阅读说明：本技术 一种水剂灭生性除草剂及其制备方法和用途 (Aqueous biocidal herbicide and preparation method and application thereof ) 是由 马梁惠东 马建义 于 2021-01-20 设计创作，主要内容包括：一种水剂灭生性除草剂及其制备方法和用途,属于新农药创制技术领域。含有：55-65份除草活性成分、15-25份氢氧化钾或氢氧化钠、15-95份水、3-7份表面活性剂,所述的除草活性成分为苯酚、2-乙基苯酚、4-甲基苯酚、2-甲氧基苯酚、4-乙基-2-甲氧基苯酚、2,6-二甲氧基苯酚、2-乙基-6-甲基苯酚中的一种或一种以上混合物。上述一种水剂灭生性除草剂及其制备方法和用途,制得的制剂对动物毒性低,环境相容性好,对环境安全,对杂草的各个生活阶段皆有效且不易产生抗性,除草效果好。(An aqueous biocidal herbicide and a preparation method and application thereof, belonging to the technical field of new pesticide creation. Comprises the following components: 55-65 parts of weeding active ingredient, 15-25 parts of potassium hydroxide or sodium hydroxide, 15-95 parts of water and 3-7 parts of surfactant, wherein the weeding active ingredient is one or a mixture of more than one of phenol, 2-ethylphenol, 4-methylphenol, 2-methoxyphenol, 4-ethyl-2-methoxyphenol, 2, 6-dimethoxyphenol and 2-ethyl-6-methylphenol. The water aqua sterilant herbicide and the preparation method and the application thereof have the advantages that the prepared preparation has low toxicity to animals, good environmental compatibility, safety to the environment, effectiveness to each life stage of weeds, difficult generation of resistance and good weeding effect.)

1. An aqueous biocidal herbicide characterized by containing: 55-65 parts of weeding active ingredient, 15-25 parts of potassium hydroxide or sodium hydroxide, 15-95 parts of water and 3-7 parts of surfactant, wherein the weeding active ingredient is one or a mixture of more than one of phenol, 2-ethylphenol, 4-methylphenol, 2-methoxyphenol, 4-ethyl-2-methoxyphenol, 2, 6-dimethoxyphenol and 2-ethyl-6-methylphenol.

2. An aqua biocidal herbicide according to claim 1 comprising: 60-62 parts of weeding active ingredients, 20-23 parts of potassium hydroxide or sodium hydroxide, 30-80 parts of water and 4-5 parts of surfactant.

3. An aqua biocidal herbicide according to claim 1 wherein the surfactant is one or more of calcium dodecylbenzenesulfonate, alkyl glycoside APG0816, alkyl glycoside APG 1214.

4. The process for producing an aqua biocidal herbicide according to claim 1 comprising the steps of: adding water into a stirring kettle, slowly adding sodium hydroxide or potassium hydroxide under stirring, slowly adding the weeding active ingredients after stirring and dissolving, adding the surfactant after stirring and dissolving, and stirring and completely dissolving, wherein the temperature in the whole preparation process is controlled to be lower than 90 ℃, so that the finished product is obtained.

5. The use of an aqueous biocidal herbicide according to claim 1 for the preparation of herbicides for the control of large crabgrass, green bristlegrass, goosegrass herb, alternanthera philoxeroides, bluegrass, bermudagrass, cattle propagation, polygonum hydropiper, cyperus rotundus, dodder.

Technical Field

The invention belongs to the technical field of new pesticide creation, and particularly relates to an aqueous biocidal herbicide as well as a preparation method and application thereof.

