阅读说明：本技术 一种水稻田用复配型除草剂及其制备工艺 (Compound herbicide for paddy field and preparation process thereof ) 是由 李玉洁 李冰清 李多才 于 2019-12-06 设计创作，主要内容包括：本发明涉及除草剂制备技术领域,具体涉及一种水稻田用复配型除草剂及其制备工艺；除草剂的原料按重量份数计包括：由五氟磺草胺、硝磺草酮和乙氧磺隆按照重量比2.8-3.2:5.0:2.5-3.5混合而成的混合药剂18-25份、苄嘧磺隆5-10份、扑草净3-7份、丁草胺10-15份、氮酮8-12份、噻酮5-8份、崩解剂1.3-1.8份、粘合剂2.2-2.8份、消泡剂0.9-1.4份和助剂4-7份；相比较于市售水稻田除草剂,本发明制备的除草剂对水稻田内的一年生禾本科、阔叶和莎科杂草均具有更好的杀除效果,效果更加显著,且除草范围也更广泛,具有很好的市场前景；另外,发明制备的除草剂可直接播撒至稻田,相比较于传统的喷雾施药方法,在施用本发明制备的除草剂时更加地省时、省工和省力。(The invention relates to the technical field of herbicide preparation, in particular to a compound herbicide for a paddy field and a preparation process thereof; the herbicide comprises the following raw materials in parts by weight: 18-25 parts of mixed medicament prepared by mixing penoxsulam, mesotrione and ethoxysulfuron according to the weight ratio of 2.8-3.2:5.0:2.5-3.5, 5-10 parts of bensulfuron methyl, 3-7 parts of prometryn, 10-15 parts of butachlor, 8-12 parts of azone, 5-8 parts of thiazone, 1.3-1.8 parts of disintegrating agent, 2.2-2.8 parts of adhesive, 0.9-1.4 parts of defoaming agent and 4-7 parts of auxiliary agent; compared with the herbicide for the rice field sold in the market, the herbicide prepared by the invention has better killing and removing effects on annual gramineous, broadleaf and sedge weeds in the rice field, has more obvious effect, wider weeding range and good market prospect; in addition, the herbicide prepared by the invention can be directly sown in the rice field, and compared with the traditional spray application method, the herbicide prepared by the invention is more time-saving, labor-saving and labor-saving when being applied.)

1. The compound herbicide for the paddy field is characterized by comprising the following raw materials in parts by weight: 18-25 parts of mixed medicament, 5-10 parts of bensulfuron methyl, 3-7 parts of prometryn, 10-15 parts of butachlor, 8-12 parts of azone, 5-8 parts of thiazone, 1.3-1.8 parts of disintegrating agent, 2.2-2.8 parts of adhesive, 0.9-1.4 parts of defoaming agent and 4-7 parts of auxiliary agent;

wherein the mixed medicament is prepared by mixing penoxsulam, mesotrione and ethoxysulfuron according to the weight ratio of 2.8-3.2:5.0: 2.5-3.5.

2. The compound herbicide for paddy field according to claim 1, wherein: the disintegrating agent is carboxymethyl starch sodium or dry starch.

3. The compound herbicide for paddy field according to claim 1, wherein: the adhesive is any one of starch, dextrin and polyvinyl alcohol.

4. The compound herbicide for paddy field according to claim 1, wherein: the defoaming agent is polydimethylsiloxane or emulsified silicone oil.

5. The compound herbicide as claimed in claim 1, wherein the adjuvant is prepared by a method comprising the steps of:

adding 3, 4-epoxy-1-butene and vinyl tri (β -methoxyethoxy) silane into a reaction vessel according to the mass ratio of 1.0-1.5:1, adding a proper amount of organic solvent and catalyst into the reaction vessel to obtain a mixed component, then connecting the reaction vessel and a condensation pipe, and magnetically stirring for 40-50min under the protection of nitrogen;

after the reaction in the step a is finished, carrying out reduced pressure distillation on the reaction product at the temperature of 80-85 ℃ for 35-50min, then placing the obtained solid product in a constant-temperature drying box, and carrying out drying treatment at the temperature of 40-50 ℃;

b, adding the dried solid product obtained in the step b and 2, 2' -dihydroxydiethylamine into a reaction kettle according to the molar ratio of 1:1.06-1.2, adding a proper amount of solvent into the reaction kettle, uniformly mixing and stirring, setting the temperature of the reaction kettle to be 75-85 ℃, and reacting for 3-4 hours at the temperature;

and after the reaction is finished, carrying out reduced pressure distillation on the reaction product obtained in the reaction kettle for 30-40min at the temperature of 80 ℃, and finally obtaining a solid, namely an auxiliary agent finished product.

6. The compound herbicide as claimed in claim 5, wherein the organic solvent used in step a is toluene, and the amount of toluene added is 40-50% of the total weight of 3, 4-epoxy-1-butene and vinyltris (β -methoxyethoxy) silane.

