阅读说明：本技术 一种含丁草胺的环保低毒除草剂组合物 (Butachlor-containing environment-friendly low-toxicity herbicide composition ) 是由 李冬兵 郑秀 于 2021-09-09 设计创作，主要内容包括：本发明涉及一种含丁草胺的环保低毒除草剂组合物,属于除草剂制备技术领域,该除草剂组合物,包括如下重量份原料：组分A 40-60份、填料2-8份、组分B 3-5份和助剂10-15份；组分A通过如下步骤制备：第一步、将丁草胺、吡嘧磺隆、丙炔噁草酮、尿素以及溶剂混合,超声分散,得到悬浮液；第二步、将悬浮液和基料混合制成有机相,然后加入聚乙烯醇和去离子水,剪切3min,然后在转速为600r/min条件下搅拌1h,经过离心、干燥,得到组分A。本发明中添加的组分A中的基料对除草剂进行包覆,提高稳定性,然后使用过程中,基料容易降解,对环境污染小。(The invention relates to an environment-friendly low-toxicity herbicide composition containing butachlor, belonging to the technical field of herbicide preparation, and the herbicide composition comprises the following raw materials in parts by weight: 40-60 parts of component A, 2-8 parts of filler, 3-5 parts of component B and 10-15 parts of auxiliary agent; component A is prepared by the following steps: firstly, mixing butachlor, pyrazosulfuron-ethyl, oxadiargyl, urea and a solvent, and performing ultrasonic dispersion to obtain a suspension; and secondly, mixing the suspension and the base material to prepare an organic phase, adding polyvinyl alcohol and deionized water, shearing for 3min, stirring for 1h at the rotating speed of 600r/min, centrifuging and drying to obtain the component A. The base material in the component A added in the invention coats the herbicide, so that the stability is improved, and then the base material is easy to degrade and has little pollution to the environment in the using process.)

1. An environment-friendly low-toxicity herbicide composition containing butachlor comprises the following raw materials in parts by weight: 40-60 parts of component A, 2-8 parts of filler, 3-5 parts of component B and 10-15 parts of auxiliary agent; the preparation method is characterized in that the component A is prepared by the following steps:

firstly, mixing butachlor, pyrazosulfuron-ethyl, oxadiargyl, urea and a solvent, and performing ultrasonic dispersion for 30-50min under the condition that the frequency is 20-40kHz to obtain a suspension;

and secondly, mixing the suspension and the base material to prepare an organic phase, adding polyvinyl alcohol and deionized water, shearing for 3min under the condition that the rotating speed is 14000r/min, stirring for 1h under the condition that the rotating speed is 600r/min, centrifuging and drying to obtain the component A.

2. The environment-friendly and low-toxicity herbicide composition containing butachlor as claimed in claim 1, wherein the solvent in the first step is dichloromethane; the weight parts of each substance are as follows: 10-20 parts of butachlor, 10-20 parts of pyrazosulfuron-ethyl, 10-20 parts of oxadiargyl, 20-30 parts of solvent and 0.5-1.5 parts of urea;

in the second step, the alcoholysis degree of the polyvinyl alcohol is 88 percent, and the polymerization degree is 1700; the dosage ratio of the suspension, the base material, the polyvinyl alcohol and the deionized water is 50 mL: 2 g: 0.5 g: 50 mL.

3. The butachlor-containing environmentally friendly and low-toxicity herbicide composition as claimed in claim 1, wherein the base material is prepared by the following steps:

step S11, adding octenyl succinic anhydride, polylactic acid and benzoyl peroxide into acetone, heating and refluxing for reaction for 1.6h, and performing post-treatment after the reaction is finished to obtain a solid a;

step S12, mixing ethylenediamine and tetrahydrofuran at 0 ℃, adding the solid a, stirring for 10min, then heating to 10 ℃, stirring for reacting for 2h, and after the reaction is finished, carrying out post-treatment to obtain a solid b;

and step S13, mixing the solid b and the starch, and then melting and blending at 160 ℃ to obtain the base material.

