CN102924405B - A kind of preparation method of bentazone aqua - Google Patents
A kind of preparation method of bentazone aqua Download PDFInfo
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- CN102924405B CN102924405B CN201210476991.1A CN201210476991A CN102924405B CN 102924405 B CN102924405 B CN 102924405B CN 201210476991 A CN201210476991 A CN 201210476991A CN 102924405 B CN102924405 B CN 102924405B
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- still
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- content
- aqua
- bentazone
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- 239000005476 Bentazone Substances 0.000 title claims abstract description 18
- ZOMSMJKLGFBRBS-UHFFFAOYSA-N bentazone Chemical compound C1=CC=C2NS(=O)(=O)N(C(C)C)C(=O)C2=C1 ZOMSMJKLGFBRBS-UHFFFAOYSA-N 0.000 title claims abstract description 18
- CNBGNNVCVSKAQZ-UHFFFAOYSA-N benzidamine Natural products C12=CC=CC=C2C(OCCCN(C)C)=NN1CC1=CC=CC=C1 CNBGNNVCVSKAQZ-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 9
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000000605 extraction Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000010409 thin film Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000008346 aqueous phase Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 7
- 239000008399 tap water Substances 0.000 claims description 7
- 235000020679 tap water Nutrition 0.000 claims description 7
- 238000005070 sampling Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 4
- 239000012074 organic phase Substances 0.000 claims description 4
- 239000012071 phase Substances 0.000 claims description 4
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 3
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 235000017550 sodium carbonate Nutrition 0.000 claims description 3
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- VYFOAVADNIHPTR-UHFFFAOYSA-N isatoic anhydride Chemical compound NC1=CC=CC=C1CO VYFOAVADNIHPTR-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000006277 sulfonation reaction Methods 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 230000007423 decrease Effects 0.000 abstract 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 230000000007 visual effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 11
- 239000000706 filtrate Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- 235000017060 Arachis glabrata Nutrition 0.000 description 1
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 235000010777 Arachis hypogaea Nutrition 0.000 description 1
- 235000018262 Arachis monticola Nutrition 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of preparation method of bentazone aqua, belong to Chemicals preparing technical field.Its technical problem to be solved is: the preparation method providing a kind of environmental protection more, bentazone aqua that visual appearance is higher.Take isatoic anhydride as raw material, first in dichloroethane solvent system through reactions such as superamide synthesis, sulfonation synthesis, closed loop synthesis, the more faint yellow aqua of bentazone can be obtained at washing, buck extraction, thin-film evaporator after concentrating.Present method decreases the use of soda acid than ordinary method, decreases the use of strongly acid wastewater, and improves the quality of product.
Description
Technical field
The present invention relates to 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, with isatoic anhydride in ethylene dichloride system through superamide synthesis, sulfonation synthesis, closed loop synthesis, washing, alkali extraction, aqueous phase as acidified, centrifugal (sheet frame) discharging, add scale surfactant formulatory aqua.Prior art repeat consumption soda acid, cost is higher; Produce acid waste water, environmental protection pressure is large; Bentazone aqua color is comparatively dark, easily produces a small amount of throw out after placing.
Summary of the invention
The object 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 preparation method for bentazone aqua, described the method, the first step, after adopting closed loop synthesis, organic phase is after washing, and throw gac, constant temperature stirs 30 minutes through Plate Filtration to extracting still; Crossing, with tap water sheet frame to extracting still, having washed; Dry up 30 minutes, unload gac;
Second step, diluted alkaline is prepared: standby 32% Ionic Membrane, to preparing still, adds tap water preparation alkali content to 5% ~ 31%, prepares for extraction;
3rd step, extraction kettle: the diluted alkaline that slow dropping is prepared in advance, dropping temperature controls at 25 ~ 60 DEG C, adjusts material pH value extremely: 3≤pH value < 7;
4th step, after material pH value mixes up, leaves standstill 2 hours, gets upper water phase materials and cross to aqueous phase transfer still through sheet frame;
5th step, content is surveyed in the sampling of transfer still aqueous phase, is concentrated into aqueous phase content according to measuring content by thin-film evaporator;
6th step, the standby still that enters to lower the temperature of concentrated good aqua, drips liquid caustic soda and adjusts pH value=7, throw 1% stablizer, stirs after 1 hour, and slowly unlatching salt solution is cooled to-1 ~ 3 DEG C and crosses to finished product still through sheet frame, excessively completely dries up sheet frame.
7th step, finished product content is surveyed in the sampling of finished product still, and content is qualified takes out 2% liquid surfactant, stirs 30 minutes, pumps into finished product storage tank.
Described stablizer is the one in sodium carbonate, sodium bicarbonate, sodium sulfate, sodium bisulfite and S-WAT.
Middle dropping temperature described in 3rd step controls at 35 ~ 45 DEG C, adjusts material pH value extremely: 5≤pH value < 7.
Diluted alkaline content described in second step controls 14 ~ 18%.