7. The compound herbicide as claimed in claim 5, wherein the concentration of the catalyst in step b is 25-30g/L chloroplatinic acid/isopropanol, and the amount of the catalyst is 4-6% of the total mass of 3, 4-epoxy-1-butene and vinyltris (β -methoxyethoxy) silane.

8. The compound herbicide for paddy field according to claim 5, wherein: and c, selecting propanol as a solvent in the step c, wherein the addition amount of the propanol is 35-50% of the total mass of the solid product and the 2, 2' -dihydroxydiethylamine.

9. The process for preparing a herbicide formulation for paddy field according to claim 1, which comprises the steps of:

s1, sequentially adding the solid raw materials except the adhesive into a gravity-free reaction kettle according to the requirements of the process formula, and stirring the solid raw materials in the reaction kettle at the speed of 360-500r/min for 40-60min to obtain a solid mixed component;

s2, putting the solid mixed component obtained in the S1 into a kneader, adding a binder and the rest raw materials into the kneader, kneading, granulating by using a rotary granulator after the kneading is finished, and finishing granules according to the requirements of different grades of commodities;

s3, putting the finally obtained wet granules in the step S2 on a fluidized bed for drying treatment, and screening and discharging after the water content in the granules is qualified;

s4, sampling and detecting each batch of products, discarding defective products, and packaging qualified products; the packaging comprises the steps of bagging, boxing, packaging and the like, metering and checking are carried out after the packaging is finished, and finally the qualified products are put in storage.

Technical Field

The invention relates to the technical field of herbicide preparation, in particular to a compound herbicide for a paddy field and a preparation process thereof.

Background

Herbicides are agents which cause complete or selective death of weeds, also known as herbicides, and are used to kill or inhibit the growth of plants. The sodium chlorate, borax, arsenate and trichloroacetic acid in the herbicide composition have withering effect on any kind of plants, and the effect is influenced by three factors of the herbicide, the plants and the environmental conditions. They are divided by action into biocidal and selective herbicides, the selective herbicides being effective in most cases, in particular derivatives of nitrophenol, chlorophenol, carbamic acid. The development of the herbicide in the world is gradually steady, the varieties with high efficiency, low toxicity, broad spectrum and low dosage are mainly developed, and the disposable treatment agent with little environmental pollution gradually becomes the mainstream.

Rice is a kind of herbaceous rice, belongs to cereals, and is the most important and longest kind of grains in the genus Oryza. However, other weeds can grow in the rice field in the rice planting process, and the weeds and the rice compete for nutrients, so people usually kill the weeds by means of herbicides. However, the weeding effect of the existing herbicide for rice is not particularly ideal, and the weeding range is relatively limited.

Disclosure of Invention

Aiming at the existing problems, the invention provides a compound herbicide for a paddy field and a preparation method thereof, which are used for solving the technical problems in the background technology.

In order to achieve the purpose, the invention adopts the following technical scheme:

the compound herbicide for the paddy field comprises the following raw materials in parts by weight: 18-25 parts of mixed medicament, 5-10 parts of bensulfuron methyl, 3-7 parts of prometryn, 10-15 parts of butachlor, 8-12 parts of azone, 5-8 parts of thiazone, 1.3-1.8 parts of disintegrating agent, 2.2-2.8 parts of adhesive, 0.9-1.4 parts of defoaming agent and 4-7 parts of auxiliary agent;

wherein the mixed medicament is prepared by mixing penoxsulam, mesotrione and ethoxysulfuron according to the weight ratio of 2.8-3.2:5.0: 2.5-3.5.

Furthermore, sodium carboxymethyl starch or dry starch is selected as the disintegrating agent.

The use of the disintegrant accelerates the rapid disintegration of the active ingredients in the herbicide into fine particles when the herbicide prepared by the invention is prepared into pesticides with different concentrations, thereby accelerating the dissolution of the active ingredients in the herbicide in the pesticide liquid and enhancing the weeding effect of the pesticide liquid.

Furthermore, the adhesive is any one of starch, dextrin and polyvinyl alcohol.

The use of the adhesive is convenient for bonding different raw materials together, thereby facilitating the smooth proceeding of the subsequent granulation process and ensuring the quality of the prepared herbicide.

Furthermore, the defoaming agent is selected from polydimethylsiloxane or silicone emulsion.

The defoaming agent can reduce the phenomenon of 'cavitation' in the prepared herbicide granules, thereby ensuring the quality of herbicide granulation.