Background

The pesticide industry of China is developed on the basis of imitation, and the prior patent method protects the process route and does not protect the compound. In 1993 new patent law was performed and the compound was protected. In order to guarantee the sustainable development of agricultural production and pesticide industry, a new layer is provided for innovation, and the creation of new pesticides is an important content of innovation. The new pesticide has large investment, long period and serious difficulty, but the national competitiveness can be enhanced only by innovating and developing new varieties and products, and the homogenization competition is avoided. In addition, the new requirements of grain safety and agricultural pest control promote the innovation of pesticides. At present, more than 50 varieties are independently created in China, but few industrial production is really realized, and less large-scale application is realized. In contrast, successful examples include that the novel bactericide, cyhalothrin, which is created by the research institute of agricultural chemicals, ltd, Jiangsu province, and the chlorfenapyr (baozuo), which is a novel insecticide and acaricide, which are created by the chemical research and development ltd, Shenyang, and the application area is large, which is also a result of the international and vigorous popularization of the neutralization. Zinc thiazole is a new bactericide developed by Zhejiang new agricultural chemical industry Co., Ltd, and the market of the variety is also the result of the self-efforts of enterprises. Some varieties cannot be well developed in the market due to the aspect of the aspect. The insecticide butryonitrile developed by Dalianrui pesticide GmbH has novel structure and good control effect on diamondback moth and the like. As can be seen, the varieties of the created pesticides are all insecticides and bactericides, but the created herbicides are fresh and have larger difficulty. Research and discovery of novel lead compounds have become important work in the creation of new herbicides. In recent years, many new molecular structures of compounds are designed, so that the structures of compounds available for screening are more and more complex, and correspondingly, the price is more and more expensive, but simple compounds are not used as spare screening compounds, and thus, simple compounds with herbicidal activity are likely to be missed.

Disclosure of Invention

Aiming at the problems in the prior art, the invention aims to design and provide a technical scheme of an aqueous biocidal herbicide, a preparation method and application thereof, and finds that simple compounds of phenols have good herbicidal activity, the simple compounds have low price, simple preparation and easily accepted price by the market, and common simple compounds widely exist in the nature, so that the human and animal safety and environmental compatibility are good; the preparation process is environment-friendly, the using method is simple, the using amount is low, and the method can be applied to a rapid weeding scheme under multiple scenes.

The water agent biocidal herbicide is characterized by comprising the following components: 55-65 parts of weeding active ingredient, 15-25 parts of potassium hydroxide or sodium hydroxide, 15-95 parts of water and 3-7 parts of surfactant, wherein the weeding active ingredient is one or a mixture of more than one of phenol, 2-ethylphenol, 4-methylphenol, 2-methoxyphenol, 4-ethyl-2-methoxyphenol, 2, 6-dimethoxyphenol and 2-ethyl-6-methylphenol.

The water agent biocidal herbicide is characterized by comprising the following components: 60-62 parts of weeding active ingredients, 20-23 parts of potassium hydroxide or sodium hydroxide, 30-80 parts of water and 4-5 parts of surfactant.

The water aqua biocidal herbicide features that the surfactant is one or the mixture of calcium dodecyl benzene sulfonate, alkyl glycoside APG0816 and alkyl glycoside APG 1214.

The preparation method of the water aqua biocidal herbicide is characterized by comprising the following steps: adding water into a stirring kettle, slowly adding sodium hydroxide or potassium hydroxide under stirring, slowly adding the weeding active ingredients after stirring and dissolving, adding the surfactant after stirring and dissolving, and stirring and completely dissolving, wherein the temperature in the whole preparation process is controlled to be lower than 90 ℃, so that the finished product is obtained.

The aqueous biocidal herbicide is applied to the preparation of herbicides for preventing and treating large crabgrass, green bristlegrass, eleusine indica, alternanthera philoxeroides, bluegrass, bermuda grass, cattle propagation, polygonum hydropiper, cyperus rotundus and semen cuscutae.

According to the water agent biocidal herbicide and the preparation method and the application thereof, the simple phenol sodium salt or potassium salt is used as a main active ingredient, and water is used as a solvent, so that the prepared preparation has low toxicity to animals, good environmental compatibility, safety to the environment, effectiveness to each life stage of weeds, difficulty in generating resistance and good weeding effect; the application method is simple, the manufacturing cost is low, and the weeding composition is suitable for weed control in various scenes.

