CN115594545A - Method for producing Gly-containing water-soluble fertilizer - Google Patents
Method for producing Gly-containing water-soluble fertilizer Download PDFInfo
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- CN115594545A CN115594545A CN202211424128.1A CN202211424128A CN115594545A CN 115594545 A CN115594545 A CN 115594545A CN 202211424128 A CN202211424128 A CN 202211424128A CN 115594545 A CN115594545 A CN 115594545A
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- glycine
- amino acid
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- mother liquor
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- 239000003337 fertilizer Substances 0.000 title claims abstract description 48
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims abstract description 186
- 239000004471 Glycine Substances 0.000 claims abstract description 79
- -1 compound amino acid Chemical class 0.000 claims abstract description 51
- 238000002156 mixing Methods 0.000 claims abstract description 42
- 239000011573 trace mineral Substances 0.000 claims abstract description 21
- 235000013619 trace mineral Nutrition 0.000 claims abstract description 21
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011575 calcium Substances 0.000 claims abstract description 20
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 20
- ZHJGWYRLJUCMRT-UHFFFAOYSA-N 5-[6-[(4-methylpiperazin-1-yl)methyl]benzimidazol-1-yl]-3-[1-[2-(trifluoromethyl)phenyl]ethoxy]thiophene-2-carboxamide Chemical compound C=1C=CC=C(C(F)(F)F)C=1C(C)OC(=C(S1)C(N)=O)C=C1N(C1=C2)C=NC1=CC=C2CN1CCN(C)CC1 ZHJGWYRLJUCMRT-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 12
- 229940038879 chelated zinc Drugs 0.000 claims abstract description 10
- 238000000909 electrodialysis Methods 0.000 claims abstract description 7
- RZLVQBNCHSJZPX-UHFFFAOYSA-L zinc sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Zn+2].[O-]S([O-])(=O)=O RZLVQBNCHSJZPX-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000011701 zinc Substances 0.000 claims abstract description 5
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 5
- 239000010413 mother solution Substances 0.000 claims abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 75
- 239000012452 mother liquor Substances 0.000 claims description 60
- 235000001014 amino acid Nutrition 0.000 claims description 51
- 238000003756 stirring Methods 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- 238000006243 chemical reaction Methods 0.000 claims description 36
- 238000001914 filtration Methods 0.000 claims description 36
- 239000013078 crystal Substances 0.000 claims description 35
- 238000005406 washing Methods 0.000 claims description 35
- 239000000725 suspension Substances 0.000 claims description 34
- 239000008367 deionised water Substances 0.000 claims description 30
- 229910021641 deionized water Inorganic materials 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 30
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000005303 weighing Methods 0.000 claims description 20
- 125000004122 cyclic group Chemical group 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- 239000013522 chelant Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000007810 chemical reaction solvent Substances 0.000 claims description 10
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 claims description 10
- 229940106681 chloroacetic acid Drugs 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims description 5
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 claims description 5
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 claims description 5
- KZSNJWFQEVHDMF-BYPYZUCNSA-N L-valine Chemical compound CC(C)[C@H](N)C(O)=O KZSNJWFQEVHDMF-BYPYZUCNSA-N 0.000 claims description 5
- 239000004472 Lysine Substances 0.000 claims description 5
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004115 Sodium Silicate Substances 0.000 claims description 5
- KZSNJWFQEVHDMF-UHFFFAOYSA-N Valine Natural products CC(C)C(N)C(O)=O KZSNJWFQEVHDMF-UHFFFAOYSA-N 0.000 claims description 5
- 235000004279 alanine Nutrition 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000011790 ferrous sulphate Substances 0.000 claims description 5
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 5
- 235000013922 glutamic acid Nutrition 0.000 claims description 5
- 239000004220 glutamic acid Substances 0.000 claims description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 5
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 239000012429 reaction media Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 239000004474 valine Substances 0.000 claims description 5
- 150000001413 amino acids Chemical class 0.000 abstract description 7
- 235000015097 nutrients Nutrition 0.000 abstract description 7
