Imidazethapyr sodium salt soluble concentrate
By reacting the imidazole niacin original drug with sodium-containing carbonate and defoaming agent under mechanical stirring, the imidazole niacin sodium salt solution agent was prepared, which solved the problem of imidazole niacin easy decomposition in a strong alkaline environment and achieved a stable solution Preparation and efficient decomposition stability.
Patent Information
- Application Number
- CN202411461396.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-18
- Publication Date
- 2025-01-14
AI Technical Summary
Imidazoleacenicotinic acid is prone to decomposition in a strong alkaline environment, resulting in the failure to register the use of imidazoleacenicotinic acid sodium salt solution agent in the prior art.
By reacting the imidazole niacin original drug with sodium-containing carbonate and defoaming agent under mechanical stirring, adding synergistic aids, imidazole niacin sodium salt solution is prepared, the stirring rate and temperature are controlled to prevent foam from being generated, and the solution is clear and clear transparent.
The prepared imidazole acenicotinic acid sodium salt solution has stable quality, passed the hot and cold storage, no abnormal phenomena such as layering, crystallization, agglomeration, turbidity, etc., and the decomposition stability is improved, and it meets the decomposition rate requirements of less than 5% of the industry standard.
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Abstract
Description
Technical Field
[0001] The invention discloses a method for preparing an imazethapyr sodium salt soluble solution, and belongs to the technical field of pesticides. Background Art
[0002] Imidazolin, also known as imazamox, belongs to the imidazolinone herbicide and is generally used in soybean fields. It has a good control effect on grass weeds in legume fields. Imidazolin is stable in acidic and neutral environments, but is easily decomposed in strong alkaline environments.
[0003] At present, the imidazolin registered in China are mainly imidazolin technical, imidazolin aqueous solution and imidazolin ammonium salt soluble solution. Imidazolin sodium salt has not yet been registered for use. This is related to the fact that imidazolin is easily decomposed in a strong alkaline environment. Summary of the invention
[0004] In view of the shortcomings of the prior art, the object of the present invention is to provide a method for preparing a soluble solution of imidazoline sodium salt. The specific method is as follows: Technical Solutions A soluble imidazole sodium salt solution comprises imidazole original drug, sodium carbonate, synergist, defoamer and water. The imidazole original drug is added into water, and the defoamer is added; the sodium carbonate is added under mechanical stirring until the aqueous solution is clarified; the synergist and the remaining amount of water are added, and stirring is continued until the solution is clear and transparent, so as to obtain the imidazole sodium salt.
[0005] The sodium-containing carbonate is one or more of sodium carbonate and sodium bicarbonate.
[0006] The molar ratio of imidacloprid technical to sodium bicarbonate is 1:0.65-1.5, preferably, the molar ratio of imidacloprid technical to sodium bicarbonate is 1:0.85-1.2.
[0007] The molar ratio of imidacloprid technical to sodium carbonate is 1:0.4-0.7, preferably, the molar ratio of imidacloprid technical to sodium carbonate is 1:0.45-0.6.
[0008] The defoamer is a compound of one or more of amino-modified silicone oil, quaternary ammonium salt / amino-modified silicone oil, hydroxyl / amino-modified silicone oil, polyether amino-modified silicone oil, epoxy-modified silicone oil, acrylate-modified silicone oil and siloxane.
[0009] The amino-modified silicone oil, hydroxyl-modified silicone oil and polyether-modified silicone oil are provided by Zhongbao Silicon Material Technology Co., Ltd.
[0010] The preparation method of the quaternary ammonium salt modified silicone oil is as follows: hydrogen-containing silicone oil and allyl-terminated epoxy polyether are mixed to react to obtain double-terminal epoxy silicone oil; double-terminal epoxy silicone oil and quaternary ammonium salt are reacted under catalyst conditions to obtain quaternary ammonium salt modified silicone oil, wherein the quaternary ammonium salt is obtained by reacting triethanolamine with hydrochloric acid, and the catalyst is chloroplatinic acid.
[0011] The epoxy-modified silicone oil and siloxane are provided by Hubei Xingrui Silicon Materials Co., Ltd.
[0012] The acrylate-modified silicone oil is obtained by reacting allyl acrylate with hydrogen-containing silicone oil in the presence of a catalyst and a polymerization inhibitor.
