WO2021254179A1 - Fenobucarb pesticide stabilizer and fenobucarb pesticide - Google Patents

Fenobucarb pesticide stabilizer and fenobucarb pesticide Download PDF

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WO2021254179A1
WO2021254179A1 PCT/CN2021/098410 CN2021098410W WO2021254179A1 WO 2021254179 A1 WO2021254179 A1 WO 2021254179A1 CN 2021098410 W CN2021098410 W CN 2021098410W WO 2021254179 A1 WO2021254179 A1 WO 2021254179A1
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stabilizer
pesticide
phosphoric acid
fenobucarb
fecbucarb
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PCT/CN2021/098410
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French (fr)
Chinese (zh)
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杨云瑶
胡晓珊
张敦河
刘亚龙
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湖南国发精细化工科技有限公司
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N47/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/10Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
    • A01N47/22O-Aryl or S-Aryl esters thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/22Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients stabilising the active ingredients

Definitions

  • the invention belongs to the field of chemistry, and in particular relates to a fecbucarb pesticide stabilizer and fecbucarb pesticide.
  • Fenbucarb is a carbamate pesticide insecticide, and its formulation is widely used in the control of rice borers and flying wind. After 6 months to 1 year, the content of qualified fendicarb often decreases in content, changes color, and expands the barrel.
  • the present invention discloses a fecbucarb pesticide stabilizer and fecbucarb pesticide.
  • the present invention increases the stability of fecbucarb. 100% stable, no content decrease, discoloration, or barrel expansion.
  • a fenbucarb pesticide stabilizer includes methanol solution and 85% phosphoric acid solution; the mass percentage concentration of phosphoric acid in the methanol and phosphoric acid solution system is ⁇ 50% and ⁇ 55%.
  • the stabilizer is added with fecbucarb pesticide under stirring conditions of 40°C-45°C, and the stirring time is 0.5-1 hour; the mass ratio of the stabilizer to fecbucarb pesticide is 0.4-0.42:1000.
  • a fecbucarb pesticide including fecbucarb technical and a stabilizer; the stabilizer includes methanol and a phosphoric acid solution with a concentration of 85%; the mass ratio of fecbucarb technical to the stabilizer is 0.4-0.42:1000; methanol and phosphoric acid The mass percentage concentration of phosphoric acid in the solution system is 50%-55%.
  • the stability of fecbucarb is increased, and the quality of fecbucarb technical with stabilizer is 100% stable after heat storage and cold storage, without content decrease, discoloration, and barrel expansion.
  • Figure 1-1 is a picture before adding 0.2g phosphoric acid concentration of 49.1% stabilizer heat storage
  • Figure 1-2 is the figure after adding 0.2g phosphoric acid concentration of 49.1% stabilizer heat storage;
  • Figure 2--1 is the figure before adding 0.21g phosphoric acid concentration of 49.1% stabilizer heat storage;
  • Figure 2-2 is the figure after adding 0.21g phosphoric acid concentration 49.1% stabilizer heat storage;
  • Figure 3--1 is the picture before thermal storage without adding stabilizer
  • Figure 3-2 is the figure after heat storage without adding stabilizer
  • Figure 4--1 is a picture before adding 0.2g phosphoric acid concentration of 50% stabilizer to heat storage
  • Figure 4-2 is the figure after adding 0.2g phosphoric acid concentration of 50% stabilizer heat storage
  • Figure 5--1 is a picture before adding 0.21g phosphoric acid concentration of 50% stabilizer to heat storage
  • Figure 5--2 is the figure after adding 0.21g phosphoric acid concentration of 50% stabilizer heat storage

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  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Zoology (AREA)
  • Dentistry (AREA)
  • Environmental Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Agronomy & Crop Science (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Medicinal Preparation (AREA)

Abstract

A fenobucarb pesticide stabilizer, comprising methanol (≥99%) and a phosphoric acid solution at a concentration of 85%; the mass percentage of phosphoric acid in a methanol and phosphoric acid solution system is 50%-55%, the stabilizer is added to the fenobucarb pesticide at 40°C-45°C stirring conditions, and the stirring time is 0.5-1 hour; and the weight ratio of the stabilizer to the fenobucarb pesticide is 0.4-0.42:1000. The stabilizer improves the stability of fenobucarb, a fenobucarb drug substance that has the stabilizer added thereto is 100% stable without content loss, discoloration or barrel swelling after hot storage and cold storage.