- 230000009471 action Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 230000008635 plant growth Effects 0.000 abstract description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000012010 growth Effects 0.000 abstract description 3
- 229910021645 metal ion Inorganic materials 0.000 abstract description 3
- 239000011574 phosphorus Substances 0.000 abstract description 3
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 3
- 239000002244 precipitate Substances 0.000 abstract description 3
- 239000002689 soil Substances 0.000 abstract description 3
- 102000004190 Enzymes Human genes 0.000 abstract description 2
- 108090000790 Enzymes Proteins 0.000 abstract description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 230000008485 antagonism Effects 0.000 abstract description 2
- 230000003851 biochemical process Effects 0.000 abstract description 2
- 159000000007 calcium salts Chemical class 0.000 abstract description 2
- 210000000170 cell membrane Anatomy 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 230000035790 physiological processes and functions Effects 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 239000011593 sulfur Substances 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract description 2
- 241000196324 Embryophyta Species 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 241000227653 Lycopersicon Species 0.000 description 3
- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C5/00—Fertilisers containing other nitrates
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Fertilizers (AREA)
Abstract
The invention relates to the technical field of crop fertilizers, and provides a method for producing a Gly-containing water-soluble fertilizer, which purifies a glycine concentrated mother solution by an electrodialysis method, and enables refined glycine prepared by purification to react with calcium nitrate tetrahydrate to prepare glycine chelated calcium, so that the condition that calcium salt and nutrient elements such as phosphorus, sulfur and the like form precipitates can be prevented, the stability of plant cell membranes can be enhanced through the action of the glycine chelated calcium, and the Gly-containing water-soluble fertilizer can participate in the regulation and control of the physiological and biochemical processes and the enzyme activity of plants, and is beneficial to the growth of plants; and secondly, the compound amino acid chelated zinc is prepared from compound amino acid prepared by mixing various amino acids and zinc sulfate heptahydrate, trace elements and various amino acid components can be provided for plants, and while a nitrogen source is provided for plant growth through the compound amino acid, the interference of soil and metal ion antagonism can be resisted through the trace element zinc, so that a stable growth environment is provided for the plants.
Description
Technical Field
The invention relates to the technical field of crop fertilizers, in particular to a method for producing a Gly-containing water-soluble fertilizer.
Background
The water-soluble fertilizer is easy to be absorbed by crops, has relatively high absorption and utilization rate, is a quick-acting fertilizer, can enable a grower to quickly see the effect and the expression of the fertilizer, and can adjust the fertilizer formula according to different growth vigors of the crops at any time; the water-soluble fertilizer can be applied to facility agriculture such as spraying and drip irrigation, so that water and fertilizer integration is realized, and the effects of saving water, fertilizer and labor are achieved. Most of the existing water-soluble fertilizers are prepared by mixing medium elements and trace elements, and some water-soluble fertilizers also have specified types of amino acids, but most of metal ions in the existing water-soluble fertilizers exist in the form of metal salts, and easily form precipitates with elements such as phosphorus and sulfur in soil in the fertilizing process, so that the absorption rate of plants is reduced, and the amino acids contained in the existing water-soluble fertilizers are less in types and cannot ensure the nutrient components of the plants comprehensively, so how to develop a water-soluble fertilizer which has comprehensive nutrient components and is beneficial to the absorption of the plants becomes a technical problem to be solved by technical personnel in the field urgently.
Disclosure of Invention
Solves the technical problem
Aiming at the defects of the prior art, the invention provides a method for producing a Gly-containing water-soluble fertilizer, so that the produced water-soluble fertilizer can ensure the comprehensive supplement of the nutrient components of plants and simultaneously can improve the absorption utilization rate of the nutrient components, thereby improving the application prospect of the water-soluble fertilizer.
Technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for producing a Gly-containing water-soluble fertilizer, which comprises the following steps:
step1, measuring 100 parts by weight of glycine concentrated mother liquor for later use, diluting the glycine concentrated mother liquor by using equivalent methanol, filtering to remove impurities after dilution is finished, adding the obtained solution into a dilute chamber charging basket of an electrodialyzer, adding distilled water into a dense chamber charging basket of the electrodialyzer, performing electrodialysis separation to obtain dilute chamber solution and dense chamber solution, heating and concentrating the dilute chamber solution at the temperature of 70-100 ℃ until glycine is crystallized and separated out, separating a crystal from the mother liquor by filtering, drying to obtain refined glycine, and recycling the mother liquor after crystallization and filtration;
step2, as per 2:3, weighing calcium nitrate tetrahydrate and refined glycine in Step1, mixing the calcium nitrate tetrahydrate and the refined glycine with deionized water, stirring the mixture at the speed of 300-400r/min for 5-10min to prepare a suspension, adjusting the pH of the suspension to 5.5 by using hydrochloric acid or ammonia water, heating the temperature to 50 ℃, pouring the suspension into a high-pressure fluid nano mill for treatment until the suspension is clear, drying the clear suspension at low temperature under reduced pressure, filtering the suspension into fine powder by using a 100-200-mesh screen, and obtaining glycine chelated calcium;
step3, weighing a certain amount of compound amino acid, dissolving the compound amino acid in deionized water with the weight 2-3 times of the weight of the compound amino acid, filtering to remove insoluble substances, adjusting the pH to 5 by using a sodium hydroxide solution, adding zinc sulfate heptahydrate with the weight of 20-30% of the compound amino acid, reacting for 30min at the water bath temperature of 60 ℃, heating, concentrating, cooling, crystallizing, filtering and drying crystals to obtain the compound amino acid chelated zinc;
step4, weighing 58-60 parts by weight of concentrated glycine mother liquor, 8-9 parts by weight of magnesium nitrate hexahydrate, 5-8 parts by weight of medium elements, 3-5 parts by weight of trace elements, 15-18 parts by weight of calcium glycine chelate in Step2, 4-5 parts by weight of zinc amino acid complex chelate in Step3 and 85-90 parts by weight of deionized water for later use;
step5, mixing the glycine concentrated mother liquor in Step4 with one half of deionized water, uniformly stirring, adding the glycine chelated calcium and the compound amino acid chelated zinc in parts by weight, and stirring again to obtain a first component;
step6, mixing magnesium nitrate hexahydrate, secondary elements, trace elements and the balance of deionized water in Step4, and stirring uniformly to obtain a second component;
and Step7, mixing the first component and the second component, uniformly stirring, filtering to remove impurities, and heating and concentrating to half of the original volume to obtain the Gly-containing water-soluble fertilizer.
Further, the preparation method of the glycine concentrated mother liquor comprises the following steps:
step1, pouring chloroacetic acid, methanol and urotropine into a reactor, stirring and dissolving, slowly introducing liquid ammonia, carrying out synthetic reaction for 2 hours at the temperature of 58-60 ℃, and maintaining the pH of a reaction system to be 7-8 in the reaction process, wherein the molar ratio of chloroacetic acid to methanol to urotropine is 1:7.5:0.2;
step2, after the reaction in the step1 is finished, keeping the temperature until crystals are separated out, cooling to room temperature, centrifuging, filtering to obtain mother liquor and crystals, washing the crystals for 2 times by using a small amount of methanol, mixing washing liquor obtained by washing with the mother liquor, and taking the washing liquor as a circulating reaction solvent;
step3, taking the cyclic reaction solvent in the step2 as a reaction medium for the next cyclic reaction to use, and obtaining mother liquor and a crystal after the last cyclic reaction is finished;
and 4, washing the crystal in the step3 for 2 times by using methanol, mixing the washed washing liquid with the mother liquor in the step3, and simply distilling the mixed washing liquid to obtain the glycine concentrated mother liquor.
Further, the stirring speed in the step1 is 500-600r/min, and the centrifugal rotating speed in the step2 is 7000-8000r/min.
Further, the number of the cycling reaction in the step3 is 3-4.
Further, the Step1 concentration by heating is carried out with stirring.
Further, the amount of the deionized water in the Step2 is 3-4 times of the total amount of the calcium nitrate tetrahydrate and the fine glycine.
Furthermore, the preparation method of the compound amino acid in Step3 comprises the following steps: weighing 17-18 parts of lysine, 1-2 parts of glutamic acid, 0.3-0.5 part of alanine, 0.03-0.05 part of valine and 0.1-0.3 part of phenylalanine according to parts by weight, mixing uniformly to obtain the compound amino acid.
Further, the medium element in Step4 is hydrated sodium silicate.
Furthermore, the trace element in Step4 is prepared by mixing boric acid and ferrous sulfate according to the same weight ratio.
Further, the stirring speed in Step5 and Step6 is 600-800r/min.
