy transmission, it is excited to feather ionization using ray and makes its molecule activation, and then makes feather occur one
Physics, the chemical change of series, destroys its original macromolecular structure, finally make mass degradation in feather, polymerization, be crosslinked or
Denaturation；After the radiation treatment, feather can quickly absorb microwave energy, preferably dissolve in ionic liquid so that whole
The individual reaction time shortens, and percent hydrolysis is greatly improved.
The present invention is heated using microwave heating technique to the feather meal after radiation treatment, through radiation treatment
So that feather meal molecule activation is so as to be easy to absorb on the basis of heat, heating of the microwave heating technique to material is more efficiently fast
Speed and penetrability is strong：Microwave can be directed through entering inside material, balanced to material inside and outside to heat, in radiation treatment and micro-
On the basis of Wave heating technology combines, the heat time is substantially reduced, save the energy.
The present invention is also carried out molten using ionic liquid on the basis of using radiation treatment and heating using microwave to material
Solution, because ionic liquid has good dissolubility energy；Room-temperature ion liquid physical efficiency selectively dissolves many inorganic matters, You Jijin
Category compound, macromolecular material, protein and enzyme etc., and also be that a kind of toxicity is low, recoverable green solvent, should be from
The addition of sub- liquid substantially increases the dissolution velocity of solute, so as to further increase reaction speed.
The method collection irradiation technique, microwave heating technique and the Ionic liquids technologies that efficiently prepare compound amino acid of the present invention
In one, ionization of the ray to feather first with irradiation is excited and makes molecule activation, on the other hand using ionic liquid to micro-
The higher absorbability and the good dissolubility to molecular substance of ripple, greatly accelerates the speed of reaction, effectively carries
High percent hydrolysis, is a kind of method for hydrolysis of new and effective green, with huge application prospect.
The present invention is established first using radiation treatment feather, heating using microwave coupled ion liquid as microwave absorption medium
Waste feathers efficiently prepare amino acid hydrolyticsolution innovative technology, compared with the widely used sulfuric acid process of current industry（Conversion ratio
60%）, this technology conversion ratio has been obviously improved more than 20%；Add radiation treatment so that the whole flow process reaction time greatly shortens,
Effectively overcome that hydrolysis effect present in conventional hydrolysis feather process is good, hydrolysis rate slow, cause secondary environmental pollution
Deng not enough；This research can be widely used in the industrial production of amino acid, and the preparation of amino acid fertilizer.
Specific embodiment
Hereinafter describe the present invention, example is served only for explaining the present invention, is not intended to limit the present invention
Scope.
Embodiment 1：
A kind of method for efficiently preparing compound amino acid, comprises the following steps：
（1）Feather is taken, be dry, pulverize to 40 mesh sieves are crossed, adopted60Co- gamma-rays carries out irradiation to it, and irradiation dose is
200KGy, radiation dose rate is 25Gy/min；
（2）In step（1）Concentration is added in feather meal after irradiated process for the hydrochloric acid of 6mol/L, stirring mixing, and heat
To 50 DEG C of hydrolysis 10min, the first hydrolyzate is obtained；Wherein, feather meal and the quality volume of hydrochloric acid are 1：5；
（3）By step（2）The first hydrolyzate for obtaining is placed in microwave reactor, and add the first hydrolyzate weight 0.5% from
Sub- liquid 1- butyl -3- methylimidazole bromides, under conditions of heating using microwave, continue to react 10min, and after cooling, Jing is filtered,
Obtain the second hydrolyzate；Wherein, heating using microwave power is 640W；
（4）Saturated calcium hydroxide solution is added in the second hydrolyzate for obtaining, the pH value of the second hydrolyzate is adjusted to 7, is filtered,
Obtain compounded amino acid hydrolysis liquid；
Take part compounded amino acid hydrolysis liquid sample Jing Kjeldahl's methods and measure total nitrogen content in sample, the detection of Jing formol titrations
Amino acid nitrogen content in sample, obtains compound amino acid conversion ratio obtained in the present embodiment for 82.97%；The compound amino acid
In contain 17 kinds of amino acid, Jing automatic amino acid analyzers analysis determine its concrete composition composition be shown in Table 1：
The compound amino acid of table 1 is constituted（g/L）
Embodiment 2：
A kind of method for efficiently preparing compound amino acid, comprises the following steps：
（1）Feather is taken, be dry, pulverize to 60 mesh sieves are crossed, adopted60Co- gamma-rays carries out irradiation to it, and irradiation dose is
250KGy, radiation dose rate is 20Gy/min；
（2）In step（1）Concentration is added in feather meal after irradiated process for the hydrochloric acid of 8mol/L, stirring mixing, and heat
To 40 DEG C of hydrolysis 5min, the first hydrolyzate is obtained；Wherein, feather meal and the quality volume of hydrochloric acid are 1：6；