4. The butachlor-containing environmentally friendly and low toxicity herbicide composition of claim 3, wherein the ratio of octenyl succinic anhydride, polylactic acid, benzoyl peroxide and acetone in step S11 is 4 g: 20 g: 0.6 g: 100 mL; the amount ratio of the solid a, ethylenediamine and tetrahydrofuran in step S12 was 2.4 g: 0.7 g: 30 mL; in the step S13, the starch is one of corn starch and cassava starch; the mass ratio of the solid b to the starch is 1: 20.

5. the butachlor-containing environment-friendly low-toxicity herbicide composition as claimed in claim 1, wherein component B is prepared by the following steps:

step A11, mixing sodium alginate and deionized water under the protection of nitrogen, adding N, N-methylene bisacrylamide and ammonium persulfate, stirring for 10min, adding acrylic acid at the temperature of 0 ℃, heating to 80 ℃ after the addition is finished, and reacting for 4h to obtain a modified sodium alginate solution;

step A12, mixing deionized water and a modified sodium alginate solution at 60 ℃, then cooling to 30 ℃, adding laccase to prepare a mixed solution, then spraying the mixed solution into a calcium chloride solution with the mass fraction of 2%, and solidifying to form a component B.

6. The butachlor-containing environmentally friendly and low toxicity herbicide composition of claim 5, wherein the amount of sodium alginate, N-methylene bisacrylamide, ammonium persulfate and acrylic acid used in step A11 is 20 mL: 0.2 g: 0.1 g: 0.8 g; the dosage ratio of the deionized water to the modified sodium alginate solution in the step A12 is 10 mL: 1g of a compound; the dosage ratio of the laccase, the deionized water and the calcium chloride solution is 1000U: 10mL of: 200 mL.

7. The butachlor-containing environment-friendly low-toxicity herbicide composition as claimed in claim 1, wherein the auxiliary agents comprise a stabilizer, a surfactant, a defoaming agent, a preservative and an antifreezing agent in a mass ratio of 3: 2.5: 2: 1: 1.5 mixing to obtain; the stabilizer is epoxidized soybean oil; the surfactant is sodium dodecyl sulfate; the preservative is gallic acid ester, and the antifreezing agent is ethylene glycol; the defoaming agent is an organic silicon defoaming agent; the filler is diatomite.

Technical Field

The invention belongs to the technical field of herbicide preparation, and particularly relates to an environment-friendly low-toxicity herbicide composition containing butachlor.

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. In order to improve the growth quality of crops, the industry is continuously dedicated to research and develop the herbicide with high weeding effect, wide weed control spectrum, low toxicity, low residue and excellent crop selectivity. In the production environment of crops, certain weeds generate certain resistance to corresponding medicines due to long-term use of certain herbicides at the present stage, the effect of the herbicides is reduced, and the herbicides can remain in the environment and have influence on the environment.

Disclosure of Invention

The invention aims to provide an environment-friendly low-toxicity herbicide composition containing butachlor.

The purpose of the invention can be realized by the following technical scheme:

an environment-friendly low-toxicity herbicide composition containing butachlor comprises the following raw materials in parts by weight: 40-60 parts of component A, 2-8 parts of filler, 3-5 parts of component B and 10-15 parts of auxiliary agent;

component A is prepared by the following steps:

firstly, mixing butachlor, pyrazosulfuron-ethyl, oxadiargyl, urea and a solvent, and performing ultrasonic dispersion for 30-50min under the condition that the frequency is 20-40kHz to obtain a suspension;

and secondly, mixing the suspension and the base material to prepare an organic phase, adding polyvinyl alcohol and deionized water, shearing for 3min under the condition that the rotating speed is 14000r/min, stirring for 1h under the condition that the rotating speed is 600r/min, centrifuging and drying to obtain the component A. The butachlor amide selective systemic conduction herbicide can act in plants, inhibit and destroy protease, influence the formation of protein, and inhibit the normal growth and development of weed buds and roots, so that weeds die; the added pyrazosulfuron-ethyl belongs to sulfonylurea herbicides, can be quickly transferred in a weed plant body, and can inhibit the growth of weeds; the added oxadiargyl can prevent and kill barnyard grass of annual and perennial grasses, abnormal sedge of sedge family, felt of cattle, and the weeds of the burclover, the duckweed, the spirogyra of algae, the small arrowroot and the like in broadleaf grass.

