CN105941477A - Garden herbicide and preparation method thereof - Google Patents
Garden herbicide and preparation method thereof Download PDFInfo
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- CN105941477A CN105941477A CN201610476081.1A CN201610476081A CN105941477A CN 105941477 A CN105941477 A CN 105941477A CN 201610476081 A CN201610476081 A CN 201610476081A CN 105941477 A CN105941477 A CN 105941477A
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- herbicide
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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
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/26—Phosphorus; Compounds 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
- 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
- A01N37/18—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 the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
- A01N37/26—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 the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof containing the group; Thio analogues thereof
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- Life Sciences & Earth Sciences (AREA)
- Dentistry (AREA)
- General Health & Medical Sciences (AREA)
- Environmental Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a garden herbicide and a preparation method thereof and relates to the field of herbicides. The garden herbicide comprises the following components in parts by mass: 5-10 parts of nano-hydroxyapatite, 10-15 parts of butachlor, 8-12 parts of pyrrolidine dithiocarbamate, 30-40 parts of deionized water, 1-2 parts of organic silicon auxiliary, 2-5 parts of synergist, 3-8 parts of dichlorophenol, 5-6 parts of arene organic solvent, 4-7 parts of liquid potassium hydroxide, 5-10 parts of anhydrous potassium carbonate, 7-10 parts of chloromethane and 8-12 parts of catalyst. By adopting the technical scheme, the preparation steps are reasonable, and the operation is convenient; and the prepared garden herbicide can seriously inhibit the weed growth and even overall kill the weeds, realizes a good inhibitory effect on various weeds and has a wide application range.
Description
Technical field
The present invention relates to herbicide field, be specifically related to a kind of gardens herbicide and preparation method thereof.
Background technology
Herbicide refers to make weeds that withered medicament occurs up hill and dale or selectively.Sodium chlorate therein, Borax, arsenic acid
Salt, trichloroacetic acid have withered effect for any kind of plant, but owing to these are respectively provided with remaining influence, so can not
It is applied in field.Selective herbicide particularly nitrophenol, chlorophenol, carbamic derivant majority are the most effective.Generation
Boundary's herbicide development is gradually steady, and main development is efficient, low toxicity, the kind of low consumption, the disposable process that environmental pollution is little
Agent is increasingly becoming main flow.
Patent No. CN 102942474 B relates to the preparation method of a kind of herbicide dicamba, including: (1) liquid hydroxide
Potassium and 2,5-chlorophenesic acid obtain 2,5-chlorophenesic acid potassium with the molar ratio reaction of 0.95:1 ~ 1:1；(2) step (1) gained
2,5-chlorophenesic acid potassium, in the presence of Anhydrous potassium carbonate and catalyst, reacts production 3,6-dichlorosalicylic acid with CO2；Control
The pressure of CO2 is 4 ~ 6MPa, reaction temperature 100 ~ 160 DEG C, Anhydrous potassium carbonate and 2, and the mol ratio of 5-chlorophenesic acid potassium is 1 ~ 2:
1 ；(3) in the basic conditions, 70 ~ 100 DEG C of temperature
Under degree, by step (2) gained 3,6-dichlorosalicylic acid is fixed through shell and tube by the mol ratio of 1:1 ~ 3.5 with chloromethanes
Bed reactor, reacts under the effect of catalyst, then obtains 3 through saponification, acidifying, 6-bis-chloro-2-methoxysalicylic acid, i.e.
Mediben.Although technique scheme step is relatively simple, but its herbicide produced, it is impossible to once inactivate all of miscellaneous
Grass, the scope of application is narrower.
Summary of the invention
Problem to be solved by this invention is to provide a kind of gardens herbicide and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of gardens herbicide, in parts by mass, described gardens herbicide includes nanometer hydroxyapatite 5-10 part, butachlor
10-15 part, carbamate 8-12 part, deionized water 30-40 part, silicone auxiliary agent 1-2 part, synergist 2-5 part, chlorophenesic acid
3-8 part, aromatic hydrocarbons organic solvent 5-6 part, liquid potassium hydroxide 4-7 part, Anhydrous potassium carbonate 5-10 part, chloromethanes 7-10 part, catalysis
Agent 8-12 part.