Detailed Description

The present invention will now be described more fully hereinafter with reference to the accompanying specific embodiments, in which some, but not all embodiments of the invention are shown. 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

Adding 15kg of tap water into a 200L stirring kettle, slowly adding 20kg of sodium hydroxide under stirring, slowly adding 60kg of phenol after stirring and dissolving, adding 5kg of surfactant calcium dodecyl benzene sulfonate after stirring and dissolving, stirring and completely dissolving, and controlling the temperature to be lower than 90 ℃ in the whole preparation process to obtain the final product herbicide aqueous solution.

Example 2

10kg of tap water is put into a 200L stirring kettle, 25kg of potassium hydroxide is slowly added under the stirring condition, 60kg of 2-ethylphenol is slowly added after stirring and dissolving, 5kg of surfactant APG0816 is added after stirring and dissolving, stirring is carried out completely, the temperature is controlled to be lower than 90 ℃ in the whole preparation process, and the finished product of the herbicide aqueous solution is obtained.

Example 3

Adding 35kg of tap water into a 200L stirring kettle, slowly adding 20kg of sodium hydroxide under stirring, slowly adding 60kg of 4-methylphenol after stirring and dissolving, adding 5kg of surfactant APG1216 after stirring and dissolving completely, and controlling the temperature to be lower than 90 ℃ in the whole preparation process to obtain the final product herbicide aqueous solution.

Example 4

30kg of tap water is put into a 200L stirring kettle, 25kg of potassium hydroxide is slowly added under the stirring condition, 60kg of 2-methoxyphenol is slowly added after stirring and dissolving, 5kg of surfactants, namely APG0816 and 2.5kg of each calcium dodecyl benzene sulfonate are added after stirring and dissolving, the mixture is completely stirred and dissolved, the temperature is controlled to be lower than 90 ℃ in the whole preparation process, and the final product of the herbicide aqueous solution is obtained.

Example 5

Adding 65kg of tap water into a 200L stirring kettle, slowly adding 20kg of sodium hydroxide under stirring, slowly adding 60kg of 4-ethyl-2-methoxyphenol after stirring and dissolving, adding 5kg of surfactants, namely APG1216 and 2.5kg of calcium dodecyl benzene sulfonate respectively after stirring and dissolving, stirring and completely dissolving, and controlling the temperature to be lower than 90 ℃ in the whole preparation process to obtain the final product herbicide aqueous solution.

Example 6

60kg of tap water is put into a 200L stirring kettle, 25kg of potassium hydroxide is slowly added under the stirring condition, 60kg of 2, 6-dimethoxyphenol is slowly added after stirring and dissolving, 5kg of surfactants, namely 2.5kg of APG0816 and 2.5kg of APG1216 are added after stirring and dissolving, and the whole preparation process is controlled at the temperature lower than 90 ℃, so that the final product herbicide aqueous solution is obtained.

Example 7

Adding 95kg of tap water into a 200L stirring kettle, slowly adding 20kg of sodium hydroxide under stirring, slowly adding 60kg of 2-ethyl-6-methylphenol after stirring and dissolving, adding 5kg of surfactant calcium dodecyl benzene sulfonate after stirring and dissolving, stirring and completely dissolving, and controlling the temperature to be lower than 90 ℃ in the whole preparation process to obtain the final product herbicide aqueous solution.

Example 8

Adding 90kg of tap water into a 200L stirring kettle, slowly adding 25kg of potassium hydroxide under the stirring condition, slowly adding 30kg of each of 2, 6-dimethoxyphenol and 2-ethyl-6-methylphenol after stirring and dissolving, adding 1kg of each of 5kg of surfactants namely calcium dodecylbenzenesulfonate 3kg, APG0816 and APG1216 after stirring and dissolving completely, and controlling the temperature to be lower than 90 ℃ in the whole preparation process to obtain the final product herbicide aqueous solution.