[0013] The defoaming agent is added before sodium carbonate or sodium bicarbonate, with an amount of 0.5%-1%, to inhibit the generation of foam in the reaction, adjust the pH of the system, and increase the decomposition stability of imidazole ethyl nicotinic acid in the solution. If the defoaming agent is added after sodium carbonate / sodium bicarbonate, it will cause the material to overflow the container. Therefore, the defoaming agent is added first, and then sodium carbonate / sodium bicarbonate.
[0014] In view of the above problems, a technical solution is also proposed. The raw materials involved are the same as above. The preparation method of imidazolin sodium salt soluble preparation comprises the following steps: (1) Dissolve sodium carbonate or sodium bicarbonate in water to prepare solution A; (2) Mix the defoamer and imidazolin technical and add them into a flask to obtain material B; The defoamer is a compound of one or more of amino-modified silicone oil, quaternary ammonium salt / amino-modified silicone oil, hydroxyl / amino-modified silicone oil, polyether amino-modified silicone oil, epoxy-modified silicone oil, acrylate-modified silicone oil and siloxane.
[0015] The amino-modified silicone oil, hydroxyl-modified silicone oil and polyether-modified silicone oil are provided by Zhongbao Silicon Material Technology Co., Ltd.
[0016] The preparation method of the quaternary ammonium salt modified silicone oil is as follows: hydrogen-containing silicone oil and allyl-terminated epoxy polyether are mixed to react to obtain double-terminal epoxy silicone oil; double-terminal epoxy silicone oil and quaternary ammonium salt are reacted under catalyst conditions to obtain quaternary ammonium salt modified silicone oil, wherein the quaternary ammonium salt is obtained by reacting triethanolamine with hydrochloric acid, and the catalyst is chloroplatinic acid.
[0017] The epoxy-modified silicone oil and siloxane are provided by Hubei Xingrui Silicon Materials Co., Ltd.
[0018] The acrylate-modified silicone oil is obtained by reacting allyl acrylate with hydrogen-containing silicone oil in the presence of a catalyst and a polymerization inhibitor.
[0019] (3) Add solution A to material B, control the stirring rate and reaction temperature, stir until the solution is clear, and then add the synergist to obtain imidazolyl nicotinic acid sodium salt.
[0020] In step (3), solution A is added dropwise; The stirring method is magnetic stirring or mechanical stirring, and the stirring rate is 150-400 rpm. Too high a stirring rate will cause a large amount of foam to be generated. Preferably, the stirring rate is 200-300 rpm.
[0021] The method has a simple preparation process, readily available raw materials, and low energy consumption. The imidazolyl nicotinic acid sodium salt soluble solution prepared by the method has stable quality, is qualified for cold and hot storage, and has no abnormal phenomena such as stratification, crystallization, agglomeration, turbidity, etc. DETAILED DESCRIPTION
[0022] The defoamer is a compound of one or more of amino-modified silicone oil, quaternary ammonium salt / amino-modified silicone oil, hydroxyl / amino-modified silicone oil, polyether amino-modified silicone oil, epoxy-modified silicone oil, acrylate-modified silicone oil and siloxane.
[0023] The amino-modified silicone oil, hydroxyl-modified silicone oil and polyether-modified silicone oil are provided by Zhongbao Silicon Material Technology Co., Ltd.
[0024] The preparation method of the quaternary ammonium salt modified silicone oil is as follows: hydrogen-containing silicone oil and allyl-terminated epoxy polyether are mixed to react to obtain double-terminal epoxy silicone oil; double-terminal epoxy silicone oil and quaternary ammonium salt are reacted under catalyst conditions to obtain quaternary ammonium salt modified silicone oil, wherein the quaternary ammonium salt is obtained by reacting triethanolamine with hydrochloric acid, and the catalyst is chloroplatinic acid.
[0025] The epoxy-modified silicone oil and siloxane are provided by Hubei Xingrui Silicon Materials Co., Ltd.
[0026] The acrylate-modified silicone oil is obtained by reacting allyl acrylate with hydrogen-containing silicone oil in the presence of a catalyst and a polymerization inhibitor.
[0027] Example 1 Mix 102.6g of imidazole ethyl nicotinic acid technical (active ingredient content 97.5%) and 300g of distilled water, add 5g of quaternary ammonium salt modified silicone oil as a defoaming agent, weigh 24.68g of sodium bicarbonate and add it into a flask (do not dissolve in water, there is water in the flask) (imidazole ethyl nicotinic acid: sodium bicarbonate = 1:0.85), stir the reaction at 200rpm until the solution is clear, add 80g of synergistic aid, make up water to 1000g, continue stirring until the solution is clear, and obtain a 10% imidazole ethyl nicotinic acid soluble solution.