Preferably, in parts by mass, described gardens herbicide includes nanometer hydroxyapatite 8 parts, butachlor 12 parts, Ji Jia
Acid esters 10 parts, deionized water 35 parts, silicone auxiliary agent 1 part, synergist 3 parts, chlorophenesic acid 5 parts, aromatic hydrocarbons organic solvent 5 parts,
Liquid potassium hydroxide 6 parts, Anhydrous potassium carbonate 8 parts, chloromethanes 8 parts, catalyst 10 parts.
A kind of method preparing gardens herbicide, described preparation method specifically includes following steps:
Step one, butachlor and deionized water are mixed, ultrasonic disperse, obtain the suspension containing butachlor；
Step 2, above-mentioned suspension adds carbamate, silicone auxiliary agent, synergist, it is warming up to 30-40 DEG C, super
Sound also stirs, and obtains suspension, standby；
Step 3, with chlorophenesic acid as raw material, react with liquid potassium hydroxide in aromatic hydrocarbons organic solvent and obtain chlorophenesic acid potassium；
Step 4, in autoclave, the chlorophenesic acid potassium of step 3 gained in the presence of Anhydrous potassium carbonate and catalyst,
To dichlorosalicylic acid；
Step 5, under the conditions of the alkalescence that pH scope is 7-12, at a temperature of 80-120 DEG C, by step 4 gained dichlorosalicylic acid
With the mol ratio that 1:3 pressed by chloromethanes through calandria type fixed bed reactor, under the effect of catalyst react, then through saponification,
Acidifying obtains methoxysalicylic acid；
Step 6, nanometer hydroxyapatite is placed in hermetic container, is evacuated and hermetically sealed, the suspension then step 2 obtained
Liquid injects in hermetic container with the speed of 0.5-1.5mL/min, injects complete, stands 10-20min, lyophilization, obtains medicine carrying
Nanometer hydroxyapatite；
Step 7, the methoxysalicylic acid that the nanometer hydroxyapatite of medicine carrying, step 5 are obtained and deionized water mixing, stirring
3-4h, is heated to 50-60 DEG C of insulation reaction 1-2h, is heated to 60-70 DEG C of insulation reaction 40-70min, is cooled in 2-3min
Room temperature,.
Preferably, the catalyst described in step 5 is the mixture of alcohols and amine, alcohols be propanol, butanol, amylalcohol,
One in alcohol, capryl alcohol, amine is the one in the isomer of triethylamine, 2-aminopropane., the above amine of fourth ammonia.
Preferably, the mixing speed in described step 7 is 600-1200r/min, and mixing time is 20-25min.
Preferably, the concentration range of the dichlorosalicylic acid obtained in described step 4 is at 10-40%.
Using technical scheme, preparation process is reasonable, it is simple to operation, and the gardens herbicide prepared can be tight
Heavily suppress weed growth, it might even be possible to make weeds somatic death, good inhibition is respectively provided with for various weeds, be suitable for model
Enclose wide.
Detailed description of the invention
For the technological means making the present invention realize, creation characteristic, reach purpose and be easy to understand with effect, below in conjunction with
Detailed description of the invention, is expanded on further the present invention.
Embodiment 1:
A kind of gardens herbicide, in parts by mass, described gardens herbicide include nanometer hydroxyapatite 5 parts, butachlor 10 parts,
Carbamate 8 parts, deionized water 30 parts, silicone auxiliary agent 1 part, synergist 2 parts, chlorophenesic acid 3 parts, aromatic hydrocarbons organic solvent 5
Part, liquid potassium hydroxide 4 parts, Anhydrous potassium carbonate 5 parts, chloromethanes 7 parts, catalyst 8 parts.