Compared with the prior art, beneficial effect of the present invention is as follows:
Quality product prepared by the inventive method is higher, and production cost is lower, reduces sewage discharge.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is traditional process flow sheet.
Embodiment
A preparation method for bentazone aqua, described the method, the first step, after adopting closed loop synthesis, organic phase is after washing, and throw gac, constant temperature stirs 30 minutes through Plate Filtration to extracting still; Crossing, with tap water sheet frame to extracting still, having washed; Dry up 30 minutes, unload gac;
Second step, diluted alkaline is prepared: standby 32% Ionic Membrane, to preparing still, adds tap water preparation alkali content to 5% ~ 31%, prepares for extraction;
3rd step, extraction kettle: the diluted alkaline that slow dropping is prepared in advance, dropping temperature controls at 25 ~ 60 DEG C, adjusts material pH value extremely: 3≤pH value < 7;
4th step, after material pH value mixes up, leaves standstill 2 hours, gets upper water phase materials and cross to aqueous phase transfer still through sheet frame;
5th step, content is surveyed in the sampling of transfer still aqueous phase, is concentrated into aqueous phase content according to measuring content by thin-film evaporator;
6th step, the standby still that enters to lower the temperature of concentrated good aqua, drips liquid caustic soda and adjusts pH value=7, throw 1% stablizer, stirs after 1 hour, and slowly unlatching salt solution is cooled to-1 ~ 3 DEG C and crosses to finished product still through sheet frame, excessively completely dries up sheet frame.
7th step, finished product content is surveyed in the sampling of finished product still, and content is qualified takes out 2% liquid surfactant, stirs 30 minutes, pumps into finished product storage tank.Described stablizer is the one in sodium carbonate, sodium bicarbonate, sodium sulfate, sodium bisulfite and S-WAT.
Now by 300g organic phase (bentazone content 40%), 2g gac drops in 500ml flask, stirring at normal temperature is suction filtration after 10 minutes, 200ml tap water, getting filtrate drops in flask, prepare 1% ~ 31% diluted alkaline simultaneously, with the diluted alkaline prepared, in 25 ~ 60 DEG C of temperature, slow regulable control filtrate pH value is extremely: 3≤pH value < 7, leave standstill 2 hours, stratified pumping phase, calculate after concentrating and regulate PH=7 with a small amount of liquid caustic soda, throw about 6g stablizer, cool to-1 ~ 4 DEG C, suction filtration is got filtrate and is dropped into about 12g tensio-active agent, obtain clear pale yellow look bentazone aqua, aqua long time without deposit produce are raw.
Claims (4)
1. a preparation method for bentazone aqua, is characterized in that: described the method, the first step, and after adopting closed loop synthesis, organic phase is after washing, and throw gac, constant temperature stirs 30 minutes through Plate Filtration to extracting still; Crossing, with tap water sheet frame to extracting still, having washed; Dry up 30 minutes, unload gac;
Second step, diluted alkaline is prepared: standby 32% Ionic Membrane, to preparing still, adds tap water preparation alkali content to 5% ~ 31%, prepares for extraction;
3rd step, extraction kettle: the diluted alkaline that slow dropping is prepared in advance, dropping temperature controls at 25 ~ 60 DEG C, adjusts material pH value to 5 ~ 7;
4th step, after material pH value mixes up, leaves standstill 2 hours, gets upper water phase materials and cross to aqueous phase transfer still through sheet frame;
5th step, content is surveyed in the sampling of transfer still aqueous phase, is concentrated into aqueous phase content according to measuring content by thin-film evaporator;
6th step, the standby still that enters to lower the temperature of concentrated good aqua, drips liquid caustic soda and adjusts pH value=7, throw 1% stablizer, stirs after 1 hour, and slowly unlatching salt solution is cooled to-1 ~ 3 DEG C and crosses to finished product still through sheet frame, excessively completely dries up sheet frame;
7th step, finished product content is surveyed in the sampling of finished product still, and content is qualified takes out 2% liquid surfactant, stirs 30 minutes, pumps 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 the one in sodium carbonate, sodium bicarbonate, sodium sulfate, sodium bisulfite and S-WAT.
3. the preparation method of a kind of bentazone aqua according to claim 1, is characterized in that: the middle dropping temperature described in the 3rd step controls at 35 ~ 45 DEG C, pH value to 5 ~ 7.
4. the preparation method of a kind of bentazone aqua according to claim 1, is characterized in that: the diluted alkaline content described in second step controls 14 ~ 18%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210476991.1A CN102924405B (en) | 2012-11-21 | 2012-11-21 | A kind of preparation method of bentazone aqua |
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| Application Number | Priority Date | Filing Date | Title |
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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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| CN102924405A CN102924405A (en) | 2013-02-13 |
| CN102924405B true CN102924405B (en) | 2016-01-20 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106543101B (en) * | 2016-11-08 | 2018-10-23 | 南京大学 | A kind of decoloration of Bentazon and method of purification |
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 |
| 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 |
-
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 |
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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. |