[0028] The synergistic aid is prepared by mixing alkyl glucoside 0810, betaine and fatty alcohol polyoxyethylene ether in a ratio of 4:1:0.1 and stirring and mixing them evenly.
[0029] Example 2 Add 102.6g of imidazole acetylcholine technical (active ingredient content 97.5%) and 300g of distilled water into a flask, add 5g of compound defoamer, weigh 34.84g of sodium bicarbonate and add into the flask (imidazole acetylcholine: sodium bicarbonate = 1:1.2), stir at 250rpm until the solution is clear, add 80g of synergistic aid, make up to 1000g with water, continue stirring until the solution is clear, and obtain 10% imidazole acetylcholine soluble solution.
[0030] The compound defoamer is prepared by mixing polyether-modified silicone oil and siloxane in a weight ratio of 1:0.75, and heating and stirring at 40-50° C. for 30 minutes.
[0031] The synergistic aid is prepared by mixing alkyl glucoside 0810, sodium lignin sulfonate and fatty alcohol polyoxyethylene ether in a ratio of 6:1:0.15 and stirring and mixing them evenly.
[0032] Example 3 Add 102.6g of imidazole acetylcholine technical (active ingredient content 97.5%) and 300g of distilled water into a flask, and add 5g of compound defoamer, weigh 16.49g of sodium carbonate and add it into the flask (imidazole acetylcholine: sodium carbonate = 1:0.45), stir at 250rpm until the solution is clear, add 80g of synergistic aid, make up to 1000g with water, and continue stirring until the solution is clear.
[0033] The composite defoamer is prepared by mixing quaternary ammonium salt modified silicone oil and acrylate modified silicone oil in a weight ratio of 1:1.2, and heating and stirring at 30° C. for 15 minutes.
[0034] The synergistic aid is prepared by mixing alkyl polyglucoside 0810, sodium dodecylbenzene sulfonate and fatty alcohol polyoxyethylene ether in a ratio of 12:1:0.3 and stirring and mixing them evenly.
[0035] Example 4 Add 102.6g of imidazole acetylcholine technical (active ingredient content 97.5%) and 300g of distilled water into a flask, add 8g of compound defoamer, weigh 21.98g of sodium carbonate and add it into the flask (imidazole acetylcholine: sodium carbonate = 1:0.6), stir at 200rpm until the solution is clear, add 80g of synergistic aid, make up to 1000g with water, and continue stirring until the solution is clear.
[0036] The compound defoamer is prepared by mixing polyether modified silicone oil and epoxy modified silicone oil in a weight ratio of 3:1, and heating and stirring at 40-45° C. for 60 minutes.
[0037] The synergistic aid is prepared by mixing alkyl polyglycoside 0810, sodium lauryl sulfate and fatty alcohol polyoxyethylene ether in a ratio of 10:1:0.25 and stirring and mixing them evenly.
[0038] Example 5 Add 102.6g of imidazole ethyl nicotinic acid technical (active ingredient content 97.5%) and 300g of distilled water into a flask, and add 5g of compound defoamer. Weigh 24.68g of sodium bicarbonate and add water to prepare a solution. Use a dropping funnel to slowly add it to the flask (imidazole ethyl nicotinic acid: sodium bicarbonate = 1:0.85). Stir the reaction at 250rpm until the solution is clear. Add 80g of synergistic aid, make up to 1000g with water, and continue stirring until the solution is clear.
[0039] The composite defoamer is prepared by mixing quaternary ammonium salt modified silicone oil and hydroxyl modified silicone oil in a weight ratio of 1:1 and stirring at 25° C. for 10 minutes.
[0040] The synergistic aid is prepared by mixing alkyl glucoside 0810, betaine and sodium lignin sulfonate in a ratio of 4:1:0.25 and stirring and mixing them evenly.
[0041] Example 6 Add 102.6g of imidazole ethyl nicotinic acid technical (active ingredient content 97.5%) and 300g of distilled water into a flask, and add 5g of compound defoamer. Weigh 34.84g of sodium bicarbonate and add water to prepare a solution. Use a dropping funnel to slowly add it into the flask (imidazole ethyl nicotinic acid: sodium bicarbonate = 1:1.2). Stir the reaction at 300rpm until the solution is clear. Add 80g of synergistic agent, make up to 1000g with water, and continue stirring until the solution is clear.
