A kind of gardens herbicide and preparation method thereof
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 play the role of withered 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 derivative majority are all effective.Generation
Boundary's herbicide development is gradually steady, and main development is efficient, low toxicity, the kind of low consumption, the little disposable process of environmental pollution
Agent is increasingly becoming main flow.
Patent No. CN 102942474 B relates to the preparation method of a kind of herbicide dicamba, comprising: (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.
Content 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;
It step 2, above-mentioned suspension adds carbamate, silicone auxiliary agent, synergist, is warming up to 30-40 DEG C, super
Sound simultaneously 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 closed container, is evacuated and hermetically sealed, the suspension then step 2 being obtained
Liquid injects in closed container with the speed of 0.5-1.5mL/min, and injection finishes, and stands 10-20min, freeze-drying, 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 propyl alcohol, butanol, amylalcohol,
Alcohol, the one in octanol, amine is the one in the isomers of triethylamine, isopropylamine, 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 obtaining 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 suppression 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 make the present invention realize technological means, 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 simultaneously
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 closed container, is evacuated and hermetically sealed, the suspension then step 2 being obtained
Liquid injects in closed container with the speed of 0.5mL/min, and injection finishes, and stands 10min, freeze-drying, 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 propyl alcohol, 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 obtaining 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 simultaneously
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 closed container, is evacuated and hermetically sealed, the suspension then step 2 being obtained
Liquid injects in closed container with the speed of 1.5mL/min, and injection finishes, and stands 20min, freeze-drying, 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 obtaining 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 simultaneously
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 closed container, is evacuated and hermetically sealed, the suspension then step 2 being obtained
Liquid injects in closed container with the speed of 1mL/min, and injection finishes, and stands 15min, freeze-drying, 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 obtaining 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.
The obvious 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 not improved design by the present invention and technical scheme directly apply to it
Its occasion, all within protection scope of the present invention.