CN111972410A - Preparation and application of trinexapac-ethyl emulsion in water - Google Patents
Preparation and application of trinexapac-ethyl emulsion in water Download PDFInfo
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- CN111972410A CN111972410A CN202010929837.XA CN202010929837A CN111972410A CN 111972410 A CN111972410 A CN 111972410A CN 202010929837 A CN202010929837 A CN 202010929837A CN 111972410 A CN111972410 A CN 111972410A
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- 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
- A01N25/00—Biocides, 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
- A01N25/02—Biocides, 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 containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- 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
- A01N37/42—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 within the same carbon skeleton a carboxylic group or a thio analogue, or a derivative thereof, and a carbon atom having only two bonds to hetero atoms with at the most one bond to halogen, e.g. keto-carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/333—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by isomerisation; by change of size of the carbon skeleton
- C07C67/343—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/02—Systems containing only non-condensed rings with a three-membered ring
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/14—The ring being saturated
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- Crystallography & Structural Chemistry (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method and application of trinexapac-ethyl emulsion in water, adding a proper amount of 3, 5-dioxygen cyclohexyl ethyl formate and cyclopropanecarboxylic acid into a reaction kettle, then adding a proper amount of nonpolar organic solvent and organic amine into the reaction kettle, adding phosphorus trichloride and a catalyst into the reaction kettle in a dropwise manner, in the process of dropping phosphorus trichloride and a catalyst, materials in a reaction kettle need to be stirred, the mixed solution after the reaction is washed by water, the non-polar organic solvent is removed, the data obtained in the four embodiments are compared, it can be seen that the trinexapac-ethyl prepared in example four has the highest preparation efficiency, the preparation efficiency is 78.5%, therefore, the raw materials comprise 20% of 3, 5-dioxyethyl cyclohexyl formate, 20% of cyclopropanecarboxylic acid, 20% of a non-polar organic solvent, 25% of organic amine and phosphorus trichloride: 10%, catalyst: 5 percent is the best proportion for preparing trinexapac-ethyl, and simultaneously, the process is simpler and the practicability is good.
Description
Technical Field
The invention relates to an emulsion for chemical industry, in particular to a preparation method and application of trinexapac-ethyl emulsion in water.
Background
Trinexapac-ethyl is a cyclohexane derivative with high plant growth regulating activity and may be also used as herbicide. The lodging-resistant agent overcomes the defects of weakened or unstable efficacy, high toxicity, high price and the like of a plurality of other plant growth regulators due to the influences of soil texture, plants, application time and the like.
Trinexapac-ethyl belongs to cyclohexane carboxylic acid plant growth regulator. Because the structural formula of the compound contains two nonadjacent carbon-carbon double bonds, a plurality of cis-trans isomers exist. The trinexapac-ethyl undergoes configuration inversion under the action of external conditions, and the trinexapac-ethyl is unstable and has poor thermal stability under the conditions of ultraviolet rays, strong acid and strong alkali, so that the original medicine of the trinexapac-ethyl is easy to decompose in the storage process. Once the trinexapac-ethyl is decomposed and the content is reduced, it cannot be processed into dosage form for use, so it must be purified and then used.
The conventional trinexapac-ethyl can be prepared by combining diethyl maleate and acetone, wherein the steps of condensation, cyclization, esterification, rearrangement and the like are carried out. Diethyl maleate is also named as diethyl maleate and is colorless transparent liquid, can be mixed with various organic solvents, is partially dissolved in benzene and chloroform, and is dissolved in water at 30 ℃ by 1.4 percent; water was dissolved in diethyl maleate at 1.9%. Diethyl maleate and 88.2 percent of water form an azeotropic mixture with an azeotropic point of 99.65 ℃; diethyl maleate is used as an intermediate of pesticide for preparing organophosphorus pesticide malathion and can also be used for producing spices. However, the method of combining diethyl maleate and acetone for preparation is still relatively complex, and the preparation efficiency is general, so that the method is not suitable for high-efficiency and low-cost industrial production.
Disclosure of Invention
The invention aims to provide preparation and application of trinexapac-ethyl emulsion in water.
