CN102924404B - A kind of preparation method of bentazone sodium salt pulvis - Google Patents
A kind of preparation method of bentazone sodium salt pulvis Download PDFInfo
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- CN102924404B CN102924404B CN201210476972.9A CN201210476972A CN102924404B CN 102924404 B CN102924404 B CN 102924404B CN 201210476972 A CN201210476972 A CN 201210476972A CN 102924404 B CN102924404 B CN 102924404B
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- bentazone
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Abstract
The invention discloses bentazone sodium salt pulvis preparation method, that relate generally to is Chemicals preparation methods.Its technical problem to be solved is: the preparation method providing a kind of convenient and practical, cost-saving, bentazone sodium salt pulvis that can be mass-produced.Take isatoic anhydride as raw material, first in dichloroethane solvent system through reactions such as superamide synthesis, sulfonation synthesis, closed loop synthesis, then washing, buck extraction, concentrated, lower the temperature, crystallization and dry packing obtain the bentazone sodium salt pulvis that can directly use.This preparation method main technique principle is simple; Save link repeatedly, cost-saving; After the packing of product, user can directly use, and succinctly facilitates environmental protection.
Description
Technical field
The present invention relates to Chemicals preparation method technical field, specifically belong to a kind of preparation method of bentazone sodium salt pulvis.
Background technology
Bentazone is a kind of widely used low toxicity herbicide, and its mode of action, mechanism mainly realize with bentazone sodium salt: contact killing type tool optionally postemergence weed control, for cauline leaf process in seedling stage, is worked by blade contact.Dry land uses, and is first transmitted to inhibited photosynthesis in chloroplast(id) by blade face infiltration.Paddy field uses, and not only by blade face infiltration but also by root absorption, is transmitted to cauline leaf, strongly hinders weeds photosynthesis and water metabolism, causes nutrition hungry, makes physiological dysfunction and lethal.Effective constituent is detoxified, to crop safety to the weak glycoconjugates metabolism of activity in tolerable crop body.After dispenser, 8 ~ 16 weeks bentazones can be decomposed by the microorganisms in soil.Can be used for the crops such as paddy rice, soybean, peanut, wheat, in the structure of agricultural production of China, serve great function.It is first output bentazone raw pesticide that tradition uses, more former medicine is made aqua, and this method produces a large amount of sour water, and expends soda acid water, is unfavorable for production cost.
Summary of the invention
The object of this invention is to provide a kind of preparation method of bentazone sodium salt pulvis, overcome the deficiencies in the prior art, method is convenient and practical, the preparation method of cost-saving, the bentazone sodium salt pulvis that can be mass-produced.
The technical solution used in the present invention is as follows:
A kind of preparation method of bentazone sodium salt pulvis, take isatoic anhydride as raw material, first in dichloroethane solvent system through reactions such as superamide synthesis, sulfonation synthesis, closed loop synthesis, the first step, terminates organic phase washing after closed loop synthesis, organic phase is added suitable quantity of water for entering to extract still, when slowly adding alkali adjustment PH=8 ~ 9, stop adding alkali, stir repetition measurement half an hour PH=8 ~ 9, stop stirring and leave standstill;
Second step, treat the layering of the first step solution left standstill: get upper water phase materials for entering concentration kettle, aqueous phase bentazone content is surveyed in sampling, carries out calculating concentrate according to aqueous phase bentazone content, concentrated rear aqueous phase bentazone content >=48% reaches requirement;
3rd step, concentrated terminates, and material is crossed to cooling still, stirs logical salt solution fast and is cooled to 9-11 DEG C, through Plate Filtration to crystallization kettle, excessively completely dries up sheet frame.
