CN112493363A - Preparation method of composite amino acid chelate - Google Patents
Preparation method of composite amino acid chelate Download PDFInfo
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- CN112493363A CN112493363A CN202011362906.XA CN202011362906A CN112493363A CN 112493363 A CN112493363 A CN 112493363A CN 202011362906 A CN202011362906 A CN 202011362906A CN 112493363 A CN112493363 A CN 112493363A
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- 150000001413 amino acids Chemical class 0.000 title claims abstract description 62
- 239000013522 chelant Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002131 composite material Substances 0.000 title description 5
- 235000001014 amino acid Nutrition 0.000 claims abstract description 83
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 27
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 27
- 235000018102 proteins Nutrition 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- -1 compound amino acid Chemical class 0.000 claims abstract description 17
- 230000009920 chelation Effects 0.000 claims abstract description 11
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005903 acid hydrolysis reaction Methods 0.000 claims abstract description 9
- 230000002378 acidificating effect Effects 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 6
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000004471 Glycine Substances 0.000 claims abstract description 5
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 claims abstract description 5
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims abstract description 5
- 235000003704 aspartic acid Nutrition 0.000 claims abstract description 5
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 235000013922 glutamic acid Nutrition 0.000 claims abstract description 5
- 239000004220 glutamic acid Substances 0.000 claims abstract description 5
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 5
- 230000004913 activation Effects 0.000 claims abstract description 4
- 150000004679 hydroxides Chemical class 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 239000000413 hydrolysate Substances 0.000 claims description 22
- 235000019764 Soybean Meal Nutrition 0.000 claims description 16
- 239000004455 soybean meal Substances 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 12
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 9
- 239000003456 ion exchange resin Substances 0.000 claims description 9
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 9
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 8
- 239000000920 calcium hydroxide Substances 0.000 claims description 8
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000001223 reverse osmosis Methods 0.000 claims description 8
- 239000008399 tap water Substances 0.000 claims description 8
- 235000020679 tap water Nutrition 0.000 claims description 8
- 238000003916 acid precipitation Methods 0.000 claims description 7
- 238000001994 activation Methods 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 7
- 230000003213 activating effect Effects 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 238000002329 infrared spectrum Methods 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 4
- 230000003472 neutralizing effect Effects 0.000 claims description 4
- 238000004806 packaging method and process Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000001694 spray drying Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052791 calcium Inorganic materials 0.000 abstract description 5
- 239000011575 calcium Substances 0.000 abstract description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 235000013305 food Nutrition 0.000 abstract description 4
- 229910052742 iron Inorganic materials 0.000 abstract description 4
- 229910052725 zinc Inorganic materials 0.000 abstract description 4
- 239000011701 zinc Substances 0.000 abstract description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 3
- 241000196324 Embryophyta Species 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 235000010627 Phaseolus vulgaris Nutrition 0.000 abstract 1
- 244000046052 Phaseolus vulgaris Species 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 239000011347 resin Substances 0.000 abstract 1
- 229920005989 resin Polymers 0.000 abstract 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 11
- 229960001484 edetic acid Drugs 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000015872 dietary supplement Nutrition 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/142—Amino acids; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/03—Organic compounds
- A23L29/045—Organic compounds containing nitrogen as heteroatom
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C11/00—Other nitrogenous fertilisers
Abstract
The invention discloses a preparation method of a compound amino acid chelate. The invention selects beans rich in amino acids such as aspartic acid, glutamic acid, glycine and the like as protein raw materials, and the protein is obtained by adopting an acid hydrolysis process and carrying out neutralization, resin deacidification, amino acid carboxyl activation, chelation, concentration and drying. The finished product does not contain inorganic acid radicals, and the total content of amino acid chelates is more than 90 percent; heating the activated acidic amino acid feed liquid to 50-90 ℃, slowly adding oxides, hydroxides or simple substances of elements such as calcium, iron and zinc, controlling the end point pH to be 4.0-10.0, and then carrying out heat preservation and chelation for 2-12 h; the product only contains amino acid, chelating elements and a small amount of water and impurities, is completely green and environment-friendly, so the biological absorption and utilization rate of the product is far higher than that of other chelating products, can be completely absorbed and utilized by passive plants, and can be widely applied to the aspects of food processing, pet feed, organic planting and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of amino acid chelates, and particularly relates to a preparation method of a compound amino acid chelate.
