CN102924405A - Method for preparing bentazone aqueous agent - Google Patents
Method for preparing bentazone aqueous agent Download PDFInfo
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- CN102924405A CN102924405A CN2012104769911A CN201210476991A CN102924405A CN 102924405 A CN102924405 A CN 102924405A CN 2012104769911 A CN2012104769911 A CN 2012104769911A CN 201210476991 A CN201210476991 A CN 201210476991A CN 102924405 A CN102924405 A CN 102924405A
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Abstract
The invention discloses a method for preparing a bentazone aqueous agent, belonging to the technical field of preparation of chemical products and aiming to provide a method for preparing a bentazone aqueous agent which is more environment-friendly and has higher appearance quality. The method comprises the following steps: taking isatoic anhydride as a raw material, carrying out amide synthesis, sulfonation synthesis and closed-loop synthesis reactions and the like in a dichloroethane solvent system, washing by water, extracting by alkaline water and concentrating by a thin-film evaporator to obtain the light-yellow bentazone aqueous agent. Compared with the traditional method, the method provided by the invention adopts less acid, base and strongly-acidic wastewater and improves the quality of the product.
Description
Technical field
The present invention relates to the Chemicals preparing technical field, specifically belong to a kind of preparation method of bentazone aqua.
Background technology
Bentazone is a kind of important fine chemical product, is a kind of widely used weedicide, can be used for the crops such as paddy rice, soybean, peanut, wheat.The preparation method of traditional bentazone aqua is so that isatoic anhydride is synthetic through superamide in the ethylene dichloride system, sulfonation synthetic, closed loop synthetic, washing, alkali extraction, aqueous phase as acidified, centrifugal (sheet frame) discharging, add scale tensio-active agent preparation aqua.Prior art repeat consumption soda acid, cost is higher; Produce acid waste water, environmental protection pressure is large; Bentazone aqua color is darker, easily produces a small amount of throw out after placing.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method of bentazone aqua, overcome the deficiencies in the prior art, quality product is higher, and production cost is lower, reduces sewage discharge.
The technical solution used in the present invention is as follows:
A kind of preparation method of bentazone aqua, described the method, the first step, adopt closed loop synthetic after organic phase through wash complete after, throw gac, constant temperature stir 30 minutes through Plate Filtration to extracting still; Crossed,, washed to extracting still with tap water washing sheet frame; Dry up 30 minutes, unload gac;
Second step, the diluted alkaline preparation: standby 32% Ionic Membrane adds tap water preparation alkali content to 5%～31% to preparing still, prepares for extracting;
In the 3rd step, extraction kettle: slowly drip the in advance diluted alkaline of preparation, dropping temperature is controlled at 25～60 ℃, transfers material pH value to 3～11;
The 4th step, after the material pH value mixes up, left standstill 2 hours, get the upper water phase materials and cross to water transfer still through sheet frame;
In the 5th step, content is surveyed in the sampling of transfer still water, is concentrated into aqueous phase content according to measuring content by thin-film evaporator;
In the 6th step, the standby still that enters to lower the temperature of concentrated good aqua drips liquid caustic soda and transfers pH value=7, throws 1% stablizer, stirs after 1 hour, slowly opens salt solution and is cooled to-1～3 ℃ and crosses to the finished product still the excessively complete sheet frame that dries up through sheet frame.
In the 7th step, finished product content is surveyed in the sampling of finished product still, and qualified 2% liquid surfactant of taking out of content stirred 30 minutes, pumped into finished product storage tank.
Described stablizer is a kind of in yellow soda ash, sodium bicarbonate, sodium sulfate, sodium bisulfite and the S-WAT.
The 3rd step, described middle dropping temperature was controlled at 35～45 ℃, pH value to 5～7.
The described diluted alkaline content of second step is controlled at 14～18%.
Compared with the prior art, beneficial effect of the present invention is as follows:
The quality product of the inventive method preparation is higher, and production cost is lower, reduces sewage discharge.
Description of drawings
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is traditional process flow sheet.
