CN111662198A - Preparation method of zinc glycinate chelate - Google Patents

Preparation method of zinc glycinate chelate Download PDF

Info

Publication number
CN111662198A
CN111662198A CN202010512871.7A CN202010512871A CN111662198A CN 111662198 A CN111662198 A CN 111662198A CN 202010512871 A CN202010512871 A CN 202010512871A CN 111662198 A CN111662198 A CN 111662198A
Authority
CN
China
Prior art keywords
zinc
zinc glycinate
glycinate chelate
glycine
water
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010512871.7A
Other languages
Chinese (zh)
Inventor
高波
吕宗良
刘忠义
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sichuan Ailong Plant Nutrition Technology Co ltd
Original Assignee
Sichuan Ailong Plant Nutrition Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sichuan Ailong Plant Nutrition Technology Co ltd filed Critical Sichuan Ailong Plant Nutrition Technology Co ltd
Priority to CN202010512871.7A priority Critical patent/CN111662198A/en
Publication of CN111662198A publication Critical patent/CN111662198A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/14Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
    • C07C227/18Preparation 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
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/38Separation; Purification; Stabilisation; Use of additives
    • C07C227/40Separation; Purification
    • C07C227/42Crystallisation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07BGENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B2200/00Indexing scheme relating to specific properties of organic compounds
    • C07B2200/13Crystalline forms, e.g. polymorphs

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a preparation method of a zinc glycinate chelate, which is used for solving the problem that water in zinc glycinate is difficult to remove, belongs to the technical field of trace element fertilizers, and comprises the following steps: dissolving glycine in distilled water, adding an inorganic zinc salt and a catalyst, reacting for 0.5-1.0 h at 50-70 ℃, crystallizing and separating to obtain a crystalline solid, removing impurities and drying to obtain a zinc glycinate chelate, wherein nano diamond powder with the total mass of 0.08-0.5 per mill of the reaction liquid is gradually added when the reaction liquid begins to crystallize, and uniformly mixing; according to the invention, by adding the nano-diamond, water and zinc glycinate can be effectively prevented from generating crystal water, the content of the crystal water is reduced, free water among crystals is easy to evaporate, the product is easy to dry, the obtained product is loose and difficult to agglomerate, the dispersibility is good, the product quality is high, and the product is easy to store.