Example 9

Adding 55kg of tap water into a 200L stirring kettle, slowly adding 20kg of sodium hydroxide under stirring, slowly adding 10kg of each of 2-ethylphenol, 4-methylphenol, 2-methoxyphenol, 4-ethyl-2-methoxyphenol, 2, 6-dimethoxyphenol and 2-ethyl-6-methylphenol after stirring and dissolving, adding 2.5kg of each of 5kg of surfactants APG0816 and APG1216 after stirring and dissolving, and completely dissolving, wherein the temperature is controlled to be lower than 90 ℃ in the whole preparation process to obtain the final product herbicide aqueous solution.

Example 10

60kg of tap water is put into a 200L stirring kettle, 25kg of potassium hydroxide is slowly added under the stirring condition, after stirring and dissolving, 5kg of each of phenol and 2-ethylphenol, 10kg of each of 4-methylphenol, 2-methoxyphenol, 4-ethyl-2-methoxyphenol, 2, 6-dimethoxyphenol and 2-ethyl-6-methylphenol are slowly added, after stirring and dissolving, 5kg of surfactants, namely 1kg of calcium dodecylbenzenesulfonate, 2kg of each of APG0816 and APG1216 are added, and after stirring and dissolving completely, the temperature is controlled to be lower than 90 ℃ in the whole preparation process, so that the final product herbicide aqueous solution is obtained.

Example 11

75kg of tap water is put into a 200L stirring kettle, 20kg of sodium hydroxide is slowly added under the stirring condition, 9kg of each of phenol, 2-ethylphenol, 4-methylphenol, 2-methoxyphenol, 4-ethyl-2-methoxyphenol and 2, 6-dimethoxyphenol and 6kg of 2-ethyl-6-methylphenol are slowly added after stirring and dissolving, 5kg of surfactants, namely 2.5kg of each of APG0816 and APG1216 are added after stirring and dissolving, and the temperature is controlled to be lower than 90 ℃ in the whole preparation process, so that the final product of the herbicide aqueous solution is obtained.

Example 12

Adding 80kg of tap water into a 200L stirring kettle, slowly adding 25kg of potassium hydroxide under stirring, slowly adding 20kg of phenol, 2-methoxyphenol and 2, 6-dimethoxyphenol respectively after stirring and dissolving, adding 5kg of surfactant, namely 1kg of calcium dodecyl benzene sulfonate, 2kg of APG0816 and 2kg of APG1216 respectively after stirring and dissolving, stirring and completely dissolving, and controlling the temperature in the whole preparation process to be lower than 90 ℃ to obtain the final product herbicide aqueous solution.

The weed control effect of the above herbicide formulation is demonstrated by experiments below. And (4) performing a field weeding test by referring to the field efficacy test rule of the Ministry of agriculture. The specific design is as follows:

the test is carried out in the university campus of agriculture and forestry in Zhejiang. The experimental land is divided into small areas with the area of 1 x 1m by thin iron wires, each test agent is provided with 4 concentration gradients, the weeds are sprayed after the test agents are diluted by water in examples 1-12, the dosage is 2 percent of the content of active ingredients, 30 kilograms of weeds are sprayed per mu, each concentration is repeatedly applied for three times, and a clear water control group and a glufosinate-ammonium control group are additionally arranged. The cells are randomly arranged. And a label is inserted into each cell, the content of the label comprises a medicament name, a pesticide application concentration and a plant name, and protection lines are arranged around the label to ensure that adjacent plants are not influenced during pesticide application. The experimental land has the advantages that the soil of the experimental land is yellow purple mud, the pH value is 6.8, the organic matter content is 2.9%, the fertility is moderate, the soil is a naturally-growing weed base, and no herbicide is applied before the experiment. The application time and method are as follows: investigating weather conditions in the future for 10 days in advance, selecting continuous clear weather, and applying the medicine in 3-10 months in 2020. Spraying by using a manual sprayer provided by Henan Yunfei science and technology Limited to ensure that the overground parts of the weeds are sprayed wet and thoroughly, no rainfall occurs within 24h after the application, and weed samples are collected at 3d and 7d (the control effect of 7 days after the application) after the application respectively (20 plants in each cell are one sample). Result analysis the fresh weight control effect of the weeds is calculated by using a formula: the fresh weight inhibition ratio (%) (CK-WT)/WT × 100, CK being the fresh weight of the clear water control group, WT being the fresh weight of the plant after application; the data obtained from the experiments are the average of three replicates. The fresh weight inhibition rates of the four tested weeds were tested for significant effect at different concentrations with three tested agents using one-way analysis of variance (ANOVA) and LSD testing. Data were statistically analyzed using SPSS 21.0.

