CN110776413A - Preparation method and application of manganese abietate - Google Patents
Preparation method and application of manganese abietate Download PDFInfo
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- CN110776413A CN110776413A CN201911054372.1A CN201911054372A CN110776413A CN 110776413 A CN110776413 A CN 110776413A CN 201911054372 A CN201911054372 A CN 201911054372A CN 110776413 A CN110776413 A CN 110776413A
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- manganese
- rosinate
- rosin
- water
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing carboxylic groups or thio analogues thereof, directly attached by the carbon atom to a cycloaliphatic ring; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/418—Preparation of metal complexes containing carboxylic acid moieties
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2603/00—Systems containing at least three condensed rings
- C07C2603/02—Ortho- or ortho- and peri-condensed systems
- C07C2603/04—Ortho- or ortho- and peri-condensed systems containing three rings
- C07C2603/22—Ortho- or ortho- and peri-condensed systems containing three rings containing only six-membered rings
- C07C2603/26—Phenanthrenes; Hydrogenated phenanthrenes
Abstract
The invention discloses a preparation method and application of manganese rosinate, and belongs to the technical field of pesticides. The preparation method of the manganese rosinate comprises the following steps: step 1: weighing manganese salt, adding water and stirring to prepare a manganese salt aqueous solution; step 2: weighing rosin, adding a reaction medium, adding alkali, heating and stirring for reaction to completely dissolve the rosin to obtain dissolved rosin; and step 3: adding a manganese salt aqueous solution into the dissolved rosin, heating and stirring the mixture, and reacting the mixture to obtain a reacted mixed solution; and 4, step 4: when the reaction medium is water, cooling the reacted mixed solution to room temperature, filtering with water, and drying to obtain solid manganese rosinate; and when the reaction medium is an organic solvent, recovering the reflux condensate, discharging and cooling to obtain the liquid manganese rosinate. The preparation method of the manganese rosinate has the advantages of simple process, easy operation, low cost, high yield, high environmental protection and the like.
Description
Technical Field
The invention relates to a preparation method and application of manganese rosinate, belonging to the technical field of pesticides.
Background
Manganese rosinate is an organic manganese microbial inoculum and a manganese-supplementing trace element fertilizer, and has the chemical name: 1, 2, 3, 4, 4a, 9, 10, 10 a-octahydro-1, 4 a-dimethyl-7- (1-methylethyl) -1-phenanthrene manganese carboxylate of the formula:
manganese rosinate is a bactericide which has good prevention and treatment effects on bacterial diseases, has good prevention and treatment effects on more than ten diseases such as epidemic diseases, downy mildew, anthracnose, rust diseases, epidemic diseases, canker, root diseases and the like, is a novel broad-spectrum bactericide, has strong adsorption and permeability on zinc rosinate, is fast to absorb by crops, is resistant to rain wash, is safe to the crops, does not generate chemical injury, is pollution-free and has no residue. Has low toxicity to human and livestock, and is a novel high-efficiency bactericide worth popularizing. The manganese rosinate is used for producing manganese rosinate bactericide and trace element manganese fertilizer effective components, and a patent and a literature report related to zinc rosinate synthesis are not found at present.
In view of the above, it is desirable to develop a method for preparing manganese rosinate and the application thereof to overcome the above-mentioned drawbacks.
Disclosure of Invention
The invention aims to provide a preparation method of manganese rosinate. The synthesized manganese rosinate has high content, is suitable for preparing various dosage forms of high-content manganese rosinate bactericides, and fills the blank in the international and domestic fields. The raw materials used in the invention are rosin, alkali, manganese salt and an organic solvent, wherein the organic solvent can be recycled, no waste gas or waste residue is generated in the production process, and the rosin is a renewable resource and also ensures the stability of the resource, so the product is an environment-friendly product.
