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CN113303337A - Production method of copper calcium sulfate - Google Patents

Production method of copper calcium sulfate Download PDF

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Publication number
CN113303337A
CN113303337A CN202110614726.4A CN202110614726A CN113303337A CN 113303337 A CN113303337 A CN 113303337A CN 202110614726 A CN202110614726 A CN 202110614726A CN 113303337 A CN113303337 A CN 113303337A
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CN
China
Prior art keywords
calcium sulfate
copper
reactor
copper calcium
stirring
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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
CN202110614726.4A
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Chinese (zh)
Inventor
盛勤明
黄勇键
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.)
Wujiang Weishida Copper Technology Co ltd
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Wujiang Weishida Copper Technology Co ltd
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Filing date
Publication date
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Priority to CN202110614726.4A priority Critical patent/CN113303337A/en
Publication of CN113303337A publication Critical patent/CN113303337A/en
Pending legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16Heavy metals; Compounds thereof
    • A01N59/20Copper
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/12Powders or granules
    • A01N25/14Powders or granules wettable
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05DINORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D3/00Calcareous fertilisers
    • C05D3/02Calcareous fertilisers from limestone, calcium carbonate, calcium hydrate, slaked lime, calcium oxide, waste calcium products
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G3/00Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/60Biocides or preservatives, e.g. disinfectants, pesticides or herbicides; Pest repellants or attractants
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G5/00Fertilisers characterised by their form
    • C05G5/20Liquid fertilisers

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  • Life Sciences & Earth Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Dentistry (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a production method of copper calcium sulfate, which comprises the following steps: the method comprises the following steps: adding water into the first reactor, stirring, adding calcium oxide into the first reactor, and uniformly stirring to obtain a suspension; step two: adding water into the second reactor, stirring, and adding copper sulfate pentahydrate into the second reactor to obtain a copper sulfate pentahydrate solution; step three: heating the second reactor to 85-95 ℃ to obtain a heated copper sulfate pentahydrate solution; step four: adding a copper sulfate pentahydrate solution into a first reactor to obtain copper calcium sulfate slurry; step five: removing water from the copper calcium sulfate slurry to obtain copper calcium sulfate; step six: transferring the copper calcium sulfate into a vacuum drying oven for baking to obtain dried copper calcium sulfate; step seven: and crushing the dried copper calcium sulfate and packaging to obtain a finished product. The copper calcium sulfate prepared by the method has high effective copper content, less copper calcium sulfate is used for producing the copper calcium sulfate wettable powder, the cost is low, the vacuum drying of the copper calcium sulfate is realized, the structure is loose, the surface area is large, the suspension force is strong, and the dispersion performance is good.