Further, the solvent in the first step is dichloromethane; the weight parts of each substance are as follows: 10-20 parts of butachlor, 10-20 parts of pyrazosulfuron-ethyl, 10-20 parts of oxadiargyl, 20-30 parts of solvent and 0.5-1.5 parts of urea;

in the second step, the alcoholysis degree of the polyvinyl alcohol is 88 percent, and the polymerization degree is 1700; the dosage ratio of the suspension, the base material, the polyvinyl alcohol and the deionized water is 50 mL: 2 g: 0.5 g: 50 mL.

Further, the base stock is prepared by the following steps:

step S11, adding octenyl succinic anhydride, polylactic acid and benzoyl peroxide into acetone, heating and refluxing for reaction for 1.6h, and after the reaction is finished, carrying out post-treatment: adding tetrahydrofuran, mixing with deionized water, and performing vacuum filtration to obtain a solid a; the octenyl succinic anhydride and the polylactic acid have free radical grafting reaction under the initiation of benzoyl peroxide to obtain solid a; wherein the dosage ratio of octenyl succinic anhydride, polylactic acid, benzoyl peroxide and acetone is 4 g: 20 g: 0.6 g: 100 mL;

step S12, mixing ethylenediamine and tetrahydrofuran at 0 ℃, adding the solid a, stirring for 10min, then heating to 10 ℃, stirring for reaction for 2h, and after the reaction is finished, carrying out post-treatment: mixing with deionized water, and performing vacuum filtration to obtain a solid b; the ethylenediamine and the solid a are subjected to acylation reaction to obtain a solid b, so that the hydrophilicity of the base material is improved, and the degradation efficiency is improved; wherein the dosage ratio of the solid a, the ethylenediamine and the tetrahydrofuran is 2.4 g: 0.7 g: 30 mL;

and step S13, mixing the solid b and the starch, and then melting and blending at 160 ℃ to obtain the base material. The starch is added to reduce the dosage of the polylactic acid and save the cost. The carboxyl in the solid b can also react with the hydroxyl of the starch, so that the compatibility of the two is improved. Wherein the starch is one of corn starch and cassava starch; the mass ratio of the solid b to the starch is 1: 20.

further, component B was prepared by the following steps:

step A11, mixing sodium alginate and deionized water under the protection of nitrogen, adding N, N-methylene bisacrylamide and ammonium persulfate, stirring for 10min, adding acrylic acid at the temperature of 0 ℃, heating to 80 ℃ after the addition is finished, reacting for 4h, and adjusting the pH value to 7 by using sodium hydroxide after the reaction is finished to obtain a modified sodium alginate solution; wherein the dosage ratio of sodium alginate, N-methylene-bisacrylamide, ammonium persulfate and acrylic acid is 20 mL: 0.2 g: 0.1 g: 0.8 g; the dosage ratio of the sodium alginate to the deionized water is 1 g: 10 mL;

step A12, mixing deionized water and a modified sodium alginate solution at 60 ℃, cooling to 30 ℃, adding laccase to prepare a mixed solution, spraying the mixed solution into a calcium chloride solution with the mass fraction of 2%, and solidifying to form a component B; wherein the dosage ratio of the deionized water to the modified sodium alginate solution is 10 mL: 1g of a compound; the dosage ratio of the laccase, the deionized water and the calcium chloride solution is 1000U: 10mL of: 200 mL.

Further, the auxiliary agent is a stabilizer, a surfactant, a defoaming agent, a preservative and an antifreezing agent according to a mass ratio of 3: 2.5: 2: 1: 1.5 mixing to obtain; the stabilizer is epoxidized soybean oil; the surfactant is sodium dodecyl sulfate; the preservative is gallic acid ester, and the antifreezing agent is ethylene glycol; the defoaming agent is an organic silicon defoaming agent; the filler is diatomite.

The invention has the beneficial effects that:

three herbicides added into the butachlor-containing environment-friendly low-toxicity herbicide composition are low-toxicity substances, the base material in the component A added in the composition coats the herbicide, the stability is improved, and then the base material is easy to degrade and has little pollution to the environment in the using process; the component B added in the invention can slowly release laccase to the environment by coating and protecting the laccase, degrade harmful components in the environment, and reduce environmental pollution and influence on crops.