A kind of method preparing gardens herbicide, described preparation method specifically includes following steps:
Step one, butachlor and deionized water are mixed, ultrasonic disperse, obtain the suspension containing butachlor；
Step 2, in above-mentioned suspension add carbamate, silicone auxiliary agent, synergist, be warming up to 30 DEG C, ultrasonic also
Stirring, obtains suspension, standby；
Step 3, with chlorophenesic acid as raw material, react with liquid potassium hydroxide in aromatic hydrocarbons organic solvent and obtain chlorophenesic acid potassium；
Step 4, in autoclave, the chlorophenesic acid potassium of step 3 gained in the presence of Anhydrous potassium carbonate and catalyst,
To dichlorosalicylic acid；
Step 5, under the conditions of the alkalescence that pH is 7, at a temperature of 80 DEG C, step 4 gained dichlorosalicylic acid is pressed with chloromethanes
The mol ratio of 1:3, through calandria type fixed bed reactor, is reacted under the effect of catalyst, then obtains first through saponification, acidifying
Epoxide salicylic acid；
Step 6, nanometer hydroxyapatite is placed in hermetic container, is evacuated and hermetically sealed, the suspension then step 2 obtained
Liquid injects in hermetic container with the speed of 0.5mL/min, injects complete, stands 10min, lyophilization, obtains the nanometer of medicine carrying
Hydroxyapatite；
Step 7, the methoxysalicylic acid that the nanometer hydroxyapatite of medicine carrying, step 5 are obtained and deionized water mixing, stirring
3h, is heated to 50 DEG C of insulation reaction 1h, is heated to 60 DEG C of insulation reaction 40min, is cooled to room temperature in 2min,.
Wherein, the catalyst described in step 5 is the mixture of alcohols and amine, and alcohols is propanol, and amine is three second
Amine.
Wherein, the mixing speed in described step 7 is 600r/min, and mixing time is 20min.
Wherein, the concentration range of the dichlorosalicylic acid obtained in described step 4 is 10%.
Embodiment 2:
A kind of gardens herbicide, in parts by mass, described gardens herbicide includes nanometer hydroxyapatite 10 parts, butachlor 15
Part, carbamate 12 parts, deionized water 40 parts, silicone auxiliary agent 2 parts, synergist 5 parts, chlorophenesic acid 8 parts, aromatic hydrocarbons are organic molten
Agent 6 parts, liquid potassium hydroxide 7 parts, Anhydrous potassium carbonate 10 parts, chloromethanes 10 parts, catalyst 12 parts.
A kind of method preparing gardens herbicide, described preparation method specifically includes following steps:
Step one, butachlor and deionized water are mixed, ultrasonic disperse, obtain the suspension containing butachlor；
Step 2, in above-mentioned suspension add carbamate, silicone auxiliary agent, synergist, be warming up to 40 DEG C, ultrasonic also
Stirring, obtains suspension, standby；
Step 3, with chlorophenesic acid as raw material, react with liquid potassium hydroxide in aromatic hydrocarbons organic solvent and obtain chlorophenesic acid potassium；
Step 4, in autoclave, the chlorophenesic acid potassium of step 3 gained in the presence of Anhydrous potassium carbonate and catalyst,
To dichlorosalicylic acid；
Step 5, under the conditions of the alkalescence that pH is 12, at a temperature of 120 DEG C, by step 4 gained dichlorosalicylic acid and chloromethanes
By the mol ratio of 1:3 through calandria type fixed bed reactor, react under the effect of catalyst, then obtain through saponification, acidifying
Methoxysalicylic acid；
Step 6, nanometer hydroxyapatite is placed in hermetic container, is evacuated and hermetically sealed, the suspension then step 2 obtained
Liquid injects in hermetic container with the speed of 1.5mL/min, injects complete, stands 20min, lyophilization, obtains the nanometer of medicine carrying
Hydroxyapatite；
Step 7, the methoxysalicylic acid that the nanometer hydroxyapatite of medicine carrying, step 5 are obtained and deionized water mixing, stirring
4h, is heated to 60 DEG C of insulation reaction 2h, is heated to 70 DEG C of insulation reaction 70min, is cooled to room temperature in 3min,.
Wherein, the catalyst described in step 5 is the mixture of alcohols and amine, and alcohols is butanol, and amine is fourth ammonia.
Wherein, the mixing speed in described step 7 is 1200r/min, and mixing time is 25min.
Wherein, the concentration range of the dichlorosalicylic acid obtained in described step 4 is 40%.
Embodiment 3: a kind of gardens herbicide, in parts by mass, described gardens herbicide includes nanometer hydroxyapatite 8
Part, butachlor 12 parts, carbamate 10 parts, deionized water 35 parts, silicone auxiliary agent 1 part, synergist 3 parts, chlorophenesic acid 5
Part, aromatic hydrocarbons organic solvent 5 parts, liquid potassium hydroxide 6 parts, Anhydrous potassium carbonate 8 parts, chloromethanes 8 parts, catalyst 10 parts.