Description

Preparation method of zinc glycinate chelate
Technical Field
A preparation method of zinc glycinate chelate belongs to the technical field of trace element fertilizers, and particularly relates to preparation of zinc-containing chelate.
Background
During the growth of plants, in order to maintain the metabolic process of the plants, a certain amount of nutrient elements need to be continuously absorbed from the outside to maintain the normal operation of the organism, and the nutrient elements can be divided into a large amount of nutrient elements and trace nutrient elements according to the absorption amount of the plants. The trace nutrient elements mainly comprise iron, manganese, boron, zinc, copper, molybdenum, chlorine and nickel, wherein the zinc is absorbed by plants in a cation form and is an irreplaceable trace element in the plant growth process, and the trace nutrient elements mainly have the following functions: (1) in plants, zinc is a constituent of certain enzymes and is also a catalyst for many enzymes; (2) influences on the metabolism of carbohydrates in plants through photosynthesis and sugar transport processes; (3) has close relation with protein metabolism, when the zinc is deficient, the protein synthesis rate and the content in the plant body are reduced, and the amino acid is accumulated and deposited; (4) can enhance the stress resistance and disease resistance of plants; (5) in the aspect of seed germination, the zinc sulfate solution with a certain concentration is used for treating the seeds, so that the germination rate of the seeds can be improved.
The plant is difficult to absorb the inorganic zinc, the absorption and bioavailability of the organic zinc are far higher than those of the inorganic zinc, and meanwhile, the amino acid is used as a carrier to chelate the zinc element and serve as a trace element fertilizer, so that the plant can better absorb the zinc element, the utilization rate is higher, and the accurate and efficient supplement of the zinc element is realized.
In the production process of the zinc glycinate chelate, the prepared wet zinc glycinate crystal needs to be dried to remove moisture so as to reach the qualified standard, the simplest and most efficient method is to increase the drying temperature to be more than 120 ℃, but the zinc glycinate crystal can be decomposed at the temperature of more than 80 ℃, if the zinc glycinate crystal is dried at low temperature, the moisture is not easy to remove, especially crystal water, the drying efficiency is low, and the zinc glycinate crystal is easy to aggregate, agglomerate and cake in the storage process due to the existence of a large amount of moisture, so that the long-term storage is not facilitated, and the product quality is influenced; in order to solve the problems, a preparation method of a zinc glycinate chelate is provided.
Disclosure of Invention
The invention aims to: the preparation method of the zinc glycinate chelate can effectively prevent water and zinc glycinate from generating crystal water, reduce the content of the crystal water, facilitate the evaporation of free water among crystals, facilitate the drying of products, ensure that the obtained products are loose and are not easy to agglomerate, have good dispersibility and high product quality, and are easy to store.
The technical scheme adopted by the invention is as follows:
in order to achieve the above object, the present invention provides a method for preparing a zinc glycinate chelate, comprising the steps of:
dissolving glycine in distilled water, adding an inorganic zinc salt and a catalyst, reacting for 0.5-1.0 h at 50-70 ℃, crystallizing and separating to obtain a crystalline solid, removing impurities and drying to obtain a zinc glycinate chelate, wherein nano diamond powder with the total mass of 0.08-0.5 per mill of the reaction liquid is gradually added when the reaction liquid starts to crystallize, and uniformly mixing, meanwhile, mother liquid after crystallization and separation is recycled and added into the raw materials for reaction, and the recycled and raw materials participate in the reaction together due to the fact that the mother liquid contains a large amount of glycine, zinc glycinate and other substances, the post-treatment is difficult, so that the recycling of the raw materials in the mother liquid can be realized, the environmental pollution is avoided, the treatment difficulty of the mother liquid is reduced, the reaction conversion rate and the yield are improved, and the cost is reduced.
Preferably, the inorganic zinc salt is any one of basic zinc carbonate, zinc sulfate, zinc hydroxide and zinc oxide.
Preferably, the catalyst is acetic acid.
Preferably, the molar ratio of the glycine to the inorganic zinc salt is (2-5) to 1.
Preferably, the molar ratio of the glycine to the catalyst is 1 (0.002-0.01).
Preferably, the impurity removal specifically comprises: the crystalline solid was washed at least 2 times with absolute ethanol. Impurities are removed by washing with ethanol, so that the product purity is higher, the dispersibility is better, the water content is reduced, and the energy consumption is saved for the subsequent drying procedure.
Preferably, the washed washing liquid is rectified by a rectifying tower, and the ethanol is separated and recovered for recycling.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. according to the method, a small amount of nano-diamond powder is gradually added when the zinc glycinate crystal is formed, the specific surface area of the nano-diamond powder is large, the nano-diamond powder has excellent adsorption capacity, and the crystal is not completely formed, so that after the nano-diamond powder is adsorbed by zinc glycinate, a barrier is formed on the surface of the zinc glycinate, water and the zinc glycinate can be effectively prevented from generating crystal water, the content of the crystal water is reduced, and the method is favorable for product storage and product quality improvement.
2. According to the method, a small amount of nano diamond powder is gradually added when the zinc glycinate crystals begin to be formed, and the nano diamond powder is adsorbed on the surfaces of the zinc glycinate crystals, so that the zinc glycinate crystals are separated from one another, are loose and are not easy to agglomerate, and the dispersibility and the quality of products are improved.
3. This send through add a small amount of nano-diamond powder gradually when beginning to form zinc glycinate crystal, nano-diamond powder adsorbs on zinc glycinate crystal surface, has reduced the bridging effect of zinc glycinate crystal inter-particle water for free water between the crystal is changeed in drying process and is evaporated out, need not improve drying temperature, makes drying effect better, and drying efficiency is higher, and the energy consumption reduces, and product moisture content is low, and product quality is high.
Detailed Description
The technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. 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 embodiment provides a preparation method of a zinc glycinate chelate, which comprises the following steps:
(1) dissolving glycine in distilled water, adding basic zinc carbonate and acetic acid, and reacting at 50-70 ℃ for 0.5-1.0 h; wherein, the mol ratio of the glycine to the basic zinc carbonate is 2: 1, and the mol ratio of the glycine to the acetic acid is 1: 0.002;
(2) cooling and crystallizing the reaction liquid, gradually adding nano diamond powder with the total mass of 0.1 per thousand of the reaction liquid when the reaction liquid starts to crystallize, uniformly mixing, carrying out solid-liquid separation after crystallization is finished to obtain a crystalline solid, recycling a mother liquid after crystallization separation, washing the crystalline solid with absolute ethyl alcohol for 2 times to obtain a wet product zinc glycinate chelate, and drying at 50-70 ℃ to obtain the zinc glycinate chelate product.
Example 2
The difference between the embodiment and the embodiment 1 is that in the step (1), the inorganic zinc salt is zinc sulfate, wherein the molar ratio of glycine to zinc sulfate is 3: 1, and the molar ratio of glycine to acetic acid is 1: 0.008; the nano diamond powder added in the step (2) accounts for 0.08 per mill of the total mass of the reaction liquid.
Example 3
The difference between the embodiment and the embodiment 1 is that in the step (1), the inorganic zinc salt is zinc sulfate, wherein the molar ratio of glycine to zinc sulfate is 4: 1, and the molar ratio of glycine to acetic acid is 1: 0.01; the nano diamond powder added in the step (2) accounts for 0.2 per mill of the total mass of the reaction liquid.
Example 4
This example is different from example 1 in that in step (1), the inorganic zinc salt is zinc hydroxide, wherein the molar ratio of glycine to zinc hydroxide is 5: 1, and the molar ratio of glycine to acetic acid is 1: 0.005; the nano diamond powder added in the step (2) accounts for 0.3 per mill of the total mass of the reaction liquid.
Example 5
This example is different from example 1 in that in step (1), the inorganic zinc salt is zinc hydroxide, wherein the molar ratio of glycine to zinc hydroxide is 3.5: 1, and the molar ratio of glycine to acetic acid is 1: 0.004; the nano diamond powder added in the step (2) accounts for 0.4 per mill of the total mass of the reaction liquid.
Example 6
The difference between the embodiment and the embodiment 1 is that in the step (1), the inorganic zinc salt is zinc sulfate, wherein the molar ratio of glycine to zinc sulfate is 4: 1, and the molar ratio of glycine to acetic acid is 1: 0.002; the nano diamond powder added in the step (2) accounts for 0.1 per mill of the total mass of the reaction liquid.
Example 7
The difference between the embodiment and the embodiment 1 is that in the step (1), the inorganic zinc salt is zinc sulfate, wherein the molar ratio of glycine to zinc sulfate is 5: 1, and the molar ratio of glycine to acetic acid is 1: 0.01; the nano diamond powder added in the step (2) accounts for 0.5 per mill of the total mass of the reaction liquid.
Example 8
The difference between the embodiment and the embodiment 1 is that in the step (1), the inorganic zinc salt is zinc sulfate, wherein the molar ratio of glycine to zinc sulfate is 2: 1, and the molar ratio of glycine to acetic acid is 1: 0.007; the nano diamond powder added in the step (2) accounts for 0.35 per mill of the total mass of the reaction liquid.
The components of the product are detected, and the product of the invention is zinc (Zn)2+Calculated) is more than or equal to 25.4 percent; the total glycine is more than or equal to 57.5 percent; the product quality is good when the free glycine is less than or equal to 0.8 percent, and other detection data are shown in the table I.
Table one, product inspection data of the present invention
Figure BDA0002529041080000041
As can be seen from the table I, the product prepared by the invention has better quality, high purity and low water content, and meets the product standard.
Finally, it should be noted that: 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 or all of the technical features may be equivalently replaced; these modifications and substitutions do not cause the essence of the corresponding technical solution to depart from the scope of the technical solution of the embodiments of the present invention, and are intended to be covered by the claims and the specification of the present invention.