Table 1 examples 1-12 herbicidal effects against 7 weeds, such as large crabgrass, green bristlegrass, goosegrass, alternanthera philoxeroides, bluegrass, cyperus rotundus, and bermudagrass 7 days after spraying a dose of 30kg per mu at 5% active ingredient concentration (%)

As can be seen in table 1, the herbicidal effects on large crabgrass, examples 1-5, 7 and 11, were not significantly different from the control agent glufosinate (i.e., herbicidal activities were equal), and examples 6, 8, 9, 10, 12 had a higher herbicidal activity than glufosinate, wherein the herbicidal activity of example 12 was 15 percentage points higher than glufosinate; herbicidal effect on green bristlegrass examples 1-12 were not significantly different from the control agent glufosinate-ammonium, the herbicidal activity of examples 1-5 was higher than glufosinate-ammonium, wherein the herbicidal activity of example 12 was 17 percentage points higher than glufosinate-ammonium; herbicidal effect on goosegrass the herbicidal activity of examples 1-5, 7, 9, 11 was not significantly different from the control agent glufosinate-ammonium, the herbicidal activity of examples 6, 8, 10, 12 was higher than glufosinate-ammonium, wherein the herbicidal activity of example 12 was 16 percentage points higher than glufosinate-ammonium; herbicidal effect on bluegrass examples 1-5, 7, 9, 11 were not significantly different from the control agent glufosinate-ammonium, examples 6, 8, 10, 12 had a herbicidal activity higher than glufosinate-ammonium, wherein the herbicidal activity of example 12 was 14 percentage points higher than glufosinate-ammonium; the weeding effect on alternanthera philoxeroides is not obviously different from that of a control medicament, namely glufosinate-ammonium in examples 1 and 3, the weeding activity of examples 2 and 4-12 is higher than that of glufosinate-ammonium, and the weeding activity of example 12 is 16 percent higher than that of glufosinate-ammonium; herbicidal effect on cyperus rotundus the herbicidal effect of examples 1-7, 11 was not significantly different from the control agent glufosinate-ammonium, the herbicidal activity of examples 8-10, 12 was higher than glufosinate-ammonium, wherein the herbicidal activity of example 12 was 12% higher than glufosinate-ammonium; herbicidal effect on bermudagrass examples 1-3 were not significantly different from the control agent glufosinate-ammonium, and examples 4-12 had a higher herbicidal activity than glufosinate-ammonium, wherein the herbicidal activity of example 12 was 15% higher than glufosinate-ammonium; in summary, the control effect of examples 1-12 on the above 5 weeds was equal to greater than that of glufosinate-ammonium, while the herbicidal activity of examples 2, 4, 6, 8, 10, 12 was greater than that of examples 1, 3, 5, 7, 9, 11, indicating that the herbicidal activity of the potassium salt was greater than that of the sodium salt. In addition, examples N-1 to 12 show that the herbicidal activity of mixtures of compounds is greater than that of the individual active ingredients at equivalent concentrations of active compound, with increasing numbers of N, increasing herbicidal activity.

The embodiments described in this specification are merely illustrative of implementations of the inventive concepts, which are intended for purposes of illustration only. The scope of the present invention should not be construed as being limited to the particular forms set forth in the examples, but rather as being defined by the claims and the equivalents thereof which can occur to those skilled in the art upon consideration of the present inventive concept.