A kind of method preparing gardens herbicide, described preparation method specifically includes following steps:
Step one, butachlor and deionized water are mixed, ultrasonic disperse, obtain the suspension containing butachlor；
Step 2, in above-mentioned suspension add carbamate, silicone auxiliary agent, synergist, be warming up to 35 DEG C, ultrasonic also
Stirring, obtains suspension, standby；
Step 3, with chlorophenesic acid as raw material, react with liquid potassium hydroxide in aromatic hydrocarbons organic solvent and obtain chlorophenesic acid potassium；
Step 4, in autoclave, the chlorophenesic acid potassium of step 3 gained in the presence of Anhydrous potassium carbonate and catalyst,
To dichlorosalicylic acid；
Step 5, under the conditions of the alkalescence that pH is 10, at a temperature of 100 DEG C, by step 4 gained dichlorosalicylic acid and chloromethanes
By the mol ratio of 1:3 through calandria type fixed bed reactor, react under the effect of catalyst, then obtain through saponification, acidifying
Methoxysalicylic acid；
Step 6, nanometer hydroxyapatite is placed in hermetic container, is evacuated and hermetically sealed, the suspension then step 2 obtained
Liquid injects in hermetic container with the speed of 1mL/min, injects complete, stands 15min, lyophilization, obtains the nanometer hydroxyl of medicine carrying
Base apatite；
Step 7, the methoxysalicylic acid that the nanometer hydroxyapatite of medicine carrying, step 5 are obtained and deionized water mixing, stirring
3h, is heated to 55 DEG C of insulation reaction 1h, is heated to 65 DEG C of insulation reaction 55min, is cooled to room temperature in 2min,.
Wherein, the catalyst described in step 5 is the mixture of alcohols and amine, and alcohols is amylalcohol, and amine is fourth ammonia.
Wherein, the mixing speed in described step 7 is 900r/min, and mixing time is 22min.
Wherein, the concentration range of the dichlorosalicylic acid obtained in described step 4 is 25%.
Based on above-mentioned, using technical scheme, preparation process is reasonable, it is simple to operation, and the gardens prepared are removed
Grass agent can seriously suppress weed growth, it might even be possible to makes weeds somatic death, is respectively provided with good suppression for various weeds
Effect, applied widely.
Obviously the present invention implements and is not subject to the restrictions described above, as long as have employed method design and the skill of the present invention
The improvement of the various unsubstantialities that art scheme is carried out, or the most improved design by the present invention and technical scheme directly apply to it
Its occasion, all within protection scope of the present invention.
Claims (6)
1. a gardens herbicide, it is characterised in that in parts by mass, described gardens herbicide includes nanometer hydroxyapatite 5-
10 parts, butachlor 10-15 part, carbamate 8-12 part, deionized water 30-40 part, silicone auxiliary agent 1-2 part, synergist 2-5
Part, chlorophenesic acid 3-8 part, aromatic hydrocarbons organic solvent 5-6 part, liquid potassium hydroxide 4-7 part, Anhydrous potassium carbonate 5-10 part, chloromethanes
7-10 part, catalyst 8-12 part.
A kind of gardens the most according to claim 1 herbicide, it is characterised in that: in parts by mass, described gardens herbicide
Including nanometer hydroxyapatite 8 parts, butachlor 12 parts, carbamate 10 parts, deionized water 35 parts, silicone auxiliary agent 1 part, increase
Effect agent 3 parts, chlorophenesic acid 5 parts, aromatic hydrocarbons organic solvent 5 parts, liquid potassium hydroxide 6 parts, Anhydrous potassium carbonate 8 parts, chloromethanes 8 parts,
Catalyst 10 parts.