Embodiment
A kind of preparation method of bentazone aqua, described the method, the first step, adopt closed loop synthetic after organic phase through wash complete after, throw gac, constant temperature stir 30 minutes through Plate Filtration to extracting still; Crossed,, washed to extracting still with tap water washing sheet frame; Dry up 30 minutes, unload gac;
Second step, the diluted alkaline preparation: standby 32% Ionic Membrane adds tap water preparation alkali content to 5%～31% to preparing still, prepares for extracting;
In the 3rd step, extraction kettle: slowly drip the in advance diluted alkaline of preparation, dropping temperature is controlled at 25～60 ℃, transfers material pH value to 3～11;
The 4th step, after the material pH value mixes up, left standstill 2 hours, get the upper water phase materials and cross to water transfer still through sheet frame;
In the 5th step, content is surveyed in the sampling of transfer still water, is concentrated into aqueous phase content according to measuring content by thin-film evaporator;
In the 6th step, the standby still that enters to lower the temperature of concentrated good aqua drips liquid caustic soda and transfers pH value=7, throws 1% stablizer, stirs after 1 hour, slowly opens salt solution and is cooled to-1～3 ℃ and crosses to the finished product still the excessively complete sheet frame that dries up through sheet frame.
In the 7th step, finished product content is surveyed in the sampling of finished product still, and qualified 2% liquid surfactant of taking out of content stirred 30 minutes, pumped into finished product storage tank.Described stablizer is a kind of in yellow soda ash, sodium bicarbonate, sodium sulfate, sodium bisulfite and the S-WAT.
Now with 300g organic phase (bentazone content 40%), the 2g gac drops in the 500ml flask, stirring at normal temperature is suction filtration after 10 minutes, the washing of 200ml tap water, getting filtrate drops in the flask, prepare simultaneously 1%～31% diluted alkaline, in 25～60 ℃ of temperature, slowly regulate control filtrate pH value 3～11 with the diluted alkaline for preparing, left standstill 2 hours, the stratified pumping phase is regulated PH=7 with a small amount of liquid caustic soda after calculating is concentrated, throws approximately 6g stablizer, cool to-1～4 ℃, suction filtration is got filtrate and is dropped into approximately 12g tensio-active agent, obtains transparent faint yellow bentazone aqua, aqua long time without deposit deposits yields.
Claims (4)
1. the preparation method of a bentazone aqua is characterized in that: described the method, the first step, adopt closed loop synthetic after organic phase through wash complete after, throw gac, constant temperature stir 30 minutes through Plate Filtration to extracting still; Crossed,, washed to extracting still with tap water washing sheet frame; Dry up 30 minutes, unload gac;
Second step, the diluted alkaline preparation: standby 32% Ionic Membrane adds tap water preparation alkali content to 5%～31% to preparing still, prepares for extracting;
In the 3rd step, extraction kettle: slowly drip the in advance diluted alkaline of preparation, dropping temperature is controlled at 25～60 ℃, transfers material pH value to 3～11;
The 4th step, after the material pH value mixes up, left standstill 2 hours, get the upper water phase materials and cross to water transfer still through sheet frame;
In the 5th step, content is surveyed in the sampling of transfer still water, is concentrated into aqueous phase content according to measuring content by thin-film evaporator;
In the 6th step, the standby still that enters to lower the temperature of concentrated good aqua drips liquid caustic soda and transfers pH value=7, throws 1% stablizer, stirs after 1 hour, slowly opens salt solution and is cooled to-1～3 ℃ and crosses to the finished product still the excessively complete sheet frame that dries up through sheet frame.
In the 7th step, finished product content is surveyed in the sampling of finished product still, and qualified 2% liquid surfactant of taking out of content stirred 30 minutes, pumped into finished product storage tank.
2. the preparation method of a kind of bentazone aqua according to claim 1 is characterized in that: described stablizer is a kind of in yellow soda ash, sodium bicarbonate, sodium sulfate, sodium bisulfite and the S-WAT.
3. the preparation method of a kind of bentazone aqua according to claim 1 is characterized in that: the 3rd step, described middle dropping temperature was controlled at 35～45 ℃, pH value to 5～7.
4. the preparation method of a kind of bentazone aqua according to claim 1, it is characterized in that: the described diluted alkaline content of second step is controlled at 14～18%.