4th step, crystallization kettle opens the cooling of chuck salt solution, about within 2 ~ 3 hours, needing slow cooling to 0 DEG C early stage, later stage salt solution valve wide open, when temperature is down to about-5 DEG C, observe in still and whether have solid to separate out, until reduce cooling rate after having solid to separate out, stir 30 minutes, confirm have a large amount of material to separate out;
5th step, precipitation material is put into whizzer and is directly dried, and after drying, bentazone sodium salt is through flash evaporation drying, first time normal temperature flash distillation, second time control temperature 50 ~ 60 DEG C of flash distillations also add bentazone solid additive, and third time temperature control 100 ~ 110 DEG C of flash distillations must become bentazone sodium salt;
6th step, will evaporate the bentazone sodium salt packaging obtained, pack greatly, big area uses or water soluble film small packages directly uses.
Compared with the prior art, beneficial effect of the present invention is as follows:
Preparation method of the present invention, can obtain the bentazone sodium salt pulvis directly used that can add water.This bentazone sodium salt pulvis compared with bentazone aqua because be use time add water, so have great advantage on transportation cost.
Embodiment
A kind of preparation method of bentazone sodium salt pulvis, take isatoic anhydride as raw material, first in dichloroethane solvent system through reactions such as superamide synthesis, sulfonation synthesis, closed loop synthesis, the first step, terminates organic phase washing after closed loop synthesis, organic phase is added suitable quantity of water for entering to extract still, when slowly adding alkali adjustment PH=8 ~ 9, stop adding alkali, stir repetition measurement half an hour PH=8 ~ 9, stop stirring and leave standstill;
Second step, treat the layering of the first step solution left standstill: get upper water phase materials for entering concentration kettle, aqueous phase bentazone content is surveyed in sampling, carries out calculating concentrate according to aqueous phase bentazone content, concentrated rear aqueous phase bentazone content >=48% reaches requirement;
3rd step, concentrated terminates, and material is crossed to cooling still, stirs logical salt solution fast and is cooled to 9-11 DEG C, through Plate Filtration to crystallization kettle, excessively completely dries up sheet frame.
4th step, crystallization kettle opens the cooling of chuck salt solution, about within 2 ~ 3 hours, needing slow cooling to 0 DEG C early stage, later stage salt solution valve wide open, when temperature is down to about-5 DEG C, observe in still and whether have solid to separate out, until reduce cooling rate after having solid to separate out, stir 30 minutes, confirm have a large amount of material to separate out;
5th step, precipitation material is put into whizzer and is directly dried, and after drying, bentazone sodium salt is through flash evaporation drying, first time normal temperature flash distillation, second time control temperature 50 ~ 60 DEG C of flash distillations also add bentazone solid additive, and third time temperature control 100 ~ 110 DEG C of flash distillations must become bentazone sodium salt;
6th step, will evaporate the bentazone sodium salt packaging obtained, pack greatly, big area uses or water soluble film small packages directly uses.
Now with by organic phase after closed loop synthesis, washing terminates, and enters to extract still add suitable quantity of water by standby for organic phase, slowly adds alkali when regulating PH=8 ~ 9, stops adding alkali, stir repetition measurement half an hour PH=8 ~ 9, stops stirring to leave standstill; After getting extraction layering, aqueous phase 300g (content 20%) obtains 120g aqueous phase after pouring into and concentrating in 250ml flask, and by its fast cooling 9-11 DEG C, and suction filtration obtains filtrate.Slow cooling-5 DEG C also produces a large amount of solid, and suction filtration obtains bentazone sodium salt crude product, finally dries and dries, and adds the grinding of solid-state auxiliary agent in proportion and evenly can obtain bentazone sodium salt pulvis.