Description

Production method of copper calcium sulfate
Technical Field
The invention relates to the field of medicine production, in particular to a production method of copper calcium sulfate.
Background
For fungal diseases on fruit trees and vegetables, the use of copper sulfate solution for control has a long history. When the copper sulfate solution is sprayed on the surface of a plant, copper ions in the copper sulfate solution enter pathogenic fungi or bacteria and are combined with biological groups to form substances such as a copper complex and the like, so that protein is denatured, metabolism is hindered and inhibited, germs die, and the purpose of sterilization is achieved.
The copper sulfate solution is prepared from copper sulfate and water according to a certain proportion. The proportion of copper sulfate and water is changed according to the spraying object, season and temperature, and the copper sulfate and water are prepared for use when in use, and are easy to deteriorate and lose efficacy if not used after long-term preparation. This results in not only troublesome use process but also a great decrease in the bactericidal effect due to the greater randomness of the copper sulfate solution when it is prepared. Meanwhile, if the copper sulfate solution is incorrectly prepared and is not standard in the using process, the leaves of the plants are easily roughened, the photosynthesis is reduced, and the growth of the plants is not facilitated. The copper sulfate solution is used as a bactericide slowly at present for various reasons, and cannot keep pace with the demand of the times.
In order to solve the problems of using a copper sulfate solution as a bactericide in the process, a pesticide manufacturer produces a copper calcium sulfate wettable powder with 77 percent of active ingredients, wherein a copper calcium sulfate raw pesticide is used as a main ingredient and accounts for 77 percent, and other additives are added. The 77% copper calcium sulfate wettable powder has the excellent sterilizing characteristic of copper sulfate, can overcome various defects of the traditional copper sulfate as a sterilizing agent in the using process, has flexible and various using methods, simple and convenient operation, high efficiency and reliability, can be used for preventing and treating diseases on the ground by spraying besides being used on plants and preventing the spread of soil diseases and insect pests. The composite calcium ion bactericide has stable bactericidal effect and longer lasting period, not only has the performance characteristics of the copper sulfate solution as the bactericide, but also can supplement nutrient calcium elements required by plants in the sterilization process due to the composite calcium ions, has the calcium supplementing effect like a human body, can improve the disease resistance of the plants and promote the growth of the plants, has the advantage of no copper sulfate solution, and is an excellent substitute of the copper sulfate solution as the bactericide.
The main component of the 77% copper calcium sulfate wettable powder is copper calcium sulfate, most of the copper calcium sulfate used by the domestic 77% copper calcium sulfate wettable powder manufacturer is imported from abroad, the cost is high, and the procurement time is long.
Disclosure of Invention
The invention solves the technical problem of providing a production method of copper calcium sulfate which is not purchased from foreign countries, can be manufactured by self, has low cost and convenient use.
The technical scheme adopted by the invention for solving the technical problems is as follows: the production method of copper calcium sulfate comprises a first reactor, a second reactor and a vacuum drying oven, and also comprises the following steps:
the method comprises the following steps: adding water into a first reactor at normal temperature, stirring, adding calcium oxide which is 10-20% of the water into the first reactor while stirring, and uniformly stirring to obtain suspension of 10-20 g/L;
step two: adding water into the second reactor, stirring, and adding 15-30% of blue vitriod of water into the second reactor while stirring to obtain 15-30% blue vitriod solution;
step three: heating the second reactor to 85-95 ℃ to obtain a heated copper sulfate pentahydrate solution;
step four: slowly adding the heated copper sulfate pentahydrate solution obtained in the step three into the first reactor, mixing with the suspension obtained in the step one, and simultaneously heating to 85-95 ℃ to obtain synthesized copper calcium sulfate slurry;
step five: filtering the copper calcium sulfate slurry obtained in the fourth step to remove most of water, so as to obtain filtered copper calcium sulfate;
step six: transferring the filtered copper calcium sulfate obtained in the fifth step into a vacuum drying oven for baking to obtain dried copper calcium sulfate, wherein the active ingredients of the copper calcium sulfate can be reserved by vacuum drying of the copper calcium sulfate, and the produced copper calcium sulfate has loose structure, large surface area, strong suspension force and good dispersibility. Therefore, the pesticide manufacturer uses less copper calcium sulfate when producing 77% copper calcium sulfate wettable powder, and has high efficiency and strong bactericidal capability in actual use.
Step seven: and C, crushing the dried copper calcium sulfate obtained in the step six, and then packaging to obtain a finished product.
Further, the method comprises the following steps: and the mixing time in the fourth step is 4-5 hours.
Further, the method comprises the following steps: the pH value of the copper calcium sulfate slurry synthesized in the fourth step is 5-8, so that the calcium oxide in the fourth step can be completely consumed, and the synthesis reaction is finished.
Further, the method comprises the following steps: the flow rate of the blue vitriod solution added in the fourth step is 100-150L/min.
Further, the method comprises the following steps: and the baking time in the sixth step is 15-20 h.
Further, the method comprises the following steps: and the temperature range of baking in the sixth step is 90-95 ℃.
Further, the method comprises the following steps: and in the sixth step, the vacuum degree in the vacuum drying oven is-0.06 to-0.095 MPa.
The invention has the beneficial effects that: the effective copper content of the copper calcium sulfate manufactured by the method is 2-3% higher than that of the currently sold copper calcium sulfate, so that a pesticide manufacturer uses less copper calcium sulfate when producing 77% copper calcium sulfate wettable powder, the efficiency is high when the pesticide manufacturer actually uses the copper calcium sulfate, the sterilization capability is strong, the vacuum drying of the copper calcium sulfate is used in the invention, the effective components of the copper calcium sulfate can be reserved, and the produced copper calcium sulfate has loose structure, large surface area, strong suspension force and good dispersion performance.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The production method of copper calcium sulfate comprises a first reactor, a second reactor and a vacuum drying oven, and also comprises the following steps:
the method comprises the following steps: adding water into a first reactor at normal temperature, stirring, adding calcium oxide which is 10-20% of the water into the first reactor while stirring, and uniformly stirring to obtain suspension of 10-20 g/L;
step two: adding water into the second reactor, stirring, and adding 15-30% of blue vitriod of water into the second reactor while stirring to obtain 15-30% blue vitriod solution;
step three: heating the second reactor to 85-95 ℃ to obtain a heated copper sulfate pentahydrate solution;
step four: slowly adding the heated copper sulfate pentahydrate solution obtained in the third step into a first reactor, mixing with the suspension obtained in the first step, and simultaneously heating to 85-95 ℃ to obtain synthesized copper calcium sulfate slurry;