Advantageous effects
The invention provides a method for producing a Gly-containing water-soluble fertilizer, which has the following beneficial effects compared with the prior art:
according to the invention, the glycine concentrated mother liquor is purified by an electrodialysis method, and refined glycine obtained by purification is reacted with calcium nitrate tetrahydrate to obtain glycine chelated calcium, so that the condition that calcium salt and nutrient elements such as phosphorus and sulfur form precipitates can be prevented, the stability of plant cell membranes can be enhanced by the action of the glycine chelated calcium, and the glycine chelated calcium can participate in the physiological and biochemical processes of plants and the regulation and control of enzyme activity, so that the growth of plants is facilitated; secondly, the compound amino acid chelated zinc is prepared from compound amino acid prepared by mixing various amino acids and zinc sulfate heptahydrate, trace elements and various amino acid components can be provided for plants, and while a nitrogen source is provided for plant growth through the compound amino acid, the interference of soil and the antagonism of metal ions can be resisted through the trace element zinc, so that a stable growth environment is provided for the plants; finally, more sufficient nutrients can be provided for plants by adding the magnesium nitrate hexahydrate, the secondary elements and the trace elements, so that the Gly-containing water-soluble fertilizer produced by the invention has better application prospect.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the method for producing the Gly-containing water-soluble fertilizer comprises the following steps:
step1, measuring 100 parts by weight of glycine concentrated mother liquor for later use, diluting the glycine concentrated mother liquor by using methanol with the same amount, filtering to remove impurities after dilution is finished, adding the obtained solution into a dilute chamber charging basket of an electrodialyzer, adding distilled water into a concentrated chamber charging basket of the electrodialyzer, performing electrodialysis separation to obtain a dilute chamber solution and a concentrated chamber solution, heating and concentrating the dilute chamber solution at the temperature of 70 ℃ until glycine is crystallized and separated out, separating a crystal from the mother liquor by filtering, drying to obtain refined glycine, and recycling the crystallized and filtered mother liquor;
step2, as per 2:3, weighing calcium nitrate tetrahydrate and refined glycine in Step1, mixing the calcium nitrate tetrahydrate and the refined glycine with deionized water, stirring the mixture at the speed of 300r/min for 5min to prepare a suspension, adjusting the pH of the suspension to 5.5 by using hydrochloric acid or ammonia water, heating the suspension to 50 ℃, pouring the suspension into a high-pressure fluid nano mill for treatment until the suspension becomes clear, drying the clear suspension at a low temperature under reduced pressure, filtering the suspension into fine powder by using a 100-mesh screen, and recording the fine powder as glycine chelated calcium;
step3, weighing a certain amount of compound amino acid, dissolving the compound amino acid in deionized water with the weight 2 times that of the compound amino acid, filtering to remove insoluble substances, adjusting the pH value to 5 by using a sodium hydroxide solution, adding zinc sulfate heptahydrate with the weight 20% of that of the compound amino acid, reacting for 30min at the water bath temperature of 60 ℃, heating, concentrating, cooling, crystallizing, filtering and drying crystals, and obtaining the compound amino acid chelated zinc;
step4, weighing 58 parts of concentrated glycine mother liquor, 8 parts of magnesium nitrate hexahydrate, 5 parts of medium elements, 3 parts of trace elements, 15 parts of calcium glycine chelate in Step2, 4 parts of zinc compound amino acid chelate in Step3 and 85 parts of deionized water for later use;
step5, mixing the glycine concentrated mother liquor in Step4 with one half of deionized water, uniformly stirring, adding the calcium glycine chelate and the compound zinc amino acid chelate according to the parts by weight, and stirring again to obtain a first component;
step6, mixing the magnesium nitrate hexahydrate, the secondary elements, the trace elements and the balance of deionized water in Step4, and stirring uniformly to obtain a second component;
and Step7, mixing the first component and the second component, uniformly stirring, filtering to remove impurities, and heating and concentrating to half of the original volume to obtain the Gly-containing water-soluble fertilizer.
The preparation method of the glycine concentrated mother liquor comprises the following steps:
step1, pouring chloroacetic acid, methanol and urotropine into a reactor, stirring and dissolving, slowly introducing liquid ammonia, carrying out synthetic reaction for 2 hours at the temperature of 58 ℃, and maintaining the pH of a reaction system to be 7 in the reaction process, wherein the molar ratio of chloroacetic acid to methanol to urotropine is 1:7.5:0.2;
step2, after the reaction in the step1 is finished, keeping the temperature until crystals are separated out, cooling to room temperature, centrifuging, filtering to obtain mother liquor and crystals, washing the crystals for 2 times by using a small amount of methanol, mixing washing liquor obtained by washing with the mother liquor, and taking the washing liquor as a circulating reaction solvent;
step3, taking the cyclic reaction solvent in the step2 as a reaction medium for the next cyclic reaction to use, and obtaining mother liquor and a crystal after the last cyclic reaction is finished;
and 4, washing the crystal in the step3 for 2 times by using methanol, mixing the washed washing liquid with the mother liquor in the step3, and simply distilling the mixed washing liquid to obtain the glycine concentrated mother liquor.