3. the method for the gardens herbicide that a kind is prepared described in claim 1-2 any one, it is characterised in that described preparation side
Method specifically includes following steps:
Step one, butachlor and deionized water are mixed, ultrasonic disperse, obtain the suspension containing butachlor；
Step 2, above-mentioned suspension adds carbamate, silicone auxiliary agent, synergist, it is warming up to 30-40 DEG C, super
Sound also stirs, and obtains suspension, standby；
Step 3, with chlorophenesic acid as raw material, react with liquid potassium hydroxide in aromatic hydrocarbons organic solvent and obtain chlorophenesic acid potassium；
Step 4, in autoclave, the chlorophenesic acid potassium of step 3 gained in the presence of Anhydrous potassium carbonate and catalyst,
To dichlorosalicylic acid；
Step 5, under the conditions of the alkalescence that pH scope is 7-12, at a temperature of 80-120 DEG C, by step 4 gained dichlorosalicylic acid
With the mol ratio that 1:3 pressed by chloromethanes through calandria type fixed bed reactor, under the effect of catalyst react, then through saponification,
Acidifying obtains methoxysalicylic acid；
Step 6, nanometer hydroxyapatite is placed in hermetic container, is evacuated and hermetically sealed, the suspension then step 2 obtained
Liquid injects in hermetic container with the speed of 0.5-1.5mL/min, injects complete, stands 10-20min, lyophilization, obtains medicine carrying
Nanometer hydroxyapatite；
Step 7, the methoxysalicylic acid that the nanometer hydroxyapatite of medicine carrying, step 5 are obtained and deionized water mixing, stirring
3-4h, is heated to 50-60 DEG C of insulation reaction 1-2h, is heated to 60-70 DEG C of insulation reaction 40-70min, is cooled in 2-3min
Room temperature,.
The preparation method of a kind of gardens the most according to claim 3 herbicide, it is characterised in that: urging described in step 5
Agent is the mixture of alcohols and amine, and alcohols is the one in propanol, butanol, amylalcohol, alcohol, capryl alcohol, amine be triethylamine,
2-aminopropane., the above amine of fourth ammonia isomer in one.
The preparation method of a kind of gardens the most according to claim 3 herbicide, it is characterised in that: stirring in described step 7
Mixing speed is 600-1200r/min, and mixing time is 20-25min.
The preparation method of a kind of gardens the most according to claim 3 herbicide, it is characterised in that: described step 4 obtains
The concentration range of dichlorosalicylic acid at 10-40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610476081.1A CN105941477A (en) | 2016-06-27 | 2016-06-27 | Garden herbicide and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610476081.1A CN105941477A (en) | 2016-06-27 | 2016-06-27 | Garden herbicide and preparation method thereof |
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| CN105941477A true CN105941477A (en) | 2016-09-21 |
Family
ID=56904066
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| CN201610476081.1A Withdrawn CN105941477A (en) | 2016-06-27 | 2016-06-27 | Garden herbicide and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106719872A (en) * | 2016-12-14 | 2017-05-31 | 安徽扬子化工有限公司 | A kind of nuisanceless herbicide of compound flowers and plants |
| CN107889831A (en) * | 2017-11-21 | 2018-04-10 | 张耀 | It is a kind of to be used to prevent and treat composition of Semen Cuscutae and its preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2034467C1 (en) * | 1993-02-01 | 1995-05-10 | Чебоксарское производственное объединение "Химпром" | Method of herbicide composition preparing |
| CN106035328A (en) * | 2016-06-25 | 2016-10-26 | 合肥隆扬农业科技有限公司 | Garden herbicide and preparation method thereof |
| CN106070195A (en) * | 2016-06-15 | 2016-11-09 | 安徽菲扬农业科技有限公司 | A kind of gardens herbicide and preparation method thereof |
-
2016
- 2016-06-27 CN CN201610476081.1A patent/CN105941477A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2034467C1 (en) * | 1993-02-01 | 1995-05-10 | Чебоксарское производственное объединение "Химпром" | Method of herbicide composition preparing |
| CN106070195A (en) * | 2016-06-15 | 2016-11-09 | 安徽菲扬农业科技有限公司 | A kind of gardens herbicide and preparation method thereof |
| CN106035328A (en) * | 2016-06-25 | 2016-10-26 | 合肥隆扬农业科技有限公司 | Garden herbicide and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106719872A (en) * | 2016-12-14 | 2017-05-31 | 安徽扬子化工有限公司 | A kind of nuisanceless herbicide of compound flowers and plants |
| CN107889831A (en) * | 2017-11-21 | 2018-04-10 | 张耀 | It is a kind of to be used to prevent and treat composition of Semen Cuscutae and its preparation method and application |
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