Background
The compound amino acid chelate, such as compound amino acid chelate calcium, iron, zinc and other elements, does not contain inorganic acid radical, and the total content of the amino acid chelate is more than 90 percent. As a food additive for the food industry; as a nutrition enhancer for pet feed; as organic chelate for supplementing nutrient elements required by crop growth. EDTA chelate compounds: EDTA (ethylene diamine tetraacetic acid) and oxides or hydroxides of elements such as calcium, iron, zinc and the like are chelated under certain conditions to obtain the EDTA chelate. Composite amino acid mixture: protein acid hydrolysate is mixed with inorganic salt of Ca, Fe, Zn and other elements under certain condition to obtain composite amino acid mixture.
However: 1. the EDTA chelate is stable in chelation, but has the following problems: EDTA is not a nutrient substance, cannot be used as a nutrient supplement, and the addition amount of EDTA in the food industry is strictly limited, so that the EDTA cannot be applied in a large scale; in the planting industry, the biggest defect of the EDTA chelate is that EDTA cannot be degraded for a long time after the EDTA enters soil. 2. The compound amino acid mixture has the following problems: low chelating rate and poor absorption capacity; if the fertilizer does not contain a large amount of chloride ions, the fertilizer cannot be used for many chlorine-prohibited crops; if the sulfate does not contain a large amount of sulfate, the sulfate forms calcium sulfate precipitate, and the absorption of calcium is influenced; if the nitrate radical is not contained in a large amount, the nitrate radical can prevent the color of the fruit from changing during use, and the fruit turns green.
Disclosure of Invention
The invention aims to: in order to solve the problems proposed above, a method for preparing a complex amino acid chelate is provided.
The technical scheme adopted by the invention is as follows: the preparation method of the compound amino acid chelate comprises the following steps:
s1, firstly, treating the tap water by using reverse osmosis equipment, and preparing the pure water required to be used during preparation;
s2, selecting defatted soybean meal as a protein raw material, performing alkali dissolution, acid precipitation and cleaning on the soybean meal to obtain separated protein, and performing acid hydrolysis on the separated protein by using dilute hydrochloric acid or dilute sulfuric acid;
s3, taking the hydrochloric acid hydrolysate in the step S2, decompressing and expelling acid, filtering for later use, or neutralizing the sulfuric acid hydrolysate with calcium hydroxide, and then performing filter pressing, and filtering for later use;
s4, deacidifying the filtrate obtained in the step S3 by an ion exchange resin column, activating amino acid carboxyl in the deacidified liquid, and preparing for chelating after the activation process is finished;
s5, adding corresponding ingredients into the feed liquid obtained in the step S4, starting to perform a chelation reaction, controlling the chelate proportion, the chelate pH, the chelate temperature and the chelate time, adding the reaction product into a concentration device, and starting to concentrate;
s6, after the concentration in the step S5 is finished, drying the concentrated solution by a spray drying device, or cooling, crystallizing, filtering and drying the concentrated solution;
and S7, packaging the finished product prepared in the step S6, and sealing and storing to finish the preparation of the whole compound amino acid chelate.
In a preferred embodiment, in step S1, the pure water is prepared from tap water by a conventional technique, and is treated by a two-stage reverse osmosis.