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| CN201210476991.1A CN102924405B (en) | 2012-11-21 | 2012-11-21 | A kind of preparation method of bentazone aqua |
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| CN201210476991.1A CN102924405B (en) | 2012-11-21 | 2012-11-21 | A kind of preparation method of bentazone aqua |
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| CN102924405B CN102924405B (en) | 2016-01-20 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103749482A (en) * | 2013-12-24 | 2014-04-30 | 江苏天容集团股份有限公司 | High-quality bentazone aqueous solution and preparation method thereof |
| CN106543101A (en) * | 2016-11-08 | 2017-03-29 | 南京大学 | A kind of bentazone decolourizes and method of purification |
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| US3875155A (en) * | 1973-03-31 | 1975-04-01 | Basf Ag | Process for making salts of 3-isopropyl-2,1,3-benzothiadiazin-(4)-one-2,2-dioxide |
| US4451378A (en) * | 1981-10-19 | 1984-05-29 | Basf Aktiengesellschaft | Isolation of 3-isopropyl-2,1,3-benzothiadiazin-4-one-2,2-dioxide from waste water from its preparation |
| WO1987003588A1 (en) * | 1985-12-03 | 1987-06-18 | Nitrokémia Ipartelepek | Process for the preparation of 3-isopropyl-benzo-2-thia-1,3-diazinone-(4)-2,2-dioxide |
| CN1063688A (en) * | 1991-01-28 | 1992-08-19 | 南开大学 | The synthetic method of Bentazon herbicide |
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| 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 |
| CN101830866A (en) * | 2010-02-03 | 2010-09-15 | 江苏省农用激素工程技术研究中心有限公司 | Method for preparing bentazone |
| CN102617511A (en) * | 2012-03-09 | 2012-08-01 | 东北大学 | Wastewater-free preparation method of bentazon |
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2012
- 2012-11-21 CN CN201210476991.1A patent/CN102924405B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3875155A (en) * | 1973-03-31 | 1975-04-01 | Basf Ag | Process for making salts of 3-isopropyl-2,1,3-benzothiadiazin-(4)-one-2,2-dioxide |
| US4451378A (en) * | 1981-10-19 | 1984-05-29 | Basf Aktiengesellschaft | Isolation of 3-isopropyl-2,1,3-benzothiadiazin-4-one-2,2-dioxide from waste water from its preparation |
| WO1987003588A1 (en) * | 1985-12-03 | 1987-06-18 | Nitrokémia Ipartelepek | Process for the preparation of 3-isopropyl-benzo-2-thia-1,3-diazinone-(4)-2,2-dioxide |
| CN1063688A (en) * | 1991-01-28 | 1992-08-19 | 南开大学 | The synthetic method of Bentazon herbicide |
| CN1267287A (en) * | 1997-08-19 | 2000-09-20 | 巴斯福股份公司 | Preparation of 3-isopropyl-1H-2,1,3-benzothiadiazin-4(3H)-one-2,2-dioxide |
| 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 |
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| CN102617511A (en) * | 2012-03-09 | 2012-08-01 | 东北大学 | Wastewater-free preparation method of bentazon |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103749482A (en) * | 2013-12-24 | 2014-04-30 | 江苏天容集团股份有限公司 | High-quality bentazone aqueous solution and preparation method thereof |
| CN103749482B (en) * | 2013-12-24 | 2017-01-18 | 江苏天容集团股份有限公司 | High-quality bentazone aqueous solution and preparation method thereof |
| CN106543101A (en) * | 2016-11-08 | 2017-03-29 | 南京大学 | A kind of bentazone decolourizes and method of purification |
| CN106543101B (en) * | 2016-11-08 | 2018-10-23 | 南京大学 | A kind of decoloration of Bentazon and method of purification |
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| CN102924405B (en) | 2016-01-20 |
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Denomination of invention: Method for preparing bentazone aqueous agent 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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Effective date of registration: 20221116 Address after: No. 9, Xingfu Road, Building Materials Chemical Industry Zone, Yumen City, Jiuquan City, Gansu Province, 735200 Patentee after: Gansu Western Xinyu Chemical Co.,Ltd. Address before: 230000 Hefei Circular Economy Demonstration Park, Anhui Province Patentee before: HEFEI XINGYU CHEMICAL Co.,Ltd. |
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