In order to achieve the purpose, the invention provides the following technical scheme:
the preparation method of the trinexapac-ethyl emulsion in water comprises the following steps:
s1: sequentially weighing raw materials with required mass fraction ratio for later use;
s2: then adding a proper amount of 3, 5-dioxygen ethyl cyclohexyl formate and cyclopropanecarboxylic acid into a reaction kettle, wherein the temperature in the reaction kettle is controlled at 140-160 ℃;
s3: adding a proper amount of non-polar organic solvent and organic amine into the reaction kettle, wherein the reaction time is 1-1.5 hours;
s4: adding phosphorus trichloride and a catalyst into a reaction kettle in a dropwise manner, wherein in the process of dropwise adding the phosphorus trichloride and the catalyst, materials in the reaction kettle need to be stirred;
s5: and washing the mixed solution after the reaction is finished with water, removing the non-polar organic solvent, and then distilling under reduced pressure to obtain the trinexapac-ethyl.
Preferably: the composite material comprises the following raw materials in parts by mass: 12-25% of 3, 5-dioxo ethyl cyclohexyl formate, 10-28% of cyclopropanecarboxylic acid, 20-30% of non-polar organic solvent, 25-30% of organic amine, and phosphorus trichloride: 8-13%, catalyst: 2 to 5 percent.
The nonpolar organic solvent is a mixture of toluene, acetonitrile, dimethylformamide and N, N-dimethylaniline; the organic amine is a mixture of dimethylamine, diethylamine, dibutylamine, trimethylamine and triethylamine.
Preferably, the mass percentage of the nonpolar organic solvent component is;
45-60% of toluene;
20-35% of acetonitrile;
8-23% of dimethylformamide;
10-22% of N, N-dimethylaniline.
Preferably, the mass percentage of the organic amine component is;
30-45% of dimethylamine;
15-20% of diethylamine;
10-25% of dibutylamine;
13-20% of trimethylamine;
10-20% of triethylamine.
Preferably, the catalyst is 4-dimethylaminopyridine.
Preferably, the reaction kettle is internally provided with a stirring paddle.
The trinexapac-ethyl emulsion in water is applied to inhibiting the growth of plants, can be used as a herbicide, can show a growth inhibition effect on cereal crops, castor-oil plants, rice and sunflowers after being mixed with water and sprayed, and can prevent lodging after being applied after budding.
Compared with the prior art, the invention has the beneficial effects that: the preparation and application of the trinexapac-ethyl emulsion in water provided by the invention are that proper amount of 3, 5-dioxygen cyclohexyl ethyl formate and cyclopropane carboxylic acid are added into a reaction kettle, then adding a proper amount of nonpolar organic solvent and organic amine into the reaction kettle, adding phosphorus trichloride and a catalyst into the reaction kettle in a dropwise manner, in the process of dropping phosphorus trichloride and a catalyst, materials in a reaction kettle need to be stirred, the mixed solution after the reaction is washed by water, the non-polar organic solvent is removed, the data obtained in the four embodiments are compared, it can be seen that the trinexapac-ethyl prepared in example four has the highest preparation efficiency, the preparation efficiency is 78.5%, therefore, the raw materials comprise 20% of 3, 5-dioxyethyl cyclohexyl formate, 20% of cyclopropanecarboxylic acid, 20% of a non-polar organic solvent, 25% of organic amine and phosphorus trichloride: 10%, catalyst: 5 percent is the best proportion for preparing trinexapac-ethyl, and simultaneously, the process is simpler and the practicability is good.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and 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.
The preparation method of the trinexapac-ethyl emulsion in water comprises the following raw materials in parts by mass: 12-25% of 3, 5-dioxo ethyl cyclohexyl formate, 10-28% of cyclopropanecarboxylic acid, 20-30% of non-polar organic solvent, 25-30% of organic amine, and phosphorus trichloride: 8-13%, catalyst: 2 to 5 percent.
The nonpolar organic solvent is a mixture of toluene, acetonitrile, dimethylformamide and N, N-dimethylaniline; the organic amine is a mixture of dimethylamine, diethylamine, dibutylamine, trimethylamine and triethylamine.
Example one
Taking raw materials: 15% of ethyl 3, 5-dioxocyclohexyl formate, 20% of cyclopropanecarboxylic acid, 22% of a nonpolar organic solvent, 28% of organic amine, phosphorus trichloride: 10%, catalyst: 5 percent.
Wherein the nonpolar organic solvent comprises the following components in percentage by mass:
50% of toluene;
25% of acetonitrile;
11% of dimethylformamide;
14% of N, N-dimethylaniline.