（3）By step（2）The first hydrolyzate for obtaining is placed in microwave reactor, and add the first hydrolyzate weight 0.3% from
Sub- liquid 1- butyl -3- methylimidazole bromides, under conditions of heating using microwave, continue to react 5min, and after cooling, Jing is filtered,
Obtain the second hydrolyzate；Wherein, heating using microwave power is 700W；
（4）Saturated calcium hydroxide solution is added in the second hydrolyzate for obtaining, the pH value of the second hydrolyzate is adjusted to 7, is filtered,
Obtain compounded amino acid hydrolysis liquid；
Take part compounded amino acid hydrolysis liquid sample Jing Kjeldahl's methods and measure total nitrogen content in sample, the detection of Jing formol titrations
Amino acid nitrogen content in sample, obtains compound amino acid conversion ratio obtained in the present embodiment for 85.3%；In the compound amino acid
Containing 17 kinds of amino acid, the analysis of Jing automatic amino acid analyzers determines its concrete composition composition and is shown in Table 2：
The compound amino acid of table 2 is constituted（g/L）
| Amino acid is constituted | Irradiation cooperates with 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 kind of method for efficiently preparing compound amino acid, comprises the following steps：
（1）Feather is taken, be dry, pulverize to 50 mesh sieves are crossed, adopted60Co- gamma-rays carries out irradiation to it, and irradiation dose is
150KGy, radiation dose rate is 50Gy/min；
（2）In step（1）Concentration is added in feather meal after irradiated process for the hydrochloric acid of 7mol/L, stirring mixing, and heat
To 60 DEG C of hydrolysis 8min, the first hydrolyzate is obtained；Wherein, feather meal and the quality volume of hydrochloric acid are 1：8；
（3）By step（2）The first hydrolyzate for obtaining is placed in microwave reactor, and adds the ion of hydrolysate weight 0.7%
Liquid 1- butyl -3- methylimidazole bromides, under conditions of heating using microwave, continue to react 8min, and after cooling, Jing is filtered, and is obtained
To the second hydrolyzate；Wherein, heating using microwave power is 600W；
（4）Saturated calcium hydroxide solution is added in the second hydrolyzate for obtaining, the pH value of the second hydrolyzate is adjusted to 7, is filtered,
Obtain compounded amino acid hydrolysis liquid；
Take part compounded amino acid hydrolysis liquid sample Jing Kjeldahl's methods and measure total nitrogen content in sample, the detection of Jing formol titrations
Amino acid nitrogen content in sample, obtains compound amino acid conversion ratio obtained in the present embodiment for 83.49%；The compound amino acid
In contain 17 kinds of amino acid, Jing automatic amino acid analyzers analysis determine its concrete composition composition be shown in Table 3：
The compound amino acid of table 3 is constituted（g/L）
| Amino acid is constituted | Irradiation cooperates with 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 kind of method for efficiently preparing compound amino acid, comprises the following steps：
（1）Feather is taken, be dry, pulverize to 60 mesh sieves are crossed, adopted60Co- gamma-rays carries out irradiation to it, and irradiation dose is
180KGy, radiation dose rate is 40Gy/min；
（2）In step（1）Concentration is added in feather meal after irradiated process for the hydrochloric acid of 8mol/L, stirring mixing, and heat
To 70 DEG C of hydrolysis 20min, the first hydrolyzate is obtained；Wherein, feather meal and the quality volume of hydrochloric acid are 1：8；
（3）By step（2）The first hydrolyzate for obtaining is placed in microwave reactor, and add the first hydrolyzate weight 0.6% from
Sub- liquid 1- butyl -3- methylimidazole bromides, under conditions of heating using microwave, continue to react 20min, and after cooling, Jing is filtered,
Obtain the second hydrolyzate；Wherein, heating using microwave power is 680W；
（4）Saturated calcium hydroxide solution is added in the second hydrolyzate for obtaining, the pH value of the second hydrolyzate is adjusted to 7, is filtered,
Obtain compounded amino acid hydrolysis liquid；
Take part compounded amino acid hydrolysis liquid sample Jing Kjeldahl's methods and measure total nitrogen content in sample, the detection of Jing formol titrations
Amino acid nitrogen content in sample, obtains compound amino acid conversion ratio obtained in the present embodiment for 84.61%；The compound amino acid
In contain 17 kinds of amino acid, Jing automatic amino acid analyzers analysis determine its concrete composition composition be shown in Table 4：
The compound amino acid of table 4 is constituted（g/L）
| Amino acid is constituted | Irradiation cooperates with 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 |
The amino acid content phase in the compound amino acid prepared using the inventive method is can be seen that by the data in above table
For existing sulfuric acid law technology is greatly enhanced, therefore, greatly improved using method of the present invention percent hydrolysis so that feather
In active ingredient can farthest be extracted, simultaneously as employing radiation treatment, microwave in a creative way first
The technology that heating and ionic liquid combine so that the reaction time greatly shortens, and extraction efficiency is significantly improved, therefore, this
The method of invention has huge application prospect.