In a preferred embodiment, in step S1, defatted soybean meal is used as a raw material, 8 to 10 times equivalent of pure water is added to the soybean meal, ph is controlled to be 8.0 to 9.0 for alkali dissolution, ph is controlled to be 3.5 to 4.5 for acid precipitation, 2 to 4 times equivalent of pure water is added to the protein slurry for cleaning, and hydrolysis is performed after protein separation is obtained, so that the obtained hydrolysate has high amino acid content, contains 18 amino acids, and is rich in amino acids such as aspartic acid, glutamic acid and glycine with excellent chelating ability.
In a preferred embodiment, in step S2, dilute hydrochloric acid or dilute sulfuric acid with concentration of 15% to 20% is used for acid hydrolysis to ensure that the protein can be hydrolyzed into free amino acids as much as possible.
In a preferred embodiment, in step S3, the hydrochloric acid hydrolysate is subjected to acid removal by a method of concentration under reduced pressure, and the sulfuric acid hydrolysate is subjected to acid removal by a method of calcium hydroxide neutralization.
In a preferred embodiment, in step S4, the liquid obtained in S3 is deacidified again by using ion exchange resin to completely remove chloride or sulfate in the liquid, and then carboxyl group activation is performed to make the amino acid have positive charge and become acidic, so that the pH is required to be less than 3.0, and the next chelation is prepared.
In a preferred embodiment, a specific kind of oxide, hydroxide or simple substance of an element to be chelated is added to the acidic amino acid feed liquid after activation in step S5, and the ratio of the amino acid to the chelating element is controlled to be 5: 1-15: 1, the chelating pH is 4.0-10.0, the chelating temperature is 50-90 ℃, and the chelating time is 2-12 h, so as to perform a chelating reaction.
In a preferred embodiment, the composite amino acid chelate product obtained in step S6 has a total content of amino acid chelate of more than or equal to 90%, and inorganic acid radicals of Cl-, SO42-, NO 3-and the like of less than or equal to 1.0%.
In a preferred embodiment, the determination of the content of amino acid chelate in step S6 comprises: according to GB5009.124, GB30605, GB30606 and GB1903.2 standards, firstly, the contents of amino acid and chelating elements are detected, and then the chelating structure is identified by adopting infrared spectrum.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. in the invention, after the hydrolysate is neutralized, the ion exchange resin is adopted to completely remove inorganic acid radicals, so that the content of amino acid is greatly improved, the production cost is saved, and the yield of the chelate is greatly increased.
2. In the invention, the product only contains amino acid, chelating elements and a small amount of water and impurities, is completely green and environment-friendly, so the biological absorption and utilization rate of the product is far higher than that of other chelating products, and the product can be completely absorbed and utilized by passive plants and can be widely applied to the aspects of food processing, pet feed, organic planting and the like.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
With reference to figure 1 of the drawings,
the first embodiment is as follows:
the preparation method of the compound amino acid chelate comprises the following steps:
s1, firstly, treating tap water by using reverse osmosis equipment, and preparing pure water required in preparation, wherein in the step S1, the pure water is prepared from the tap water by adopting a common technology and is in a two-stage reverse osmosis treatment mode; in step S1, defatted soybean meal is used as a raw material, 8 times equivalent of pure water of the soybean meal is added, ph is controlled to be 8.0 for alkali dissolution, ph is controlled to be 3.5 for acid precipitation, 2 times equivalent of pure water is added to the protein slurry for cleaning, and hydrolysis is performed after protein separation is obtained, so that the prepared hydrolysate has high amino acid content, contains 18 kinds of amino acids, and is rich in amino acids such as aspartic acid, glutamic acid, glycine and the like with excellent chelating ability;
s2, selecting defatted soybean meal as a protein raw material, performing alkali dissolution, acid precipitation and cleaning on the soybean meal to obtain separated protein, and performing acid hydrolysis on the separated protein by using dilute hydrochloric acid or dilute sulfuric acid, wherein in the step S2, 15% -20% of dilute hydrochloric acid or dilute sulfuric acid is used for performing acid hydrolysis to ensure that the protein can be hydrolyzed into free amino acid as much as possible;