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.

Example 1

Preparing a base material:

step S11, adding octenyl succinic anhydride, polylactic acid and benzoyl peroxide into acetone, heating and refluxing for reaction for 1.6h, and after the reaction is finished, carrying out post-treatment: adding tetrahydrofuran, mixing with deionized water, and performing vacuum filtration to obtain a solid a; wherein the dosage ratio of octenyl succinic anhydride, polylactic acid, benzoyl peroxide and acetone is 4 g: 20 g: 0.6 g: 100 mL;

step S12, mixing ethylenediamine and tetrahydrofuran at 0 ℃, adding the solid a, stirring for 10min, then heating to 10 ℃, stirring for reaction for 2h, and after the reaction is finished, carrying out post-treatment: mixing the solid with deionized water, and carrying out vacuum filtration to obtain a solid b, wherein the dosage ratio of the solid a to the ethylenediamine to the tetrahydrofuran is 2.4 g: 0.7 g: 30 mL;

and step S13, mixing the solid b and the starch, and then melting and blending at 160 ℃ to obtain the base material. Wherein the starch is one of corn starch and cassava starch; the mass ratio of the solid b to the starch is 1: 20.

example 2

Preparation of component A:

mixing butachlor, pyrazosulfuron-ethyl, oxadiargyl, urea and a solvent, and performing ultrasonic dispersion for 30min under the condition that the frequency is 20kHz to obtain a suspension;

and secondly, mixing the suspension and the base material to prepare an organic phase, adding polyvinyl alcohol and deionized water, shearing for 3min under the condition that the rotating speed is 14000r/min, stirring for 1h under the condition that the rotating speed is 600r/min, centrifuging and drying to obtain the component A.

Wherein, the solvent in the first step is dichloromethane; the weight parts of each substance are as follows: 10 parts of butachlor, 10 parts of pyrazosulfuron-ethyl, 10 parts of oxadiargyl, 20 parts of solvent and 0.5 part of urea; in the second step, the alcoholysis degree of the polyvinyl alcohol is 88 percent, and the polymerization degree is 1700; the dosage ratio of the suspension, the base material, the polyvinyl alcohol and the deionized water is 50 mL: 2 g: 0.5 g: 50 mL; the base stock was prepared as in example 1.

Example 3

Preparation of component A:

mixing butachlor, pyrazosulfuron-ethyl, oxadiargyl, urea and a solvent, and performing ultrasonic dispersion for 50min under the condition of the frequency of 40kHz to obtain a suspension;

and secondly, mixing the suspension and the base material to prepare an organic phase, adding polyvinyl alcohol and deionized water, shearing for 3min under the condition that the rotating speed is 14000r/min, stirring for 1h under the condition that the rotating speed is 600r/min, centrifuging and drying to obtain the component A.

Wherein, the solvent in the first step is dichloromethane; the weight parts of each substance are as follows: 20 parts of butachlor, 20 parts of pyrazosulfuron-ethyl, 20 parts of oxadiargyl, 30 parts of solvent and 1.5 parts of urea; in the second step, the alcoholysis degree of the polyvinyl alcohol is 88 percent, and the polymerization degree is 1700; the dosage ratio of the suspension, the base material, the polyvinyl alcohol and the deionized water is 50 mL: 2 g: 0.5 g: 50 mL; the base stock was prepared as in example 1.

Example 4

Preparation of component B:

step A11, mixing sodium alginate and deionized water under the protection of nitrogen, adding N, N-methylene bisacrylamide and ammonium persulfate, stirring for 10min, adding acrylic acid at the temperature of 0 ℃, heating to 80 ℃ after the addition is finished, reacting for 4h, and adjusting the pH value to 7 by using sodium hydroxide after the reaction is finished to obtain a modified sodium alginate solution; wherein the dosage ratio of sodium alginate, N-methylene-bisacrylamide, ammonium persulfate and acrylic acid is 20 mL: 0.2 g: 0.1 g: 0.8 g;

step A12, mixing deionized water and a modified sodium alginate solution at 60 ℃, cooling to 30 ℃, adding laccase to prepare a mixed solution, spraying the mixed solution into a calcium chloride solution with the mass fraction of 2%, and solidifying to form a component B; wherein the dosage ratio of the deionized water to the modified sodium alginate solution is 10 mL: 1g of a compound; the dosage ratio of the laccase, the deionized water and the calcium chloride solution is 1000U: 10mL of: 200 mL.