Claims (1)
1. the preparation method of a bentazone sodium salt pulvis, it is characterized in that: take isatoic anhydride as raw material, first in dichloroethane solvent system through superamide synthesis, sulfonation synthesis, closed loop building-up reactions, the first step, organic phase washing after closed loop synthesis is terminated, organic phase being added suitable quantity of water for entering to extract still, slowly adding alkali and regulating pH value;
Second step, treat the layering of the first step solution left standstill: get upper water phase materials for entering concentration kettle, aqueous phase bentazone content is surveyed in sampling, carries out calculating concentrate according to aqueous phase bentazone content, concentrated rear aqueous phase bentazone content >=48% reaches requirement;
3rd step, concentrated terminates, and material is crossed to cooling still, stirs logical salt water for cooling fast, through Plate Filtration to crystallization kettle, excessively completely dries up sheet frame;
4th step, crystallization kettle opens the cooling of chuck salt solution, and early stage needs slow cooling to 0 DEG C in 2 ~ 3 hours, whether later stage salt solution valve wide open, when temperature is down to-5 DEG C, observe in still and have solid to separate out, until reduce cooling rate after having solid to separate out, stir 30 minutes, confirm have a large amount of material to separate out;
5th step, precipitation material is put into whizzer and is directly dried, and after drying, bentazone sodium salt is through flash evaporation drying, obtains bentazone sodium salt;
6th step, will evaporate the bentazone sodium salt packaging obtained, pack greatly, big area uses or water soluble film small packages directly uses;
Wherein, the described the first step adds alkali and regulates PH=8 ~ 9, described the 3rd step-down Wen Wendu to 9-11 DEG C, the 5th described step flash evaporation drying, will through three flash distillations, first time normal temperature flash distillation, second time control temperature 50 ~ 60 DEG C of flash distillations also add bentazone solid additive, third time temperature control 100 ~ 110 DEG C of flash distillations.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210476972.9A CN102924404B (en) | 2012-11-21 | 2012-11-21 | A kind of preparation method of bentazone sodium salt pulvis |
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| CN201210476972.9A CN102924404B (en) | 2012-11-21 | 2012-11-21 | A kind of preparation method of bentazone sodium salt pulvis |
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| CN102924404A CN102924404A (en) | 2013-02-13 |
| CN102924404B true CN102924404B (en) | 2016-01-20 |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105566249B (en) * | 2015-12-29 | 2019-06-04 | 浙江中山化工集团股份有限公司 | Prepare the process and thus obtained Bentazon sodium salt raw medicine of high-content Bentazon sodium salt raw medicine |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3935201A (en) * | 1973-11-15 | 1976-01-27 | Basf Aktiengesellschaft | Production of 2,1,3-benzothiadiazin-4-one-2,2-dioxides |
| CN1063688A (en) * | 1991-01-28 | 1992-08-19 | 南开大学 | The synthetic method of Bentazon herbicide |
| CN101481361A (en) * | 2008-01-09 | 2009-07-15 | 苏州联合伟业科技有限公司 | Technique of preparing high-purity bentazone raw pesticide |
| CN101863858A (en) * | 2010-06-07 | 2010-10-20 | 江苏绿利来股份有限公司 | Synthetic method of bentazone |
-
2012
- 2012-11-21 CN CN201210476972.9A patent/CN102924404B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3935201A (en) * | 1973-11-15 | 1976-01-27 | Basf Aktiengesellschaft | Production of 2,1,3-benzothiadiazin-4-one-2,2-dioxides |
| CN1063688A (en) * | 1991-01-28 | 1992-08-19 | 南开大学 | The synthetic method of Bentazon herbicide |
| CN101481361A (en) * | 2008-01-09 | 2009-07-15 | 苏州联合伟业科技有限公司 | Technique of preparing high-purity bentazone raw pesticide |
| CN101863858A (en) * | 2010-06-07 | 2010-10-20 | 江苏绿利来股份有限公司 | Synthetic method of bentazone |
Non-Patent Citations (1)
| Title |
|---|
| "除草剂苯达松新工艺的合成研究";周善波等;《江苏农药》;20001215(第4期);第2.2.3-2.2.4部分 * |
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Denomination of invention: Method for preparing bentazone sodium salt powder Effective date of registration: 20200603 Granted publication date: 20160120 Pledgee: Huishang Bank Co.,Ltd. Hefei Branch Pledgor: HEFEI XINGYU CHEMICAL Co.,Ltd. Registration number: Y2020980002756 |
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Date of cancellation: 20220921 Granted publication date: 20160120 Pledgee: Huishang Bank Co.,Ltd. Hefei Branch Pledgor: HEFEI XINGYU CHEMICAL Co.,Ltd. Registration number: Y2020980002756 |
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