s3, taking the hydrochloric acid hydrolysate in the step S2, decompressing and expelling acid, filtering for later use, or neutralizing the sulfuric acid hydrolysate with calcium hydroxide, and then performing filter pressing, and filtering for later use; in step S3, acid removal is performed on the hydrochloric acid hydrolysate by a method of reduced pressure concentration, and acid removal is performed on the sulfuric acid hydrolysate by a method of calcium hydroxide neutralization;
s4, deacidifying the filtrate obtained in the step S3 by an ion exchange resin column, activating amino acid carboxyl in the deacidified liquid, and preparing for chelating after the activation process is finished; in step S4, deacidifying the liquid obtained in step S3 again by using ion exchange resin to completely remove chloride ions or sulfate radicals in the liquid, activating carboxyl to enable amino acid to have positive charges and become acidic, and preparing for next chelation, wherein the pH is required to be less than 3.0;
s5, adding corresponding ingredients into the feed liquid obtained in the step S4, starting to perform a chelation reaction, controlling the chelate proportion, the chelate pH, the chelate temperature and the chelate time, adding the reaction product into a concentration device, and starting to concentrate; adding a specific kind of oxide, hydroxide or simple substance of an element to be chelated into the activated acidic amino acid feed liquid in the step S5, controlling the ratio of the amino acid to the chelating element to be 5: 1-15: 1, the chelating pH value to be 4.0-10.0, the chelating temperature to be 50-90 ℃ and the chelating time to be 2-12 h, and carrying out a chelating reaction;
s6, after the concentration in the step S5 is finished, drying the concentrated solution by a spray drying device, or cooling, crystallizing, filtering and drying the concentrated solution; the total content of the amino acid chelate in the finished product of the compound amino acid chelate obtained in the step S6 is more than or equal to 90 percent, and inorganic acid radicals such as Cl-, SO42-, NO 3-and the like are less than or equal to 1.0 percent;
s7, packaging the finished product prepared in the step S6, and sealing and storing to finish the preparation of the whole compound amino acid chelate; step S6 determination of amino acid chelate content: according to GB5009.124, GB30605, GB30606 and GB1903.2 standards, firstly, the contents of amino acid and chelating elements are detected, and then the chelating structure is identified by adopting infrared spectrum.
Example two:
the preparation method of the compound amino acid chelate comprises the following steps:
s1, firstly, treating tap water by using reverse osmosis equipment, and preparing pure water required in preparation, wherein in the step S1, the pure water is prepared from the tap water by adopting a common technology and is in a two-stage reverse osmosis treatment mode; in step S1, defatted soybean meal is used as a raw material, 10-fold equivalent of pure water is added to the soybean meal, ph is controlled to be 9.0 for alkali dissolution, ph is controlled to be 4.5 for acid precipitation, and 4-fold equivalent of pure water is added to the protein slurry for cleaning to obtain protein isolate, and then hydrolysis is performed, so that the prepared hydrolysate has high amino acid content, contains 18 kinds of amino acids, and is rich in amino acids such as aspartic acid, glutamic acid, glycine and the like with excellent chelating ability;
s2, selecting defatted soybean meal as a protein raw material, performing alkali dissolution, acid precipitation and cleaning on the soybean meal to obtain separated protein, and performing acid hydrolysis on the separated protein by using dilute hydrochloric acid or dilute sulfuric acid, wherein in the step S2, 15% -20% of dilute hydrochloric acid or dilute sulfuric acid is used for performing acid hydrolysis to ensure that the protein can be hydrolyzed into free amino acid as much as possible;
s3, taking the hydrochloric acid hydrolysate in the step S2, decompressing and expelling acid, filtering for later use, or neutralizing the sulfuric acid hydrolysate with calcium hydroxide, and then performing filter pressing, and filtering for later use; in step S3, acid removal is performed on the hydrochloric acid hydrolysate by a method of reduced pressure concentration, and acid removal is performed on the sulfuric acid hydrolysate by a method of calcium hydroxide neutralization;