The stirring speed in step1 is 500r/min, and the centrifugal rotation speed in step2 is 7000r/min.
The number of the cyclic reaction in step3 was 3.
The heat concentration in Step1 was carried out with stirring.
The amount of deionized water in Step2 is 3 times of the total amount of calcium nitrate tetrahydrate and refined glycine.
The preparation method of the compound amino acid in Step3 comprises the following steps: weighing 17 parts of lysine, 1 part of glutamic acid, 0.3 part of alanine, 0.03 part of valine and 0.1 part of phenylalanine according to parts by weight, mixing uniformly to obtain the compound amino acid.
The medium element in Step4 is hydrated sodium silicate.
The trace element in Step4 is prepared by mixing boric acid and ferrous sulfate according to the same weight ratio.
The stirring speed in Step5 and Step6 was 600r/min.
Example 2:
the method for producing the Gly-containing water-soluble fertilizer comprises the following steps:
step1, measuring 100 parts by weight of glycine concentrated mother liquor for later use, diluting the glycine concentrated mother liquor by using methanol with the same amount, filtering to remove impurities after dilution is finished, adding the obtained solution into a dilute chamber charging basket of an electrodialyzer, adding distilled water into a concentrated chamber charging basket of the electrodialyzer, performing electrodialysis separation to obtain a dilute chamber solution and a concentrated chamber solution, heating and concentrating the dilute chamber solution at the temperature of 100 ℃ until glycine is crystallized and separated out, separating a crystal from the mother liquor by filtering, drying to obtain refined glycine, and recycling the crystallized and filtered mother liquor;
step2, as per 2:3, weighing calcium nitrate tetrahydrate and refined glycine in Step1, mixing the calcium nitrate tetrahydrate and the refined glycine with deionized water, stirring the mixture at the speed of 400r/min for 10min to prepare a suspension, adjusting the pH of the suspension to 5.5 by using hydrochloric acid or ammonia water, heating the suspension to 50 ℃, pouring the suspension into a high-pressure fluid nano mill for treatment until the suspension becomes clear, drying the clear suspension at a low temperature under reduced pressure, filtering the suspension into fine powder by using a 200-mesh screen, and recording the fine powder as glycine chelated calcium;
step3, weighing a certain amount of compound amino acid, dissolving the compound amino acid in deionized water with the weight 3 times that of the compound amino acid, filtering to remove insoluble substances, adjusting the pH to 5 by using a sodium hydroxide solution, adding zinc sulfate heptahydrate with the weight 30% of the compound amino acid, reacting for 30min at the water bath temperature of 60 ℃, heating, concentrating, cooling, crystallizing, filtering and drying crystals, and obtaining the compound amino acid chelated zinc;
step4, weighing 60 parts by weight of concentrated glycine mother liquor, 9 parts by weight of magnesium nitrate hexahydrate, 8 parts by weight of medium elements, 5 parts by weight of trace elements, 18 parts by weight of calcium glycine chelate in Step2, 5 parts by weight of zinc amino acid complex chelate in Step3 and 90 parts by weight of deionized water for later use;
step5, mixing the glycine concentrated mother liquor in Step4 with one half of deionized water, uniformly stirring, adding the calcium glycine chelate and the compound zinc amino acid chelate according to the parts by weight, and stirring again to obtain a first component;
step6, mixing the magnesium nitrate hexahydrate, the secondary elements, the trace elements and the balance of deionized water in Step4, and stirring uniformly to obtain a second component;
and Step7, mixing the first component and the second component, uniformly stirring, filtering to remove impurities, and heating and concentrating to half of the original volume to obtain the Gly-containing water-soluble fertilizer.