Wherein the mass percentage of the organic amine component is;
35% of dimethylamine;
20% of diethylamine;
14% of dibutylamine;
15% of trimethylamine;
and 16% of triethylamine.
Based on the raw material proportion, the specific raw material proportion process is as follows:
the first step is as follows: sequentially weighing raw materials with required mass fraction ratio for later use;
the second step is that: then adding appropriate amounts of ethyl 3, 5-dioxy-cyclohexanecarboxylate and cyclopropanecarboxylic acid into a reaction kettle, wherein the reaction kettle is internally provided with a stirring paddle, and the molar mass ratio of the ethyl 3, 5-dioxy-cyclohexanecarboxylate to the cyclopropanecarboxylic acid is 1: 1.33, wherein the temperature in the reaction kettle is controlled to be 140-160 ℃;
the third step: and adding proper amounts of a non-polar organic solvent and an organic amine into the reaction kettle, wherein the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the non-polar organic solvent is 1: 1.47, wherein the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the organic amine is 1: 1.87, the reaction time is 1-1.5 hours;
the fourth step: and then adding phosphorus trichloride and a catalyst into the reaction kettle in a dropwise manner, wherein the molar mass ratio of the 3, 5-dioxygen ethyl cyclohexyl formate to the phosphorus trichloride is 1: 0.67, the molar mass ratio of ethyl 3, 5-dioxacyclohexanecarboxylate to catalyst at this time was 1: 0.33, the catalyst is 4-dimethylamino pyridine, and materials in the reaction kettle need to be stirred in the process of dropping phosphorus trichloride and the catalyst;
the fifth step: and washing the mixed solution after the reaction is finished with water, removing the non-polar organic solvent, and then carrying out reduced pressure distillation to obtain the trinexapac-ethyl, wherein the target product 4-cyclopropyl (hydroxy) methylene 3, 5-dioxo-cyclohexane carboxylic acid ethyl ester is obtained through the raw material proportion and the preparation steps, namely the trinexapac-ethyl, and finally the preparation efficiency of the trinexapac-ethyl is 71.5% through calculation.
Example two
Taking raw materials: 20% of ethyl 3, 5-dioxocyclohexyl formate, 15% of cyclopropanecarboxylic acid, 25% of a nonpolar organic solvent, 25% of an organic amine, 25% of phosphorus trichloride: 10%, catalyst: 5 percent.
Wherein the nonpolar organic solvent comprises the following components in percentage by mass:
45% of toluene;
30% of acetonitrile;
11% of dimethylformamide;
14% of N, N-dimethylaniline.
Wherein the mass percentage of the organic amine component is;
35% of dimethylamine;
20% of diethylamine;
14% of dibutylamine;
15% of trimethylamine;
and 16% of triethylamine.
Based on the raw material proportion, the specific raw material proportion process is approximately the same as that of the first embodiment, wherein the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the cyclopropanecarboxylic acid in the reaction kettle is 1: 0.75; the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the non-polar organic solvent is 1: 1.25; the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the organic amine is 1: 1.25; the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the phosphorus trichloride is 1: 0.5; the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the catalyst is 1: 0.25.
the target product 4-cyclopropyl (hydroxy) methylene 3, 5-dioxo-cyclohexane carboxylic acid ethyl ester, namely the trinexapac-ethyl, is obtained through the final reduced pressure distillation of the raw material proportion and the preparation steps, and finally the preparation efficiency of the trinexapac-ethyl is obtained through calculation and is 66.5%.
EXAMPLE III
Taking raw materials: 25% of ethyl 3, 5-dioxocyclohexyl formate, 10% of cyclopropanecarboxylic acid, 25% of a nonpolar organic solvent, 25% of an organic amine, 25% of phosphorus trichloride: 10%, catalyst: 5 percent.
Wherein the nonpolar organic solvent comprises the following components in percentage by mass:
50% of toluene;
35% of acetonitrile;
11% of dimethylformamide;
14% of N, N-dimethylaniline.
Wherein the mass percentage of the organic amine component is;
35% of dimethylamine;
20% of diethylamine;
14% of dibutylamine;
15% of trimethylamine;
and 16% of triethylamine.