s4, deacidifying the filtrate obtained in the step S3 by an ion exchange resin column, activating amino acid carboxyl in the deacidified liquid, and preparing for chelating after the activation process is finished; in step S4, deacidifying the liquid obtained in step S3 again by using ion exchange resin to completely remove chloride ions or sulfate radicals in the liquid, activating carboxyl to enable amino acid to have positive charges and become acidic, and preparing for next chelation, wherein the pH is required to be less than 3.0;
s5, adding corresponding ingredients into the feed liquid obtained in the step S4, starting to perform a chelation reaction, controlling the chelate proportion, the chelate pH, the chelate temperature and the chelate time, adding the reaction product into a concentration device, and starting to concentrate; adding a specific kind of oxide, hydroxide or simple substance of an element to be chelated into the activated acidic amino acid feed liquid in the step S5, controlling the ratio of the amino acid to the chelating element to be 5: 1-15: 1, the chelating pH value to be 4.0-10.0, the chelating temperature to be 50-90 ℃ and the chelating time to be 2-12 h, and carrying out a chelating reaction;
s6, after the concentration in the step S5 is finished, drying the concentrated solution by a spray drying device, or cooling, crystallizing, filtering and drying the concentrated solution; the total content of the amino acid chelate in the finished product of the compound amino acid chelate obtained in the step S6 is more than or equal to 90 percent, and inorganic acid radicals such as Cl-, SO42-, NO 3-and the like are less than or equal to 1.0 percent;
s7, packaging the finished product prepared in the step S6, and sealing and storing to finish the preparation of the whole compound amino acid chelate; step S6 determination of amino acid chelate content: according to GB5009.124, GB30605, GB30606 and GB1903.2 standards, firstly, the contents of amino acid and chelating elements are detected, and then the chelating structure is identified by adopting infrared spectrum.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. The preparation method of the compound amino acid chelate is characterized by comprising the following steps: the preparation method of the compound amino acid chelate comprises the following steps:
s1, firstly, treating the tap water by using reverse osmosis equipment, and preparing the pure water required to be used during preparation;
s2, selecting defatted soybean meal as a protein raw material, performing alkali dissolution, acid precipitation and cleaning on the soybean meal to obtain separated protein, and performing acid hydrolysis on the separated protein by using dilute hydrochloric acid or dilute sulfuric acid;
s3, taking the hydrochloric acid hydrolysate in the step S2, decompressing and expelling acid, filtering for later use, or neutralizing the sulfuric acid hydrolysate with calcium hydroxide, and then performing filter pressing, and filtering for later use;
s4, deacidifying the filtrate obtained in the step S3 by an ion exchange resin column, activating amino acid carboxyl in the deacidified liquid, and preparing for chelating after the activation process is finished;
s5, adding corresponding ingredients into the feed liquid obtained in the step S4, starting to perform a chelation reaction, controlling the chelate proportion, the chelate pH, the chelate temperature and the chelate time, adding the reaction product into a concentration device, and starting to concentrate;
s6, after the concentration in the step S5 is finished, drying the concentrated solution by a spray drying device, or cooling, crystallizing, filtering and drying the concentrated solution;
and S7, packaging the finished product prepared in the step S6, and sealing and storing to finish the preparation of the whole compound amino acid chelate.
2. The method of preparing a complex amino acid chelate according to claim 1, characterized in that: in the step S1, the pure water is prepared from tap water by a common technique, which is a two-stage reverse osmosis treatment.
3. The method of preparing a complex amino acid chelate according to claim 1, characterized in that: in the step S1, defatted soybean meal is used as a raw material, 8-10 times equivalent of pure water of soybean meal is added, ph is controlled to be 8.0-9.0 alkali-soluble, ph is controlled to be 3.5-4.5 acid-precipitated, 2-4 times equivalent of pure water is added to protein mud for cleaning, and hydrolysis is performed after protein separation is obtained, so that the prepared hydrolysate has high amino acid content, contains 18 kinds of amino acids, and is rich in amino acids such as aspartic acid, glutamic acid and glycine with excellent chelating ability.