The foregoing is only presently preferred embodiments of the present invention, not to limit the present invention, all spirit in the present invention and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (8)
1. a kind of method for efficiently preparing compound amino acid, is characterized in that, comprise the following steps：
（1）Feather is taken, 40-60 mesh sieves were crushed to, is adopted60Co- gamma-rays carries out irradiation to it；
（2）By step（1）Feather meal after irradiated process is hydrolyzed, and obtains the first hydrolyzate；
（3）In step（2）Ionic liquid is added in the first hydrolyzate for obtaining, and under conditions of heating using microwave, continues to react
5-20min, filters, and obtains the second hydrolyzate；
（4）The pH of the second hydrolyzate is adjusted to neutrality, that is, obtains compound amino acid.
2. the method for efficiently preparing compound amino acid according to claim 1, is characterized in that, step（1）In, using irradiation
During processing method, irradiation dose is 150-250KGy, and radiation dose rate is 20-50Gy/min.
3. the method for efficiently preparing compound amino acid according to claim 1, is characterized in that, step（2）Detailed process
For：
In step（1）Concentration is added in feather meal after irradiated process for the hydrochloric acid of 6-8mol/L, stirring mixing, and be heated to
40-70 DEG C of hydrolysis 5-20min, obtains the first hydrolyzate；Wherein, feather meal and the quality volume of hydrochloric acid are 1：5-8.
4. the method for efficiently preparing compound amino acid according to claim 1, is characterized in that, step（3）Detailed process
For：
By step（2）The first hydrolyzate for obtaining is placed in microwave reactor, and adds the first hydrolyzate weight 0.3%-
0.7% ionic liquid 1-butyl-3-methyl imidazolium bromide, under conditions of heating using microwave, continues to react 5-20min, obtains the
Two hydrolyzates；Wherein, heating using microwave power is 600-700W.
5. the method for efficiently preparing compound amino acid according to claim 1, is characterized in that, step（4）In, add saturation
Aqua calcis adjusts the pH value of the second hydrolyzate to neutrality, that is, obtain compound amino acid.
6. the method for efficiently preparing compound amino acid according to claim 2, is characterized in that, using irradiation treatment method
When, irradiation dose is 200KGy, and radiation dose rate is 25Gy/min.
7. the method for efficiently preparing compound amino acid according to claim 3, is characterized in that, step（2）Detailed process
For：
In step（1）Concentration is added in feather meal after irradiated process for the hydrochloric acid of 6mol/L, stirring mixing, and it is heated to 50
DEG C hydrolysis 8min, obtain the first hydrolyzate；Wherein, feather meal and the quality volume of hydrochloric acid are 1：5.
8. the method for efficiently preparing compound amino acid according to claim 4, is characterized in that, step（3）Detailed process
For：
By step（2）The first hydrolyzate for obtaining is placed in microwave reactor, and adds the first hydrolyzate weight 0.5%
Ionic liquid 1-butyl-3-methyl imidazolium bromide, under conditions of heating using microwave, continues to react 8min, obtains the second hydrolyzate；
Wherein, heating using microwave power is 640W.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107686851A (en) * | 2017-09-19 | 2018-02-13 | 荆门市欣胱生物工程股份有限公司 | A kind of method that feather microwave hydrolysis prepares compound amino acid |
| 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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107686851A (en) * | 2017-09-19 | 2018-02-13 | 荆门市欣胱生物工程股份有限公司 | A kind of method that feather microwave hydrolysis prepares compound amino acid |
| 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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| CN106631648B (en) | 2019-09-06 |
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