Based on the raw material proportion, the specific raw material proportion process is approximately the same as that of the first embodiment, wherein the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the cyclopropanecarboxylic acid in the reaction kettle is 1: 0.4; the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the non-polar organic solvent is 1: 1; the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the organic amine is 1: 1; the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the phosphorus trichloride is 1: 0.4; the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the catalyst is 1: 0.2.
the target product 4-cyclopropyl (hydroxy) methylene 3, 5-dioxo-cyclohexane carboxylic acid ethyl ester, namely the trinexapac-ethyl, is obtained through the final reduced pressure distillation of the raw material proportion and the preparation steps, and finally the preparation efficiency of the trinexapac-ethyl is obtained through calculation and is 61.5%.
Example four
Taking raw materials: 20% of ethyl 3, 5-dioxocyclohexyl formate, 20% of cyclopropanecarboxylic acid, 20% of a nonpolar organic solvent, 25% of an organic amine, phosphorus trichloride: 10%, catalyst: 5 percent.
Wherein the nonpolar organic solvent comprises the following components in percentage by mass:
55% of toluene;
30% of acetonitrile;
11% of dimethylformamide;
14% of N, N-dimethylaniline.
Wherein the mass percentage of the organic amine component is;
30% of dimethylamine;
20% of diethylamine;
14% of dibutylamine;
20% of trimethylamine;
and 16% of triethylamine.
Based on the raw material proportion, the specific raw material proportion process is approximately the same as that of the first embodiment, wherein the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the cyclopropanecarboxylic acid in the reaction kettle is 1: 1; the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the non-polar organic solvent is 1: 1; the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the organic amine is 1: 1.25; the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the phosphorus trichloride is 1: 0.5; the molar mass ratio of the 3, 5-dioxy cyclohexyl ethyl formate to the catalyst is 1: 0.25.
the target product 4-cyclopropyl (hydroxy) methylene 3, 5-dioxo-cyclohexane carboxylic acid ethyl ester, namely the trinexapac-ethyl, is obtained through the final reduced pressure distillation of the raw material proportion and the preparation steps, and finally the preparation efficiency of the trinexapac-ethyl is calculated to be 78.5%.
The trinexapac-ethyl emulsion in water is applied to inhibiting the growth of plants, can be used as a herbicide, can show a growth inhibition effect on cereal crops, castor-oil plants, rice and sunflowers after being mixed with water and sprayed, and can prevent lodging after being applied after budding.
The aqueous emulsion of trinexapac-ethyl prepared in four examples, which are respectively listed as example 1, example 2, example 3 and example 4, were applied by adding water to a suitable concentration, while adding control example 1 mainly comprising purified water and control example 2 mainly comprising other herbicides, and example 1, example 2, example 3, example 4, control example 1 and control example 2 were sprayed on crops in a uniform environment, the test crops were sugar cane, soil texture was loam, and main weeds were dominant weeds such as crabgrass, miscanthus, cyperus rotundus, morning glory, amaranthus viridis, mallow, spanishneedles herb, setaria pinicola, bermudagrimony and tupellus cylindrica. Examples 1, 2, 3, 4, 1 and 2 were applied at 375 g/ha, a blank group was set, 7 treatments were performed at 4 repetitions per treatment, 20 treatment plots were performed, the treatments were randomized in a block arrangement, 30 square meters per plot area, and foliage spray was performed at 3-5 leaf stage of weed growth. And (4) taking 4 points per plot with each point being 0.25 square meter 20 days after the application, investigating the weed species and quantity, weighing, and comparing with the weight of the blank group of weeds to calculate the control effect. When the sugarcane is harvested, 30 plants are independently harvested in each cell for yield measurement, and the yield increase rate is calculated. The results of the tests are shown in the following table.
The table shows that the trinexapac-ethyl emulsion in water in the example 4 has a large influence on weeds after being applied, and meanwhile, the yield of crops can be increased, the upward production speed of the crops can be reduced, and lodging of the crops can be avoided.
In summary, the following steps: the preparation and application of the trinexapac-ethyl emulsion in water provided by the invention are that proper amount of 3, 5-dioxygen cyclohexyl ethyl formate and cyclopropane carboxylic acid are added into a reaction kettle, then adding a proper amount of nonpolar organic solvent and organic amine into the reaction kettle, adding phosphorus trichloride and a catalyst into the reaction kettle in a dropwise manner, in the process of dropping phosphorus trichloride and a catalyst, materials in a reaction kettle need to be stirred, the mixed solution after the reaction is washed by water, the non-polar organic solvent is removed, the data obtained in the four embodiments are compared, it can be seen that the trinexapac-ethyl prepared in example four has the highest preparation efficiency, the preparation efficiency is 78.5%, therefore, the raw materials comprise 20% of 3, 5-dioxyethyl cyclohexyl formate, 20% of cyclopropanecarboxylic acid, 20% of a non-polar organic solvent, 25% of organic amine and phosphorus trichloride: 10%, catalyst: 5 percent is the best proportion for preparing trinexapac-ethyl, and simultaneously, the process is simpler and the practicability is good.