The preparation method of the glycine concentrated mother liquor comprises the following steps:
step1, pouring chloroacetic acid, methanol and urotropine into a reactor, stirring and dissolving, slowly introducing liquid ammonia, carrying out synthetic reaction for 2 hours at the temperature of 60 ℃, and maintaining the pH of a reaction system to be 8 in the reaction process, wherein the molar ratio of chloroacetic acid to methanol to urotropine is 1:7.5:0.2;
step2, after the reaction in the step1 is finished, keeping the temperature until crystals are separated out, cooling to room temperature, centrifuging, filtering to obtain mother liquor and crystals, washing the crystals for 2 times by using a small amount of methanol, mixing washing liquor obtained by washing with the mother liquor, and taking the washing liquor as a circulating reaction solvent;
step3, taking the cyclic reaction solvent in the step2 as a reaction medium for the next cyclic reaction to use, and obtaining mother liquor and a crystal after the last cyclic reaction is finished;
and 4, washing the crystal in the step3 for 2 times by using methanol, mixing the washed washing liquid with the mother liquor in the step3, and simply distilling the mixed washing liquid to obtain the glycine concentrated mother liquor.
The stirring speed in the step1 is 600r/min, and the centrifugal rotating speed in the step2 is 8000r/min.
The number of the cyclic reaction in the step3 is 4.
The heat concentration in Step1 was carried out with stirring.
The amount of deionized water in Step2 is 4 times of the total amount of calcium nitrate tetrahydrate and refined glycine.
The preparation method of the compound amino acid in Step3 comprises the following steps: weighing 18 parts of lysine, 2 parts of glutamic acid, 0.5 part of alanine, 0.05 part of valine and 0.3 part of phenylalanine according to parts by weight, mixing uniformly to obtain the compound amino acid.
The medium element in Step4 is hydrated sodium silicate.
The trace element in Step4 is prepared by mixing boric acid and ferrous sulfate according to the same weight ratio.
The stirring speed in Step5 and Step6 was 600r/min.
Example 3:
the method for producing the Gly-containing water-soluble fertilizer comprises the following steps:
step1, measuring 100 parts by weight of glycine concentrated mother liquor for later use, diluting the glycine concentrated mother liquor by using methanol with the same amount, filtering to remove impurities after dilution is finished, adding the obtained solution into a dilute chamber charging basket of an electrodialyzer, adding distilled water into a concentrated chamber charging basket of the electrodialyzer, performing electrodialysis separation to obtain a dilute chamber solution and a concentrated chamber solution, heating and concentrating the dilute chamber solution at the temperature of 80 ℃ until glycine is crystallized and separated out, separating a crystal from the mother liquor by filtering, drying to obtain refined glycine, and recycling the crystallized and filtered mother liquor;
step2, as per 2:3, weighing calcium nitrate tetrahydrate and refined glycine in Step1, mixing the calcium nitrate tetrahydrate and the refined glycine with deionized water, stirring the mixture at the speed of 400r/min for 8min to prepare a suspension, adjusting the pH of the suspension to 5.5 by using hydrochloric acid or ammonia water, heating the suspension to 50 ℃, pouring the suspension into a high-pressure fluid nano mill for treatment until the suspension becomes clear, drying the clear suspension at a low temperature under reduced pressure, filtering the suspension into fine powder by using a 200-mesh screen, and recording the fine powder as glycine chelated calcium;
step3, weighing a certain amount of compound amino acid, dissolving the compound amino acid in deionized water with the weight 3 times that of the compound amino acid, filtering to remove insoluble substances, adjusting the pH to 5 by using a sodium hydroxide solution, adding zinc sulfate heptahydrate with the weight 25% of the compound amino acid, reacting at the water bath temperature of 60 ℃ for 30min, heating, concentrating, cooling and crystallizing after reaction, filtering and drying crystals, and obtaining the compound amino acid chelated zinc;
step4, weighing 59 parts of concentrated glycine mother liquor, 9 parts of magnesium nitrate hexahydrate, 7 parts of medium elements, 4 parts of trace elements, 16 parts of calcium glycine chelate in Step2, 5 parts of zinc compound amino acid chelate in Step3 and 88 parts of deionized water for later use;
step5, mixing the glycine concentrated mother liquor in Step4 with one half of deionized water, uniformly stirring, adding the glycine chelated calcium and the compound amino acid chelated zinc in parts by weight, and stirring again to obtain a first component;
step6, mixing the magnesium nitrate hexahydrate, the secondary elements, the trace elements and the balance of deionized water in Step4, and stirring uniformly to obtain a second component;
and Step7, mixing the first component and the second component, uniformly stirring, filtering to remove impurities, and heating and concentrating to half of the original volume to obtain the Gly-containing water-soluble fertilizer.