Claims (7)

1. The preparation method of the zinc glycinate chelate is characterized by comprising the following steps of:
dissolving glycine in distilled water, adding an inorganic zinc salt and a catalyst, reacting for 0.5-1.0 h at 50-70 ℃, crystallizing and separating to obtain a crystalline solid, removing impurities, and drying to obtain a zinc glycinate chelate, wherein nano diamond powder with the total mass of 0.08-0.5 per mill of the reaction liquid is gradually added when the reaction liquid begins to crystallize, and uniformly mixing.
2. The method for preparing zinc glycinate chelate according to claim 1, wherein any one of basic zinc carbonate, zinc sulfate, zinc hydroxide and zinc oxide is adopted as the inorganic zinc salt.
3. The method of claim 1, wherein the catalyst is acetic acid.
4. The method for preparing the zinc glycinate chelate according to claim 1, wherein the molar ratio of the glycine to the inorganic zinc salt is (2-5) to 1.
5. The method for preparing the zinc glycinate chelate according to claim 1, wherein the molar ratio of the glycine to the catalyst is 1 (0.002-0.01).
6. The preparation method of the zinc glycinate chelate according to claim 1, characterized in that the impurity removal is specifically: the crystalline solid was washed at least 2 times with absolute ethanol.
7. The preparation method of the zinc glycinate chelate according to claim 6, wherein the washed washing liquid is rectified by a rectifying tower, and the ethanol is separated and recovered for recycling.
CN202010512871.7A 2020-06-08 2020-06-08 Preparation method of zinc glycinate chelate Pending CN111662198A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010512871.7A CN111662198A (en) 2020-06-08 2020-06-08 Preparation method of zinc glycinate chelate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010512871.7A CN111662198A (en) 2020-06-08 2020-06-08 Preparation method of zinc glycinate chelate