Further, the preparation method of the auxiliary agent comprises the following steps:

a. adding 3, 4-epoxy-1-butene and vinyl tri (β -methoxyethoxy) silane into a reaction vessel according to the mass ratio of 1.0-1.5:1, adding a proper amount of organic solvent and catalyst into the reaction vessel to obtain a mixed component, then connecting the reaction vessel and a condensation pipe, and magnetically stirring for 40-50min under the protection of nitrogen;

b. after the reaction in the step a is finished, carrying out reduced pressure distillation on the reaction product at the temperature of 80-85 ℃ for 35-50min, then placing the obtained solid product in a constant-temperature drying box, and carrying out drying treatment at the temperature of 40-50 ℃;

c. b, adding the dried solid product obtained in the step b and 2, 2' -dihydroxydiethylamine into a reaction kettle according to the molar ratio of 1:1.06-1.2, adding a proper amount of solvent into the reaction kettle, uniformly mixing and stirring, setting the temperature of the reaction kettle to be 75-85 ℃, and reacting for 3-4 hours at the temperature;

d. and after the reaction is finished, carrying out reduced pressure distillation on the reaction product obtained in the reaction kettle for 30-40min at the temperature of 80 ℃, and finally obtaining a solid, namely an auxiliary agent finished product.

Furthermore, the organic solvent in the step a is toluene, and the adding amount of the toluene is 40-50% of the total mass of the 3, 4-epoxy-1-butene and the vinyl tri (β -methoxyethoxy) silane.

Under the action of chloroplatinic acid/isopropanol solution, relevant functional groups between 3, 4-epoxy-1-butene and vinyl tri (β -methoxyethoxy) silane are subjected to chemical grafting reaction, so that the 3, 4-epoxy-1-butene and the vinyl tri (β -methoxyethoxy) silane are connected with each other by a chemical bond with larger bond energy, the surface tension of herbicide fog drops can be remarkably increased, the herbicide fog drops are ensured to be more firmly adsorbed on weed blades, the rainwater erosion resistance of the herbicide is enhanced, and the weeding effect of the herbicide is increased and prolonged.

Furthermore, the catalyst in the step b is chloroplatinic acid/isopropanol solution with the concentration of 25-30g/L, and the adding amount of the catalyst is 4-6% of the total mass of the 3, 4-epoxy-1-butene and the vinyl tri (β -methoxyethoxy) silane.

The application of the chloroplatinic acid/isopropanol solution can reduce the activation energy required by the chemical reaction of the 3, 4-epoxy-1-butene and the vinyl tris (β -methoxyethoxy) silane, thereby accelerating the chemical reaction rate between the two and obviously shortening the time required for preparing the auxiliary agent.

Furthermore, the solvent in the step c is propanol, and the addition amount of the propanol is 35-50% of the total mass of the solid product and the 2, 2' -dihydroxydiethylamine.

The propanol is convenient to increase the contact area between different types of reactant molecules, so that the collision probability of different reactant molecules is increased, and the reaction rate is improved.

A preparation process of a compound herbicide for paddy fields comprises the following steps:

s1, sequentially adding the solid raw materials except the adhesive into a gravity-free reaction kettle according to the requirements of the process formula, and stirring the solid raw materials in the reaction kettle at the speed of 360-500r/min for 40-60min to obtain a solid mixed component;

s2, putting the solid mixed component obtained in the S1 into a kneader, adding a binder and the rest raw materials into the kneader, kneading, granulating by using a rotary granulator after the kneading is finished, and finishing granules according to the requirements of different grades of commodities;

s3, putting the finally obtained wet granules in the step S2 on a fluidized bed for drying treatment, and screening and discharging after the water content in the granules is qualified;

s4, sampling and detecting each batch of products, discarding defective products, and packaging qualified products; the packaging comprises the steps of bagging, boxing, packaging and the like, metering and checking are carried out after the packaging is finished, and finally the qualified products are put in storage.

By adopting the technical scheme, the invention has the beneficial effects that:

1. under the action of chloroplatinic acid/isopropanol solution, the related functional groups between 3, 4-epoxy-1-butene and vinyl tri (β -methoxyethoxy) silane are subjected to chemical grafting reaction, so that the 3, 4-epoxy-1-butene and the vinyl tri (β -methoxyethoxy) silane are connected by chemical bonds with larger bond energy, the surface tension of herbicide fog drops can be remarkably increased, the herbicide fog drops are more firmly adsorbed on weed blades, the rain wash resistance of the herbicide is enhanced, and the weeding effect of the herbicide is increased and prolonged.

2. The invention takes penoxsulam, mesotrione, ethoxysulfuron, bensulfuron, prometryn, butachlor and the like as main raw materials for preparing the herbicide; wherein, the raw materials are mutually cooperated, so that the weeding effect of the prepared herbicide is obviously improved. Moreover, the weeding range is wider, and the weeding composition has good killing effect on annual gramineous, broadleaf and sedge weeds in the paddy field. And the herbicide prepared by the invention can be directly sown in the rice field, and compared with the traditional spray application method, the herbicide prepared by the invention is more time-saving, labor-saving and labor-saving when being applied.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, 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. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.