The preparation method of the glycine concentrated mother liquor comprises the following steps:
step1, pouring chloroacetic acid, methanol and urotropine into a reactor, stirring and dissolving, slowly introducing liquid ammonia, carrying out synthetic reaction for 2 hours at the temperature of 59 ℃, and maintaining the pH of a reaction system to be 8 in the reaction process, wherein the molar ratio of chloroacetic acid to methanol to urotropine is 1:7.5:0.2;
step2, after the reaction in the step1 is finished, keeping the temperature until crystals are separated out, cooling to room temperature, centrifuging, filtering to obtain mother liquor and crystals, washing the crystals for 2 times by using a small amount of methanol, mixing washing liquor obtained by washing with the mother liquor, and taking the washing liquor as a circulating reaction solvent;
step3, taking the cyclic reaction solvent in the step2 as a reaction medium for the next cyclic reaction to use, and obtaining mother liquor and a crystal after the last cyclic reaction is finished;
and 4, washing the crystal in the step3 for 2 times by using methanol, mixing the washed washing liquid with the mother liquor in the step3, and simply distilling the mixed washing liquid to obtain the glycine concentrated mother liquor.
The stirring speed in the step1 is 500r/min, and the centrifugal rotating speed in the step2 is 8000r/min.
The number of the cyclic reaction in step3 was 3.
The heat concentration in Step1 was carried out with stirring.
The amount of deionized water in Step2 is 3 times of the total amount of calcium nitrate tetrahydrate and refined glycine.
The preparation method of the compound amino acid in Step3 comprises the following steps: weighing 18 parts of lysine, 1 part of glutamic acid, 0.4 part of alanine, 0.04 part of valine and 0.2 part of phenylalanine according to parts by weight, mixing uniformly to obtain the compound amino acid.
The medium element in Step4 is hydrated sodium silicate.
The trace element in Step4 is prepared by mixing boric acid and ferrous sulfate according to the same weight ratio.
The stirring speed in Step5 and Step6 was 700r/min.
Comparative example:
an amino acid-containing water-soluble fertilizer randomly selected in the market.
Performance detection
Randomly dividing 4 test fields of 3 m multiplied by 10m in the test field, planting tomatoes of the same variety according to the same planting mode, reserving one test field without spraying fertilizer to be recorded as a blank group, spraying the water-soluble fertilizers in the examples 1-3 and the comparative example to the other four test fields respectively to be recorded as the examples 1, 2, 3 and the comparative example, and recording the tomato yield of different test fields, wherein the recorded data are shown in the following table:
| test field | Example 1 | Example 2 | Example 3 | Comparative example | Blank group |
| Average mu yield (kilogram) | 4536 | 4329 | 4598 | 2721 | 1815 |
The data in the table show that the tomato yield per mu of the test Tian Shili-3 is significantly higher than the comparative and blank groups, thus indicating that the Gly water-soluble fertilizer produced by the inventive examples 1-3 contributes to the improvement of the crop yield; therefore, the Gly-containing water-soluble fertilizer prepared by the invention has better application prospect and market popularization value.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising a … …" does not exclude the presence of another identical element in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for producing a Gly-containing water-soluble fertilizer is characterized by comprising the following steps:
step1, measuring 100 parts by weight of glycine concentrated mother liquor for later use, diluting the glycine concentrated mother liquor by using methanol with the same amount, filtering to remove impurities after dilution is finished, adding the obtained solution into a dilute chamber charging basket of an electrodialyzer, adding distilled water into a concentrated chamber charging basket of the electrodialyzer, performing electrodialysis separation to obtain a dilute chamber solution and a concentrated chamber solution, heating and concentrating the dilute chamber solution at the temperature of 70-100 ℃ until glycine is crystallized and separated out, separating a crystal from the mother liquor by filtering, drying to obtain refined glycine, and recycling the crystallized and filtered mother liquor;
step2, as per 2:3, weighing calcium nitrate tetrahydrate and refined glycine in Step1, mixing the calcium nitrate tetrahydrate and the refined glycine with deionized water, stirring the mixture for 5 to 10 minutes at the speed of 300 to 400r/min to prepare a suspension, adjusting the pH of the suspension to 5.5 by using hydrochloric acid or ammonia water, heating the suspension to 50 ℃, pouring the suspension into a high-pressure fluid nano mill for treatment until the suspension becomes clear, drying the clear suspension at a low temperature under reduced pressure, filtering the suspension into fine powder by using a 100 to 200-mesh screen, and obtaining the fine powder which is recorded as glycine chelated calcium;