The technical scheme for solving the technical problems is as follows: a preparation method of manganese rosinate comprises the following steps:
step 1: weighing 10-50 parts by weight of manganese salt, adding water, stirring, and preparing into a manganese salt aqueous solution with the mass percent of 10% -50%;
step 2: weighing 20-70 parts by weight of rosin, adding a reaction medium which is 1-50 times of the total weight of manganese salt and the rosin, wherein the reaction medium is water or an organic solvent, adding 1-30 parts by weight of alkali, heating and stirring for reaction to completely dissolve the rosin to obtain the dissolved rosin;
and step 3: adding the manganese salt aqueous solution with the mass percentage of 10-50% obtained in the step 1 into the dissolved rosin obtained in the step 2, heating and stirring the mixture, and reacting the mixture to obtain a reacted mixed solution;
and 4, step 4: when the reaction medium in the step 2 is water, cooling the mixed solution obtained in the step 3 after the reaction to room temperature, filtering with water, and drying to obtain solid manganese rosinate; and (3) when the reaction medium in the step (2) is an organic solvent, recovering the reflux condensate, discharging and cooling to obtain the liquid manganese rosinate.
The invention has the beneficial effects that:
(1) the preparation method of the manganese rosinate has the advantages of simple process, easy operation, low cost, high yield, high environmental protection and the like, is suitable for preparing high-content manganese rosinate bactericides with various formulations, and fills the blank in the international and domestic fields.
(2) The raw materials used in the invention are rosin, alkali, manganese salt and organic solvent, wherein the organic solvent can be recycled, no waste gas or waste residue is generated in the production process, and the rosin is a renewable resource and also ensures the stability of the resource, so the product is an environment-friendly product.
(3) According to the preparation method of manganese rosinate, organic solvent or water is adopted as a reaction medium in the step 2, water or organic solvent is adopted in the step 4 to prepare manganese rosinate, and waste water generated in the reaction process can be used for fertilizer production without discharging waste gas.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, in the step 1, the manganese salt is one or a mixture of manganese sulfate, manganese chloride and manganese acetate.
Further, in step 2, the reaction medium is one of water or an organic solvent.
Furthermore, the organic solvent is one or a mixture of more of toluene, xylene, trimethylbenzene and pure benzene.
Further, in the step 2, the alkali is one or a mixture of several of sodium hydroxide, potassium hydroxide and ammonia water.
Further, in the step 2, the reaction temperature is 50-100 ℃, and the reaction time is 0.1-2 h.
Further, in the step 3, the reaction temperature is 70-140 ℃, and the reaction time is 0.2-3 h.
Further, in step 4, the drying temperature is 100 ℃.
The second purpose of the invention is to provide the application of the manganese rosinate prepared by the method. The manganese rosinate prepared by the invention can be used for preparing various dosage forms of high-content manganese rosinate bactericides, has wide market prospect, and is suitable for large-scale popularization and application.
The technical scheme for solving the technical problems is as follows: the manganese abietate prepared by the method is applied to the preparation of manganese abietate bactericides.
The invention has the beneficial effects that: the manganese rosinate prepared by the invention can be used for preparing various dosage forms of high-content manganese rosinate bactericides, has wide market prospect, and is suitable for large-scale popularization and application.
The solid manganese rosinate prepared by the invention has high manganese rosinate content, and can be used for preparing various dosage forms of high-content manganese rosinate bactericides, such as 20% manganese rosinate suspending agent, 20% manganese rosinate wettable powder, 15% manganese rosinate emulsion and the like.
On the basis of the technical scheme, the invention can be further improved as follows.
Furthermore, the dosage form of the manganese rosinate bactericide is one or more of a suspending agent, wettable powder and missible oil.
Detailed Description
The principles and features of this invention are described below in conjunction with specific embodiments, which are set forth merely to illustrate the invention and are not intended to limit the scope of the invention.
Example 1
The preparation method of manganese rosinate in the embodiment comprises the following steps:
step 1: weighing 8.5kg of manganese sulfate monohydrate, adding 40kg of water, and stirring to prepare a manganese salt aqueous solution;
step 2: weighing 15.2kg of rosin, adding 280kg of water, adding 5kg of potassium hydroxide, starting a reflux device in a reaction kettle with a vacuum reflux device, heating to 80 ℃, and carrying out reflux reaction for 1 hour to completely dissolve to obtain dissolved rosin;
and step 3: adding the manganese salt aqueous solution obtained in the step 1 into the dissolved rosin obtained in the step 2, heating and stirring the mixture to 100 ℃, and reacting for 2 hours to obtain a reacted mixed solution;
and 4, step 4: and (3) cooling the reacted mixed solution obtained in the step (3) to room temperature, filtering with water, and drying at 100 ℃ to obtain 17kg of solid manganese rosinate, wherein the mass percentage of the manganese rosinate is 95%.