[0042] The compound defoamer is prepared by mixing polyether-modified silicone oil and siloxane in a weight ratio of 4:3, and heating and stirring at 40-50° C. for 30 minutes.
[0043] The synergistic aid is prepared by mixing alkyl glucoside 0810, betaine and sodium lauryl sulfate in a ratio of 8:2:0.25 and stirring the mixture to form a uniform mixture.
[0044] Example 7 Add 102.6g of imidazole ethyl nicotinic acid technical (active ingredient content 97.5%) and 300g of distilled water into a flask, and add 5g of compound defoamer. Weigh 18.32g of sodium bicarbonate and add water to prepare a solution. Use a dropping funnel to slowly add it into the flask (imidazole ethyl nicotinic acid: sodium carbonate = 1:0.5). Stir the reaction at 250rpm until the solution is clear. Add 80g of synergistic agent, make up to 1000g with water, and continue stirring until the solution is clear.
[0045] The composite defoamer is prepared by mixing quaternary ammonium salt modified silicone oil and acrylate modified silicone oil in a weight ratio of 1:1.2, and heating and stirring at 30° C. for 15 minutes.
[0046] The synergistic aid is prepared by mixing alkyl polyglycoside 0810, betaine and sodium dodecylbenzene sulfonate in a ratio of 4:1:0.2 and stirring and mixing them evenly.
[0047] Example 8 Add 102.6g of imidazole ethyl nicotinic acid technical (active ingredient content 97.5%) and 300g of distilled water into a flask, and add 8g of compound defoamer. Weigh 20.15g of sodium bicarbonate and add water to prepare a solution. Use a dropping funnel to slowly add it into the flask (imidazole ethyl nicotinic acid: sodium carbonate = 1:0.55). Stir the reaction at 300rpm until the solution is clear. Add 80g of synergistic agent, make up to 1000g with water, and continue stirring until the solution is clear.
[0048] The compound defoamer is prepared by mixing polyether modified silicone oil and epoxy modified silicone oil in a weight ratio of 3:1, and heating and stirring at 40-45° C. for 60 minutes.
[0049] The synergistic aid is prepared by mixing alkyl glucoside 0810, betaine and sodium lignin sulfonate in a ratio of 4:1:0.25 and stirring and mixing them evenly.
[0050] Comparative Example 1 102.6 g of imidazole ethyl nicotinic acid technical (active ingredient content 97.5%) and 300 g of distilled water were added to a flask, 41.47 g of 30% sodium hydroxide solution was added dropwise into the flask (imidazole ethyl nicotinic acid: sodium hydroxide = 1:0.9), and the reaction was stirred at 250 rpm until the solution was clear, 80 g of a synergist was added, water was added to 1000 g, and stirring was continued until the solution was clear. The synergist was alkyl glycoside 0810, betaine, and fatty alcohol polyoxyethylene ether, which were mixed in a ratio of 4:1:0.1, and stirred to mix evenly.
[0051] Comparative Example 2 Add 102.6g of imidazolin technical (active ingredient content 97.5%) and 300g of distilled water into a flask, add 46.08g of 30% sodium hydroxide solution dropwise into the flask (imidazolin: sodium hydroxide = 1:1), stir at 250rpm until the solution is clear, add 80g of synergistic aid, add water to 1000g, and continue stirring until the solution is clear.
[0052] The synergistic aid is prepared by mixing alkyl polyglycoside 0810, betaine and sodium dodecylbenzene sulfonate in a ratio of 4:1:0.2 and stirring and mixing them evenly.
[0053] Comparative Example 3: 102.6 g of imidazole acetylcholine technical (active ingredient content 97.5%) and 300 g of distilled water were added to a flask, 50.69 g of 30% sodium hydroxide solution was added dropwise to the flask (imidazole acetylcholine: sodium hydroxide = 1:1.1), the reaction was stirred at 250 rpm until the solution was clear, 80 g of synergistic aid was added, water was added to 1000 g, and stirring was continued until the solution was clear.
[0054] The synergistic aid is prepared by mixing alkyl polyglycoside 0810, sodium lauryl sulfate and fatty alcohol polyoxyethylene ether in a ratio of 10:1:0.25 and stirring to mix them evenly.