step3, weighing a certain amount of compound amino acid, dissolving the compound amino acid in deionized water with the weight 2-3 times of the weight of the compound amino acid, filtering to remove insoluble substances, adjusting the pH to 5 by using a sodium hydroxide solution, adding zinc sulfate heptahydrate with the weight of 20-30% of the compound amino acid, reacting for 30min at the water bath temperature of 60 ℃, heating, concentrating, cooling, crystallizing, filtering and drying crystals to obtain the compound amino acid chelated zinc;
step4, weighing 58-60 parts by weight of concentrated glycine mother liquor, 8-9 parts by weight of magnesium nitrate hexahydrate, 5-8 parts by weight of medium elements, 3-5 parts by weight of trace elements, 15-18 parts by weight of calcium glycine chelate in Step2, 4-5 parts by weight of zinc amino acid complex chelate in Step3 and 85-90 parts by weight of deionized water for later use;
step5, mixing the glycine concentrated mother liquor in Step4 with one half of deionized water, uniformly stirring, adding the glycine chelated calcium and the compound amino acid chelated zinc in parts by weight, and stirring again to obtain a first component;
step6, mixing magnesium nitrate hexahydrate, secondary elements, trace elements and the balance of deionized water in Step4, and stirring uniformly to obtain a second component;
and Step7, mixing the first component and the second component, uniformly stirring, filtering to remove impurities, and heating and concentrating to half of the original volume to obtain the Gly-containing water-soluble fertilizer.
2. The method for producing the Gly-containing water-soluble fertilizer according to claim 1, wherein the method for preparing the mother solution of concentrated glycine comprises the following steps:
step1, pouring chloroacetic acid, methanol and urotropine into a reactor, stirring and dissolving, slowly introducing liquid ammonia, carrying out synthetic reaction for 2 hours at the temperature of 58-60 ℃, and maintaining the pH of a reaction system to be 7-8 in the reaction process, wherein the molar ratio of chloroacetic acid to methanol to urotropine is 1:7.5:0.2;
step2, after the reaction in the step1 is finished, keeping the temperature until crystals are separated out, cooling to room temperature, centrifuging, filtering to obtain mother liquor and crystals, washing the crystals for 2 times by using a small amount of methanol, mixing washing liquor obtained by washing with the mother liquor, and taking the washing liquor as a circulating reaction solvent;
3, taking the cyclic reaction solvent in the step2 as a reaction medium for the next cyclic reaction to obtain mother liquor and a crystal until the last cyclic reaction is finished;
and 4, washing the crystal in the step3 for 2 times by using methanol, mixing the washed washing liquid with the mother liquor in the step3, and simply distilling the mixed washing liquid to obtain the glycine concentrated mother liquor.
3. The method for producing the Gly-containing water-soluble fertilizer according to claim 2, wherein the stirring speed in the step1 is 500-600r/min, and the centrifugal rotation speed in the step2 is 7000-8000r/min.
4. The method for producing the Gly-containing water-soluble fertilizer according to claim 2, wherein the number of the circulating reactions in the step3 is 3-4.
5. The method for producing the Gly-containing water-soluble fertilizer according to claim 1, wherein Step1 is heated and concentrated under the condition of continuous stirring.
6. The method for producing the Gly-containing water-soluble fertilizer according to claim 1, wherein the amount of the deionized water in Step2 is 3-4 times of the total amount of the calcium nitrate tetrahydrate and the refined glycine.
7. The method for producing the Gly-containing water-soluble fertilizer according to claim 1, wherein the method for preparing the compound amino acid in Step3 comprises the following steps: weighing 17-18 parts of lysine, 1-2 parts of glutamic acid, 0.3-0.5 part of alanine, 0.03-0.05 part of valine and 0.1-0.3 part of phenylalanine according to parts by weight, mixing uniformly to obtain the compound amino acid.
8. The process for producing a Gly-containing water-soluble fertilizer according to claim 1, wherein the medium element in Step4 is sodium silicate hydrate.
9. The method for producing the Gly-containing water-soluble fertilizer according to claim 1, wherein the trace element in Step4 is boric acid and ferrous sulfate which are mixed according to the same weight ratio.
10. The method for producing the Gly-containing water-soluble fertilizer according to claim 1, wherein the stirring speed in Step5 and Step6 is 600-800r/min.
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