Publications (1)

Publication Number Publication Date
CN111662198A true CN111662198A (en) 2020-09-15

Family

ID=72387004

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010512871.7A Pending CN111662198A (en) 2020-06-08 2020-06-08 Preparation method of zinc glycinate chelate

Country Status (1)

Country Link
CN (1) CN111662198A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113105352A (en) * 2021-04-16 2021-07-13 铂尊投资集团有限公司 Method for preparing food-grade and feed-grade zinc glycinate and implementation device thereof
CN115819263A (en) * 2022-12-07 2023-03-21 贵州大学 Organic zinc-selenium chelate, functional fertilizer, and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107652196A (en) * 2017-10-20 2018-02-02 衡阳德邦新金生物科技有限公司 A kind of removal technique of the glycine zine crystallization water
CN109480095A (en) * 2019-01-03 2019-03-19 常宁德邦生物科技有限公司 A kind of preparation method of loose non-caking feed addictive glycine zine
CN110041215A (en) * 2019-05-09 2019-07-23 河北力维素科技有限公司 A kind of preparation method of food-grade glycine zine chelate

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107652196A (en) * 2017-10-20 2018-02-02 衡阳德邦新金生物科技有限公司 A kind of removal technique of the glycine zine crystallization water
CN109480095A (en) * 2019-01-03 2019-03-19 常宁德邦生物科技有限公司 A kind of preparation method of loose non-caking feed addictive glycine zine
CN110041215A (en) * 2019-05-09 2019-07-23 河北力维素科技有限公司 A kind of preparation method of food-grade glycine zine chelate

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113105352A (en) * 2021-04-16 2021-07-13 铂尊投资集团有限公司 Method for preparing food-grade and feed-grade zinc glycinate and implementation device thereof
CN115819263A (en) * 2022-12-07 2023-03-21 贵州大学 Organic zinc-selenium chelate, functional fertilizer, and preparation method and application thereof

Similar Documents

Publication Publication Date Title
CN102390844B (en) Preparation process of large-grain ammonium sulfate crystals
CN111662198A (en) Preparation method of zinc glycinate chelate
CN109052434B (en) Method for jointly producing soda ash and composite nitrogen fertilizer by taking mirabilite and ammonium bicarbonate as raw materials
CN111892067B (en) Preparation method and application of salt-making brine and large-particle high-calcium salt
CN103496715A (en) Method for producing industrial grade superior ammonium sulfate through coked coarse ammonium sulfate dilution crystallization
CN113651306A (en) Preparation method of lithium difluorophosphate
CN110963826A (en) Method for preparing phosphate concentrate and by-product calcium magnesium nitrate liquid fertilizer by chemical beneficiation
CN110668488A (en) Production method of zinc sulfate monohydrate
CN110668489A (en) Method for preparing zinc sulfate monohydrate from zinc-containing waste residue
CN1736870A (en) Method for preparing potassium nitrate using nitric acid conversion methdo
CN102491406B (en) Method for preparing gallium sulfate
CN103397111A (en) Preparation method of granulated crystal sugar
CN102372292A (en) Technology for preparing potassium sulfate with potassium-rich mother liquid and phosphogypsum
CN111777523A (en) Preparation method of glycine iron chelate
CN114702075A (en) Purification preparation method of manganese sulfate
CN111646914A (en) Preparation method of copper glycine chelate
CN109480095B (en) Preparation method of loose and non-caking feed additive zinc glycinate
CN102617219A (en) Production method of amino acid foliar-fertilizer
CN115535979B (en) Potassium dihydrogen phosphate and method for preparing potassium dihydrogen phosphate by using calcium hydrogen phosphate
CN103496716B (en) Method for producing industrial excellent ammonium sulfate through coarse ammonium sulfate coking coupling evaporation solventing-out crystallization
CN1212270C (en) Improved process for producing sodium ferrocyanide and potassium ferrocyanide
CN110790685A (en) Method for producing urea phosphate by wet-process phosphoric acid reduced pressure evaporation coupled elution crystallization
CN104843745B (en) A kind of control method of double decomposition potassium nitrate product granularity
CN103496714A (en) Method for producing industrial grade superior ammonium sulfate through coked coarse ammonium sulfate
CN103497132B (en) Utilize D, the saponification liquor that L-Methionine is produced prepares N-methylol-D, the method for L-Methionine calcium

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20200915

WD01 Invention patent application deemed withdrawn after publication