Example 5

An environment-friendly low-toxicity herbicide composition containing butachlor comprises the following raw materials in parts by weight: 40 parts of component A, 2 parts of filler, 3 parts of component B and 10 parts of auxiliary agent; preparing into 15 percent aqueous emulsion according to a conventional preparation method.

Wherein the auxiliary agent is a stabilizer, a surfactant, a defoaming agent, a preservative and an antifreezing agent in a mass ratio of 3: 2.5: 2: 1: 1.5 mixing to obtain; the stabilizer is epoxidized soybean oil; the surfactant is sodium dodecyl sulfate; the preservative is gallic acid ester, and the antifreezing agent is ethylene glycol; the defoaming agent is an organic silicon defoaming agent; the filler is diatomite; component a was prepared as in example 3; component B was prepared as in example 4.

Example 6

An environment-friendly low-toxicity herbicide composition containing butachlor comprises the following raw materials in parts by weight: 50 parts of a component A, 5 parts of a filler, 4 parts of a component B and 12 parts of an auxiliary agent; preparing into 15 percent aqueous emulsion according to a conventional preparation method.

Wherein the auxiliary agent is a stabilizer, a surfactant, a defoaming agent, a preservative and an antifreezing agent in a mass ratio of 3: 2.5: 2: 1: 1.5 mixing to obtain; the stabilizer is epoxidized soybean oil; the surfactant is sodium dodecyl sulfate; the preservative is gallic acid ester, and the antifreezing agent is ethylene glycol; the defoaming agent is an organic silicon defoaming agent; the filler is diatomite; component a was prepared as in example 3; component B was prepared as in example 4.

Example 7

An environment-friendly low-toxicity herbicide composition containing butachlor comprises the following raw materials in parts by weight: 60 parts of a component A, 8 parts of a filler, 5 parts of a component B and 15 parts of an auxiliary agent; preparing into 15 percent aqueous emulsion according to a conventional preparation method.

Wherein the auxiliary agent is a stabilizer, a surfactant, a defoaming agent, a preservative and an antifreezing agent in a mass ratio of 3: 2.5: 2: 1: 1.5 mixing to obtain; the stabilizer is epoxidized soybean oil; the surfactant is sodium dodecyl sulfate; the preservative is gallic acid ester, and the antifreezing agent is ethylene glycol; the defoaming agent is an organic silicon defoaming agent; the filler is diatomite; component a was prepared as in example 3; component B was prepared as in example 4.

Comparative example 1

The base material in example 3 was changed to polylactic acid, and the remaining raw materials and preparation process were kept unchanged.

Comparative example 2

Component A from example 6 was replaced with the sample from comparative example 1, and the remaining starting materials and preparation were kept unchanged.

Comparative example 3

Component B from example 6 was removed and the remaining raw materials and preparation were kept unchanged.

The samples prepared in examples 5 to 7 and comparative examples 2 to 3 were tested, and the test results are shown in table 1 below: taking 6 groups of farmlands, dividing each cassava farmland into 3 parallel groups with the same area and size, carrying out weeding test on the experimental farmlands by using the herbicide compositions of the examples 1-3 and the comparative examples 1-3 in the period that the height of the emergence of weeds is not equal to 30cm, and counting the weed control effect within 20 days;

grading the phytotoxicity standard: level 1: the cassava grows normally and has no any damage symptom; and 2, stage: the cassava has slight phytotoxicity, and the phytotoxicity rate is less than 10 percent; and 3, level: the cassava can be recovered later without influencing the yield due to the medium phytotoxicity; 4, level: cassava has serious phytotoxicity and is difficult to recover, so that the yield is reduced: and 5, stage: the cassava has serious phytotoxicity and can not be recovered, thereby causing obvious yield reduction or no yield.

TABLE 1

From the above table 1, it can be seen that the herbicide composition prepared by the invention has good control effect and little harm to crops.

In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.