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.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (7)
1. The preparation method of the trinexapac-ethyl emulsion in water is characterized by comprising the following steps:
s1: sequentially weighing raw materials with required mass fraction ratio for later use;
s2: then adding a proper amount of 3, 5-dioxygen ethyl cyclohexyl formate and cyclopropanecarboxylic acid into a reaction kettle, wherein the temperature in the reaction kettle is controlled at 140-160 ℃;
s3: adding a proper amount of non-polar organic solvent and organic amine into the reaction kettle, wherein the reaction time is 1-1.5 hours;
s4: adding phosphorus trichloride and a catalyst into a reaction kettle in a dropwise manner, wherein in the process of dropwise adding the phosphorus trichloride and the catalyst, materials in the reaction kettle need to be stirred;
s5: and washing the mixed solution after the reaction is finished with water, removing the non-polar organic solvent, and then distilling under reduced pressure to obtain the trinexapac-ethyl.
2. The preparation method of the trinexapac-ethyl emulsion in water as claimed in claim 1, wherein: the composite material comprises the following raw materials in parts by mass: 12-25% of 3, 5-dioxo ethyl cyclohexyl formate, 10-28% of cyclopropanecarboxylic acid, 20-30% of non-polar organic solvent, 25-30% of organic amine, and phosphorus trichloride: 8-13%, catalyst: 2 to 5 percent;
the nonpolar organic solvent is a mixture of toluene, acetonitrile, dimethylformamide and N, N-dimethylaniline; the organic amine is a mixture of dimethylamine, diethylamine, dibutylamine, trimethylamine and triethylamine.
3. The preparation method of the trinexapac-ethyl emulsion in water as claimed in claim 2, wherein: the mass percentage of the nonpolar organic solvent component is;
45-60% of toluene;
20-35% of acetonitrile;
8-23% of dimethylformamide;
10-22% of N, N-dimethylaniline.
4. The preparation method of the trinexapac-ethyl emulsion in water as claimed in claim 2, wherein: the mass percentage of the organic amine component is as follows;
30-45% of dimethylamine;
15-20% of diethylamine;
10-25% of dibutylamine;
13-20% of trimethylamine;
10-20% of triethylamine.
5. The preparation method of the trinexapac-ethyl emulsion in water as claimed in claim 1, wherein: the catalyst is 4-dimethylamino pyridine.
6. The preparation method of the trinexapac-ethyl emulsion in water as claimed in claim 1, wherein: the reaction kettle is internally provided with a stirring paddle.
7. The use of the trinexapac-ethyl aqueous emulsion as claimed in claim 1, wherein the trinexapac-ethyl aqueous emulsion is used for inhibiting the growth of plants and can be used as herbicide, the trinexapac-ethyl aqueous emulsion can show growth inhibition effect on cereal crops, castor, rice and sunflower after being mixed with water and sprayed, and the application after germination can prevent lodging.
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| CN1850776A (en) * | 2006-05-19 | 2006-10-25 | 浙江大学 | Method for preparing trinexapac-ethyl |
| CN102101830A (en) * | 2010-12-06 | 2011-06-22 | 张家港田由新材料科技有限公司 | Method for preparing trinexapac-ethyl |
| CN102295563A (en) * | 2011-07-13 | 2011-12-28 | 迈克斯(如东)化工有限公司 | Preparation method of trinexapac-ethyl |
| CN102911058A (en) * | 2012-11-19 | 2013-02-06 | 江苏扬农化工股份有限公司 | Synthetic method of plant growth regulator trinexapac-ethyl intermediate 3-carbethoxy-5-oxo-cyclohexane-1-enol cyclopropanecarboxylate |
| CN105085270A (en) * | 2015-08-19 | 2015-11-25 | 迈克斯(如东)化工有限公司 | Preparation method of trinexapac-ethyl and intermediate thereof |
| CN106831416A (en) * | 2016-12-29 | 2017-06-13 | 淮安国瑞化工有限公司 | A kind of preparation method of high content TrinexAN_SNacethyl active compound |
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