[0055] Comparative Example 4: 102.6 g of imidazole ethyl nicotinic acid technical (active ingredient content 97.5%) and 300 g of distilled water were added to a flask, 41.47 g of 30% sodium hydroxide solution was added dropwise to the flask (imidazole ethyl nicotinic acid: sodium hydroxide = 1:0.9), and then 5 g of a defoaming agent prepared by mixing amino polyether modified silicone oil and epoxy modified silicone oil was added, and the mixture was stirred at 250 rpm until the solution was clear, 80 g of a synergist was added, water was added to 1000 g, and stirring was continued until the solution was clear.
[0056] The synergistic aid is prepared by mixing alkyl glucoside 0810, betaine and sodium lignin sulfonate in a ratio of 4:1:0.25 and stirring and mixing them evenly.
[0057] Comparative Example 5: 102.6 g of imidazole ethyl nicotinic acid technical (active ingredient content 97.5%) and 300 g of distilled water were added to a flask, 50.69 g of 30% sodium hydroxide solution was added dropwise into the flask (imidazole ethyl nicotinic acid: sodium hydroxide = 1:1.1), and then 5 g of a defoaming agent prepared by mixing quaternary ammonium salt / amino-modified silicone oil and acrylate-modified silicone oil was added, and the mixture was stirred at 250 rpm until the solution was clear, 80 g of a synergistic agent was added, water was added to 1000 g, and stirring was continued until the solution was clear.
[0058] The synergistic aid is prepared by mixing alkyl polyglucoside 0810, sodium dodecylbenzene sulfonate and fatty alcohol polyoxyethylene ether in a ratio of 12:1:0.3 and stirring and mixing them evenly.
[0059] Index detection According to industry standards, high performance liquid chromatography and a pH meter were used to detect the content and pH of the room temperature (25°C) and hot storage samples (54°C) of the embodiments and comparative examples, and the decomposition rate of the samples after hot storage was calculated. The results are shown in the table below.
[0060]
[0061] As can be seen from the above table, in the comparative example, sodium hydroxide was used to react with imidazole acetylcholine, and imidazole acetylcholine was decomposed more. However, in the examples of the present application, the decomposition rate of imidazole acetylcholine sodium salt prepared by using sodium bicarbonate or sodium carbonate was lower, which met the requirements of less than 5% in various standards.
Claims
1. A soluble preparation of imidacloprid sodium salt, characterized in that: The formula comprises the following components: imidazolin technical, sodium carbonate salt, synergistic aid, defoamer and water; the defoamer is a compound of one or more of amino-modified silicone oil, quaternary ammonium salt-modified silicone oil, hydroxyl-modified silicone oil, polyether-modified silicone oil, epoxy-modified silicone oil, acrylate-modified silicone oil and siloxane.
2. The imidazoline sodium salt soluble preparation according to claim 1, characterized in that: The sodium carbonate salt is one or more of sodium carbonate and sodium bicarbonate.
3. The imidazoline sodium salt soluble preparation according to claim 2, characterized in that: The molar ratio of imidacloprid technical to sodium bicarbonate is 1:0.65-1.5, preferably, the molar ratio of imidacloprid technical to sodium bicarbonate is 1:0.85-1.
2.
4. The imazethapyr sodium salt soluble preparation according to claim 2, characterized in that: The molar ratio of imidacloprid technical to sodium carbonate is 1:0.4-0.7, preferably, the molar ratio of imidacloprid technical to sodium carbonate is 1:0.45-0.
6.
5. The imazethapyr sodium salt soluble preparation according to claim 1, characterized in that: The defoaming agent is added before sodium carbonate or sodium bicarbonate, and the dosage is 0.5%-1%.
6. The imazethapyr sodium salt soluble preparation according to claim 1, characterized in that: The synergistic aid is selected from one or more of alkyl polyglycoside 0810, fatty alcohol polyoxyethylene ether, betaine, sodium dodecylbenzene sulfonate, sodium dodecyl sulfate, and sodium lignin sulfonate.
7. The method for preparing the soluble solution of imazethapyr sodium salt according to any one of claims 1 to 6, characterized in that: The steps include: (1) Dissolve sodium carbonate or sodium bicarbonate in water to prepare solution A; (2) Mixing the defoamer and imidacloprid technical to obtain material B; (3) Add solution A to material B, control the stirring rate and reaction temperature, stir until the solution is clear, and then add the synergist to obtain imidazolyl nicotinic acid sodium salt.
8. The method for preparing the soluble solution of imazethapyr sodium salt according to claim 7, characterized in that: Solution A was added dropwise; the stirring rate was 150~400rpm.