Description

一种仲丁威农药稳定剂及仲丁威农药A kind of fecbucarb pesticide stabilizer and fecbucarb pesticide 技术领域Technical field
本发明属于化学领域,特别涉及了一种仲丁威农药稳定剂及仲丁威农药。The invention belongs to the field of chemistry, and in particular relates to a fecbucarb pesticide stabilizer and fecbucarb pesticide.
背景技术Background technique
仲丁威是一种氨基甲酸酯类农药杀虫剂,其制剂广泛用入水稻螟虫、飞風防治。合格仲丁威储存6过月至1年以后时常出现含量下降、变色、胀桶等现象。Fenbucarb is a carbamate pesticide insecticide, and its formulation is widely used in the control of rice borers and flying wind. After 6 months to 1 year, the content of qualified fendicarb often decreases in content, changes color, and expands the barrel.
发明内容Summary of the invention
针对上述问题本发明公开了一种仲丁威农药稳定剂及仲丁威农药,本发明增加了仲丁威的稳定性,加入稳定剂的仲丁威原药经过热储、冷储后其质量100%稳定,无含量下降、变色、胀桶现象。In view of the above problems, the present invention discloses a fecbucarb pesticide stabilizer and fecbucarb pesticide. The present invention increases the stability of fecbucarb. 100% stable, no content decrease, discoloration, or barrel expansion.
为实现上述目的,本发明的技术方案如下:In order to achieve the above objective, the technical scheme of the present invention is as follows:
一种仲丁威农药稳定剂,包括甲醇溶液和浓度为85%磷酸溶液;甲醇与磷酸溶液体系中磷酸的质量百分比浓度为≥50%且<55%。A fenbucarb pesticide stabilizer includes methanol solution and 85% phosphoric acid solution; the mass percentage concentration of phosphoric acid in the methanol and phosphoric acid solution system is ≥50% and <55%.
进一步的改进,所述稳定剂在40℃--45℃搅拌条件加加入仲丁威农药,搅拌时间为0.5-1小时;稳定剂与仲丁威农药的质量比为0.4-0.42:1000。As a further improvement, the stabilizer is added with fecbucarb pesticide under stirring conditions of 40°C-45°C, and the stirring time is 0.5-1 hour; the mass ratio of the stabilizer to fecbucarb pesticide is 0.4-0.42:1000.
一种仲丁威农药,包括仲丁威原药和稳定剂;稳定剂包括甲醇和浓度为85%磷酸溶液;仲丁威原药与稳定剂的质量比为0.4-0.42:1000;甲醇与磷酸溶液体系中磷酸的质量百分比浓度为50%-55%。A fecbucarb pesticide, including fecbucarb technical and a stabilizer; the stabilizer includes methanol and a phosphoric acid solution with a concentration of 85%; the mass ratio of fecbucarb technical to the stabilizer is 0.4-0.42:1000; methanol and phosphoric acid The mass percentage concentration of phosphoric acid in the solution system is 50%-55%.
本发明的优点:The advantages of the present invention:
增加了仲丁威的稳定性,加入稳定剂的仲丁威原药经过热储、冷储后其质量100%稳定,无含量下降、变色、胀桶现象。The stability of fecbucarb is increased, and the quality of fecbucarb technical with stabilizer is 100% stable after heat storage and cold storage, without content decrease, discoloration, and barrel expansion.
附图说明Description of the drawings
图1--1为加入0.2g磷酸浓度为49.1%稳定剂热储前的图;Figure 1-1 is a picture before adding 0.2g phosphoric acid concentration of 49.1% stabilizer heat storage;
图1--2为加入0.2g磷酸浓度为49.1%稳定剂热储后的图;Figure 1-2 is the figure after adding 0.2g phosphoric acid concentration of 49.1% stabilizer heat storage;
图2--1为加入0.21g磷酸浓度为49.1%稳定剂热储前的图;Figure 2--1 is the figure before adding 0.21g phosphoric acid concentration of 49.1% stabilizer heat storage;
图2--2为加入0.21g磷酸浓度为49.1%稳定剂热储后的图;Figure 2-2 is the figure after adding 0.21g phosphoric acid concentration 49.1% stabilizer heat storage;
图3--1为未加入稳定剂热储前的图;Figure 3--1 is the picture before thermal storage without adding stabilizer;
图3--2为未加入稳定剂热储后的图;Figure 3-2 is the figure after heat storage without adding stabilizer;
图4--1为加入0.2g磷酸浓度为50%稳定剂热储前的图;Figure 4--1 is a picture before adding 0.2g phosphoric acid concentration of 50% stabilizer to heat storage;
图4--2为加入0.2g磷酸浓度为50%稳定剂热储后的图;Figure 4-2 is the figure after adding 0.2g phosphoric acid concentration of 50% stabilizer heat storage;
图5--1为加入0.21g磷酸浓度为50%稳定剂热储前的图;Figure 5--1 is a picture before adding 0.21g phosphoric acid concentration of 50% stabilizer to heat storage;
图5--2为加入0.21g磷酸浓度为50%稳定剂热储后的图;Figure 5--2 is the figure after adding 0.21g phosphoric acid concentration of 50% stabilizer heat storage;
具体实施方式detailed description
下面进一步说明其技术方案。The technical solution is further explained below.
实施例1Example 1
一种改善仲丁威农药储存稳定性的药剂:磷酸--甲醇溶液。在仲丁威合产品中间储槽中,控制温度40℃--45℃边搅拌边加入一定浓度、数量的磷酸--甲醇溶液,控温均质0.5-1小时,得到的仲丁威原药经过热储、冷储后其质量100%稳定,无含量下降、变色、胀桶现象。A medicament for improving the storage stability of fecbucarb pesticide: phosphoric acid-methanol solution. In the intermediate storage tank of fecbucarb product, add a certain concentration and quantity of phosphoric acid-methanol solution while stirring at the temperature of 40℃-45℃, and homogenize for 0.5-1 hour to obtain fecbucarb technical After heat storage and cold storage, its quality is 100% stable, and there is no content decrease, discoloration, or barrel expansion.
实施步骤:Implementation steps:
1、磷酸--甲酸溶液酸制备:1. Phosphoric acid-formic acid solution acid preparation:
--取工业磷酸(85%),甲醇(99.5%),调制成不同磷酸甲醇溶液。- Take industrial phosphoric acid (85%) and methanol (99.5%) to prepare different phosphoric acid methanol solutions.
2、稳定加入2. Join in stably
--向5台带搅拌玻璃反应器中加入合格仲丁威原药1000g,置入40℃-45℃的水浴中。- Add 1000g of qualified fecbucarb technical to 5 glass reactors with stirring, and put them in a water bath at 40℃-45℃.
--再向反应器中分别加入不同浓度、不同重量的磷酸-甲醇溶液,在控温搅拌的条件下均质0.5小时。--Add phosphoric acid-methanol solutions of different concentrations and different weights into the reactor, and homogenize for 0.5 hours under the condition of temperature control and stirring.
3、储存试验:3. Storage test:
----将加入稳定剂的仲丁威分别取样分析仲丁威的含量并作好记录,各取100g左右仲丁威,另分装入100ml透明磨口瓶中(保持密封无渗漏),贴好标签。----Sampling the fecbucarb with stabilizer to analyze the content of fecbucarb and make a record, take about 100g of fecbucarb each, and put them into 100ml transparent ground bottle (keep sealed and leak-free) , Label it well.
----将热储恒温箱温度设置45℃,对加入稳定剂(含空白)仲丁威进行储存试验。----Set the temperature of the thermal storage thermostat to 45°C, and carry out the storage test on adding the stabilizer (including blank) Fencarb.
---15天、30天后取样观察对照。--Sampling and observation control after 15 days and 30 days.
4、记录表4. Record table
1)、结果记录:1), result record:
Figure PCTCN2021098410-appb-000001
Figure PCTCN2021098410-appb-000001
图片见说明书附图。The pictures are shown in the attached drawings.
生产应用:Production application:
按量上述例4加入稳定剂后无客户投诉。There is no customer complaint after adding stabilizer according to the amount in the above example 4.
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本发明的保护范围并不仅局限于上述实施例,凡属于本发明思路下的技术方案均属于本发明的保护范围。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理前提下的若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。The basic principles, main features and advantages of the present invention have been shown and described above. The protection scope of the present invention is not limited to the above-mentioned embodiments, and all technical solutions under the idea of the present invention belong to the protection scope of the present invention. It should be pointed out that for those of ordinary skill in the art, several improvements and modifications made without departing from the principle of the present invention should also be regarded as the protection scope of the present invention.