The solid manganese rosinate prepared by the method is applied to the preparation of manganese rosinate bactericides. The dosage form of the manganese rosinate bactericide is a suspending agent.
Example 2
The preparation method of manganese rosinate in the embodiment comprises the following steps:
step 1: weighing 15kg of tetrahydrate manganese sulfate, adding 44kg of water, and stirring to prepare a manganese salt aqueous solution;
step 2: weighing 15kg of rosin, adding 478kg of water, adding 4kg of potassium hydroxide, starting a reflux device in a reaction kettle with a vacuum reflux device, heating to 90 ℃, and carrying out reflux reaction for 1 hour to completely dissolve to obtain dissolved rosin;
and step 3: adding the manganese salt aqueous solution obtained in the step 1 into the dissolved rosin obtained in the step 2, heating and stirring the mixture to 90 ℃, and reacting the mixture for 3 hours to obtain a reacted mixed solution;
and 4, step 4: and (3) cooling the reacted mixed solution obtained in the step (3) to room temperature, filtering with water, and drying at 100 ℃ to obtain 18kg of solid manganese rosinate, wherein the mass percentage of the manganese rosinate is 90%.
The solid manganese rosinate prepared by the method is applied to the preparation of manganese rosinate bactericides. The dosage form of the manganese rosinate bactericide is wettable powder.
Example 3
The preparation method of manganese rosinate in the embodiment comprises the following steps:
step 1: weighing 4kg of tetrahydrate manganese sulfate and 4kg of manganese sulfate, adding 8kg of water, and stirring to prepare a manganese salt aqueous solution;
step 2: weighing 15kg of rosin, adding 1440kg of water, adding 9kg of ammonia water, starting a reflux device in a reaction kettle with a vacuum reflux device, heating to 100 ℃, and carrying out reflux reaction for 0.1 hour to completely dissolve to obtain dissolved rosin;
and step 3: adding the manganese salt aqueous solution obtained in the step 1 into the dissolved rosin obtained in the step 2, heating and stirring the mixture to 95 ℃, and reacting the mixture for 3 hours to obtain a reacted mixed solution;
and 4, step 4: and (3) cooling the reacted mixed solution obtained in the step (3) to room temperature, filtering with water, and drying at 100 ℃ to obtain 17.5kg of solid manganese rosinate, wherein the mass percentage of the manganese rosinate is 93%.
The solid manganese rosinate prepared by the method is applied to the preparation of manganese rosinate bactericides. The formulation of the manganese rosinate bactericide is missible oil.
Example 4
The preparation method of manganese rosinate in the embodiment comprises the following steps:
step 1: weighing 4.3kg of manganese acetate, adding 5kg of water, and stirring to prepare a manganese salt aqueous solution;
step 2: weighing 15kg of rosin, adding 25kg of dimethylbenzene and 25kg of trimethylbenzene, adding 2.1kg of sodium hydroxide, starting a reflux device in a reaction kettle with a vacuum reflux device, heating to 50 ℃, and carrying out reflux reaction for 2 hours to completely dissolve to obtain dissolved rosin;
and step 3: adding the manganese salt aqueous solution obtained in the step 1 into the dissolved rosin obtained in the step 2, heating and stirring the mixture to 140 ℃, and reacting the mixture for 0.5 hour to obtain a reacted mixed solution;
and 4, step 4: and (3) recovering the reflux condensate of the mixed solution obtained in the step (3), discharging and cooling to obtain 20kg of liquid manganese rosinate, wherein the mass percentage of the manganese rosinate is 80%.
The solid manganese rosinate prepared by the method is applied to the preparation of manganese rosinate bactericides. The dosage form of the manganese rosinate bactericide is a suspending agent.