step five: filtering the copper calcium sulfate slurry obtained in the fourth step to remove most of water, so as to obtain filtered copper calcium sulfate;
step six: transferring the filtered copper calcium sulfate obtained in the fifth step into a vacuum drying oven for baking to obtain dried copper calcium sulfate, wherein the active ingredients of the copper calcium sulfate can be reserved by vacuum drying of the copper calcium sulfate, and the produced copper calcium sulfate has loose structure, large surface area, strong suspension force and good dispersibility. Therefore, the pesticide manufacturer uses less copper calcium sulfate when producing 77% copper calcium sulfate wettable powder, and has high efficiency and strong bactericidal capability in actual use.
Step seven: and C, crushing the dried copper calcium sulfate obtained in the step six, and then packaging to obtain a finished product.
On the basis, the mixing time in the fourth step is 4-5 hours.
On the basis, the pH value of the copper calcium sulfate slurry synthesized in the fourth step is 5-8, so that the calcium oxide in the fourth step can be completely consumed, and the synthesis reaction is finished.
On the basis, the flow rate of the copper sulfate pentahydrate solution added in the fourth step is 100-150L/min.
On the basis, the baking time in the sixth step is 15-20 h.
On the basis, the temperature range of baking in the sixth step is 90-95 ℃.
On the basis, the vacuum degree in the vacuum drying oven in the sixth step is-0.06 to-0.095 MPa.
The first embodiment is as follows:
the method comprises the following steps: adding 1000L of water into a first reactor at normal temperature, stirring, adding 10Kg of calcium oxide into the first reactor while stirring, and uniformly stirring to obtain 10g/L suspension;
step two: adding 500L of water into the second reactor, stirring, and adding 75Kg of blue vitriol into the second reactor while stirring to obtain 15% blue vitriol solution;
step three: heating the second reactor to 85 ℃ to obtain a heated copper sulfate pentahydrate solution;
step four: slowly adding the heated copper sulfate pentahydrate solution obtained in the third step into a first reactor, mixing with the suspension obtained in the first step, and simultaneously heating to 85-95 ℃ to obtain synthesized copper calcium sulfate slurry;
step five: filtering the copper calcium sulfate slurry obtained in the fourth step to remove most of water, so as to obtain filtered copper calcium sulfate;
step six: transferring the filtered copper calcium sulfate obtained in the fifth step into a vacuum drying oven for baking at 90 ℃ and the vacuum degree of-0.090 MPa for 18h to obtain dried copper calcium sulfate;
step seven: and C, crushing the dried copper calcium sulfate obtained in the step six, and then packaging to obtain a finished product.
Example two:
the method comprises the following steps: adding 800L of water into a first reactor at normal temperature, stirring, adding 16Kg of calcium oxide into the first reactor while stirring, and uniformly stirring to obtain 20g/L suspension;
step two: adding 400L of water into the second reactor, stirring, and adding 120Kg of blue copperas into the second reactor while stirring to obtain 30% blue copperas solution;
step three: heating the second reactor to 95 ℃ to obtain a heated copper sulfate pentahydrate solution;
step four: slowly adding the heated copper sulfate pentahydrate solution obtained in the third step into a first reactor, mixing with the suspension obtained in the first step, and simultaneously heating to 85-95 ℃ to obtain synthesized copper calcium sulfate slurry;
step five: filtering the copper calcium sulfate slurry obtained in the fourth step to remove most of water, so as to obtain filtered copper calcium sulfate;
step six: transferring the filtered copper calcium sulfate obtained in the fifth step into a vacuum drying oven for baking at the baking temperature of 95 ℃ and the vacuum degree of-0.075 MPa for 15 hours to obtain dried copper calcium sulfate;
step seven: and C, crushing the dried copper calcium sulfate obtained in the step six, and then packaging to obtain a finished product.
Example three:
the method comprises the following steps: adding 1500L of water into a first reactor at normal temperature, stirring, adding 22.5Kg of calcium oxide into the first reactor while stirring, and uniformly stirring to obtain 15g/L of suspension;
step two: adding 500L of water into the second reactor, stirring, and adding 100Kg of blue vitriol into the second reactor while stirring to obtain 20% blue vitriol solution;
step three: heating the second reactor to 90 ℃ to obtain a heated copper sulfate pentahydrate solution;
step four: slowly adding the heated copper sulfate pentahydrate solution obtained in the third step into a first reactor, mixing with the suspension obtained in the first step, and simultaneously heating to 85-95 ℃ to obtain synthesized copper calcium sulfate slurry;
step five: filtering the copper calcium sulfate slurry obtained in the fourth step to remove most of water, so as to obtain filtered copper calcium sulfate;
step six: transferring the filtered copper calcium sulfate obtained in the fifth step into a vacuum drying oven for baking at the baking temperature of 93 ℃ and the vacuum degree of-0.06 MPa for 20 hours to obtain dried copper calcium sulfate;
step seven: and C, crushing the dried copper calcium sulfate obtained in the step six, and then packaging to obtain a finished product.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. The production method of copper calcium sulfate comprises a first reactor, a second reactor and a vacuum drying oven, and is characterized in that: also comprises the following steps:
the method comprises the following steps: adding water into a first reactor at normal temperature, stirring, adding calcium oxide which is 10-20% of the water into the first reactor while stirring, and uniformly stirring to obtain suspension of 10-20 g/L;
step two: adding water into the second reactor, stirring, and adding 15-30% of blue vitriod of water into the second reactor while stirring to obtain 15-30% blue vitriod solution;
step three: heating the second reactor to 85-95 ℃ to obtain a heated copper sulfate pentahydrate solution;
step four: slowly adding the heated copper sulfate pentahydrate solution obtained in the third step into a first reactor, mixing with the suspension obtained in the first step, and simultaneously heating to 85-95 ℃ to obtain synthesized copper calcium sulfate slurry;
step five: filtering the copper calcium sulfate slurry obtained in the fourth step to remove most of water, so as to obtain filtered copper calcium sulfate;
step six: transferring the filtered copper calcium sulfate obtained in the fifth step into a vacuum drying oven for baking to obtain dried copper calcium sulfate;
step seven: and C, crushing the dried copper calcium sulfate obtained in the step six, and then packaging to obtain a finished product.
2. The method for producing copper calcium sulfate according to claim 1, wherein: and the mixing time in the fourth step is 4-5 hours.
3. The method for producing copper calcium sulfate according to claim 1, wherein: and the pH value of the copper calcium sulfate slurry synthesized in the fourth step is 5-8.
4. The method for producing copper calcium sulfate according to claim 1, wherein: the flow rate of the blue vitriod solution added in the fourth step is 100-150L/min.
5. The method for producing copper calcium sulfate according to claim 1, wherein: and the baking time in the sixth step is 15-20 h.
6. The method for producing copper calcium sulfate according to claim 1, wherein: and the temperature range of baking in the sixth step is 90-95 ℃.
7. The method for producing copper calcium sulfate according to claim 1, wherein: and in the sixth step, the vacuum degree in the vacuum drying oven is-0.06 to-0.095 MPa.
CN202110614726.4A 2021-06-02 2021-06-02 Production method of copper calcium sulfate Pending CN113303337A (en)