Claims (3)

  1. 一种仲丁威农药稳定剂,其特征在于,包括甲醇溶液和浓度为85%磷酸溶液;甲醇与磷酸溶液体系中磷酸的质量百分比为≥50%且<55%。A fenbucarb pesticide stabilizer, which is characterized in that it comprises a methanol solution and a phosphoric acid solution with a concentration of 85%; the mass percentage of phosphoric acid in the methanol and phosphoric acid solution system is ≥50% and <55%.
  2. 如权利要求1所述的仲丁威农药稳定剂,其特征在于,所述稳定剂在40℃--45℃搅拌条件加加入仲丁威农药,搅拌时间为0.5-1小时;稳定剂与仲丁威农药的质量比为0.4-0.42:1000。The fecbucarb pesticide stabilizer according to claim 1, wherein the stabilizer is added with fecbucarb pesticide under stirring conditions of 40°C-45°C, and the stirring time is 0.5-1 hour; The mass ratio of Dingwei pesticide is 0.4-0.42:1000.
  3. 一种仲丁威农药,其特征在于,包括仲丁威原药和稳定剂;稳定剂包括甲醇和浓度为85%磷酸溶液;仲丁威原药与稳定剂的质量比为0.4-0.42:1000;甲醇与磷酸溶液体系中磷酸的质量百分比浓度为50%-55%。A fecbucarb pesticide, which is characterized in that it comprises fecbucarb technical and a stabilizer; the stabilizer includes methanol and a phosphoric acid solution with a concentration of 85%; the mass ratio of fecbucarb technical and the stabilizer is 0.4-0.42:1000 ; The mass percentage concentration of phosphoric acid in the methanol and phosphoric acid solution system is 50%-55%.
PCT/CN2021/098410 2020-06-18 2021-06-04 Fenobucarb pesticide stabilizer and fenobucarb pesticide WO2021254179A1 (en)

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