Example 5
The preparation method of manganese rosinate in the embodiment comprises the following steps:
step 1: weighing 8kg of manganese sulfate, adding 20kg of water, and stirring to prepare a manganese salt aqueous solution;
step 2: weighing 15kg of rosin, adding 132kg of dimethylbenzene, adding 1kg of sodium hydroxide and 2.5kg of potassium hydroxide, starting a reflux device in a reaction kettle with a vacuum reflux device, heating to 80 ℃, and carrying out reflux reaction for 1 hour to completely dissolve to obtain dissolved rosin;
and step 3: adding the manganese salt aqueous solution obtained in the step 1 into the dissolved rosin obtained in the step 2, heating and stirring the mixture to 120 ℃, and reacting the mixture for 1.5 hours to obtain a reacted mixed solution;
and 4, step 4: and (3) recovering the reflux condensate of the mixed solution obtained in the step (3), discharging and cooling to obtain 21kg of liquid manganese rosinate, wherein the mass percentage of the manganese rosinate is 75%.
The solid manganese rosinate prepared by the method is applied to the preparation of manganese rosinate bactericides. The formulation of the manganese rosinate bactericide is missible oil.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. The preparation method of manganese rosinate is characterized by comprising the following steps:
step 1: weighing 10-50 parts by weight of manganese salt, adding water, stirring, and preparing into a manganese salt aqueous solution with the mass percent of 10% -50%;
step 2: weighing 20-70 parts by weight of rosin, adding a reaction medium which is 1-50 times of the total weight of manganese salt and the rosin, wherein the reaction medium is water or an organic solvent, adding 1-30 parts by weight of alkali, heating and stirring for reaction to completely dissolve the rosin to obtain the dissolved rosin;
and step 3: adding the manganese salt aqueous solution with the mass percentage of 10-50% obtained in the step 1 into the dissolved rosin obtained in the step 2, heating and stirring the mixture, and reacting the mixture to obtain a reacted mixed solution;
and 4, step 4: when the reaction medium in the step 2 is water, cooling the mixed solution obtained in the step 3 after the reaction to room temperature, filtering with water, and drying to obtain solid manganese rosinate; and (3) when the reaction medium in the step (2) is an organic solvent, recovering the reflux condensate, discharging and cooling to obtain the liquid manganese rosinate.
2. The method for preparing manganese rosinate according to claim 1, wherein in step 1, the manganese salt is one or a mixture of manganese sulfate, manganese chloride and manganese acetate.
3. The method of claim 1, wherein in step 2, the reaction medium is one of water or an organic solvent.
4. The method for preparing manganese rosinate according to claim 3, wherein the organic solvent is one or a mixture of toluene, xylene, trimethylbenzene and pure benzene.
5. The method for preparing manganese rosinate according to claim 1, wherein in step 2, the alkali is one or a mixture of sodium hydroxide, potassium hydroxide and ammonia water.
6. The method for preparing manganese rosinate according to claim 1, wherein in step 2, the reaction temperature is 50 ℃ to 100 ℃ and the reaction time is 0.1h to 2 h.
7. The method for preparing manganese rosinate according to claim 1, wherein in step 3, the reaction temperature is 70 ℃ to 140 ℃ and the reaction time is 0.2h to 3 h.
8. The method of claim 1, wherein the drying temperature in step 4 is 100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201911054372.1A CN110776413A (en) | 2019-10-31 | 2019-10-31 | Preparation method and application of manganese abietate |
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| CN201911054372.1A CN110776413A (en) | 2019-10-31 | 2019-10-31 | Preparation method and application of manganese abietate |
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| CN110776413A true CN110776413A (en) | 2020-02-11 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047830A (en) * | 2020-09-22 | 2020-12-08 | 广西茂源科技有限公司 | Preparation method and application of calcium rosinate |
-
2019
- 2019-10-31 CN CN201911054372.1A patent/CN110776413A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047830A (en) * | 2020-09-22 | 2020-12-08 | 广西茂源科技有限公司 | Preparation method and application of calcium rosinate |
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Application publication date: 20200211 |