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CN202110614726.4A CN113303337A (en) 2021-06-02 2021-06-02 Production method of copper calcium sulfate

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Application Number Priority Date Filing Date Title
CN202110614726.4A CN113303337A (en) 2021-06-02 2021-06-02 Production method of copper calcium sulfate

Publications (1)

Publication Number Publication Date
CN113303337A true CN113303337A (en) 2021-08-27

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113968588A (en) * 2021-11-19 2022-01-25 吴江市威士达铜业科技有限公司 A kind of production method of copper oxide

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070003635A1 (en) * 2003-04-16 2007-01-04 Frederic Ferrier Method of producing copper hydoroxosulphates and copper fungicidal compositions containing same
US20180263246A1 (en) * 2015-07-01 2018-09-20 Phytoncide Lab Co., Ltd. Highly concentrated high-functional lime bordeaux liquid and method for preparing same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070003635A1 (en) * 2003-04-16 2007-01-04 Frederic Ferrier Method of producing copper hydoroxosulphates and copper fungicidal compositions containing same
US20180263246A1 (en) * 2015-07-01 2018-09-20 Phytoncide Lab Co., Ltd. Highly concentrated high-functional lime bordeaux liquid and method for preparing same

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘琪 编著: "《有机梅生产技术》", 30 September 2008, 金盾出版社 *
邱强 主编: "《原色葡萄病虫图谱》", 31 March 2000, 中国科学技术出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113968588A (en) * 2021-11-19 2022-01-25 吴江市威士达铜业科技有限公司 A kind of production method of copper oxide

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Application publication date: 20210827