4. The method of preparing a complex amino acid chelate according to claim 1, characterized in that: in step S2, dilute hydrochloric acid or dilute sulfuric acid of 15% to 20% is used for acid hydrolysis to ensure that the protein can be hydrolyzed into free amino acids as much as possible.
5. The method of preparing a complex amino acid chelate according to claim 1, characterized in that: in the step S3, acid removal is performed on the hydrochloric acid hydrolysate by a method of vacuum concentration, and acid removal is performed on the sulfuric acid hydrolysate by a method of calcium hydroxide neutralization.
6. The method of preparing a complex amino acid chelate according to claim 1, characterized in that: in the step S4, the liquid obtained in S3 is deacidified again by ion exchange resin to completely remove chloride ions or sulfate radicals in the liquid, and then carboxyl group activation is performed to make amino acid have positive charges and become acidic, and the pH is required to be less than 3.0, so as to prepare for next chelation.
7. The method of preparing a complex amino acid chelate according to claim 1, characterized in that: adding specific oxides, hydroxides or simple substances of elements to be chelated into the activated acidic amino acid feed liquid in the step S5, controlling the ratio of the amino acid to the chelating elements to be 5: 1-15: 1, the chelating pH value to be 4.0-10.0, the chelating temperature to be 50-90 ℃ and the chelating time to be 2-12 h, and carrying out a chelating reaction.
8. The method of preparing a complex amino acid chelate according to claim 1, characterized in that: the total content of the amino acid chelate in the finished product of the compound amino acid chelate obtained in the step S6 is more than or equal to 90 percent, and inorganic acid radicals such as Cl-, SO42-, NO 3-and the like are less than or equal to 1.0 percent.
9. The method of preparing a complex amino acid chelate according to claim 6, characterized in that: the determination of the content of the amino acid chelate in the step S6: according to GB5009.124, GB30605, GB30606 and GB1903.2 standards, firstly, the contents of amino acid and chelating elements are detected, and then the chelating structure is identified by adopting infrared spectrum.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112048528A (en) * | 2020-09-16 | 2020-12-08 | 四川绵竹市瑞洋生物技术有限公司 | Method for preparing compound amino acid by enzymolysis process |
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| CN85105574A (en) * | 1985-01-17 | 1987-01-14 | 四川大学 | From livestock blood, obtain through refining method of compound amino-acid |
| CN1334260A (en) * | 2001-09-05 | 2002-02-06 | 四川省丰禾实业有限责任公司 | Process for preparing leaf fertilizer by chelating amino acids with trace elements |
| CN1379019A (en) * | 2002-04-25 | 2002-11-13 | 丁奕翔 | Composite vegetative amino acid and its preparing process |
| CN111374295A (en) * | 2020-04-16 | 2020-07-07 | 无锡秋可生物科技有限公司 | Preparation method and application of high-quality food-grade plant-derived compound amino acid |
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| CN85105574A (en) * | 1985-01-17 | 1987-01-14 | 四川大学 | From livestock blood, obtain through refining method of compound amino-acid |
| CN1334260A (en) * | 2001-09-05 | 2002-02-06 | 四川省丰禾实业有限责任公司 | Process for preparing leaf fertilizer by chelating amino acids with trace elements |
| CN1379019A (en) * | 2002-04-25 | 2002-11-13 | 丁奕翔 | Composite vegetative amino acid and its preparing process |
| CN111374295A (en) * | 2020-04-16 | 2020-07-07 | 无锡秋可生物科技有限公司 | Preparation method and application of high-quality food-grade plant-derived compound amino acid |
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Application publication date: 20210316 |