CN101298441B - Method for reclaiming 1,2- benzoisothiazoline-3-ketone from mother liquor - Google Patents
Method for reclaiming 1,2- benzoisothiazoline-3-ketone from mother liquor Download PDFInfo
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- CN101298441B CN101298441B CN2008101229154A CN200810122915A CN101298441B CN 101298441 B CN101298441 B CN 101298441B CN 2008101229154 A CN2008101229154 A CN 2008101229154A CN 200810122915 A CN200810122915 A CN 200810122915A CN 101298441 B CN101298441 B CN 101298441B
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- ketone
- mother liquor
- bit
- benzisothiazole
- organic solvent
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Abstract
The invention relates to a method for recovering BIT from a leaching mother liquor of 1, 2-benzoisothiazoline-3-ketone (BIT); the method includes the following steps: adding acid or alkali into the BIT leaching mother liquor to adjust the pH between 1.5 and 5, filtering and obtaining clear mother liquor; moreover, adding macropore absorption resin into an absorption column; after conventional pretreatment, absorbing the BIT in the clear mother liquor of the BIT by the absorption resin under the conditions of controlling the temperature of 20 to 60 DEG C and flow speed of 8 to 20BV/h; carrying out desorption by using sig water or an organic solvent as the desorption liquor and controlling the temperature of 25 to 60 DEG C as well as the flow speed of 2 to 3 BV/h; recovering the BIT sig water by desorption or separating the BIT by the desorption of the organic solvent through distillation and recovering the organic solvent. The recovering rate of the BIT is more than 90 percent by adopting the method of the invention; the absorption effluent is easier to control than the original mother liquor. The method of the invention is simple and easy to carry out; the resin can be repeatedly used and the cost is low.
Description
Technical field
The present invention relates to 1, the recovery of 2-benzisothiazole-3-ketone (BIT) specifically, is the method that from mother liquor, reclaims BIT with resin.
Background technology
In BIT bullion and the acidified mother liquor, contain the BIT of the 1-1.5 ‰ that has an appointment, after the recycling of the BIT in the mother liquor, carry out wastewater treatment again, can reduce the wasting of resources on the one hand, obtain economic benefit, also can reduce the difficulty and the cost of wastewater treatment on the other hand.Do not see as yet at present the report that from the leaching mother liquor, reclaims BIT is arranged.
Summary of the invention
The purpose of this invention is to provide a kind of method that from BIT leaching mother liquor, reclaims BIT.
The objective of the invention is to realize through following technical scheme:
A kind ofly from mother liquor, reclaim 1, the method for 2-benzisothiazole-3-ketone, it is made up of following steps:
Steps A: will contain 1, the mother liquor of 2-benzisothiazole-3-ketone adds acid or alkali and regulates pH to 1.5-5, filters, and obtains clarified mother liquor;
Step B: in adsorption column, pack into strong polarity or nonpolar macroporous adsorption resin; After conventional pre-treatment, the steps A gained contained 1, the clarified mother liquor of 2-benzisothiazole-3-ketone; It is under the 8-20BV/h condition with flow velocity that controlled temperature is 20-60 ℃; Through polymeric adsorbent, 1, the 2-benzisothiazole-3-ketone is adsorbed;
Step C: with the sig water is elutriant, and controlled temperature is 25-60 ℃, and flow velocity is 2-3BV/h, carries out desorption, obtains 1, and the alkaline solution of 2-benzisothiazole-3-ketone reclaims; Or be elutriant with the organic solvent, be 2-3BV/h at 40-60 ℃, flow velocity, carry out desorption;
Step D: as if being elutriant with the organic solvent, then the organic solvent desorption liquid with step C gained goes out BIT through fractionation by distillation, reclaims organic solvent.
Above-mentioned recovery 1, the method for 2-benzisothiazole-3-ketone, the dilute alkaline soln described in the step C is the 2%-5% sodium hydroxide solution.
Above-mentioned recovery 1, the method for 2-benzisothiazole-3-ketone, the organic solvent described in the step C is industrial alcohol or acetone.
Adopt the inventive method, the recovery of BIT is＞95%, and absorption effluent is easier to administer than original nut liquid.The inventive method is simple, and resin can be reused, and cost is low.
Embodiment
Below through embodiment the present invention is made further detailed description.
Embodiment 1
With BIT leaching mother liquor 500ml, to filter and obtain clarified mother liquor, BIT concentration is about 1000-1500mg/L, pH value of solution=1.5; Get strong polar macroporous adsorption resin (on the south the become civilized NKA-2 type of plant produced be example, NKA-2 is vinylbenzene-diethylbenzene structure) 10ml and adorn post, (pre-treatment: use industrial Ethanol Treatment down at 60 ℃, wash down for 25 ℃, flow velocity is 2BV/h.) above-mentioned clarified mother liquor is passed through strong polar macroporous adsorbent resin column, adsorption temp is 60 ℃, flow velocity 8BV/h, absorption effluent BIT concentration is 56mg/L, the recovery about 95.5%.Adsorbing saturated back use industrial alcohol is 60 ℃ in temperature, and flow velocity is to carry out desorption under the 2BV/h condition, obtains the BIT ethanolic soln, and fractionation by distillation obtains BIT and ethanol, and desorption rate is 99%.
Embodiment 2
With BIT leaching mother liquor 500ml, to filter and obtain clarified mother liquor, BIT concentration is about 1000-1500mg/L, pH value of solution=5; Get nonpolar macroporous adsorption resin (on the south become civilized the H103 type of plant produced be example) 10ml and adorn post, (pre-treatment: 60 ℃ handle with 3% sodium hydroxide solution down and washing to neutrality, flow velocity is 2BV/h.) above-mentioned clarified mother liquor is passed through nonpolarity macroporous adsorptive resins chromatographic column, adsorption temp is 25 ℃, flow velocity 16BV/h, absorption effluent BIT concentration is 42mg/L, the recovery about 96.6%.Adsorbing saturated back use 3% sodium hydroxide solution is 60 ℃ in temperature, and flow velocity is to carry out desorption under the 2BV/h condition, obtains the BIT alkaline solution, and desorption rate is 98.6%.
Embodiment 3
With BIT leaching mother liquor 500ml, to filter and obtain clarified mother liquor, BIT concentration is about 1000-1500mg/L, pH value of solution=2.6; Get strong polar macroporous adsorption resin (on the south the become civilized NKA-2 type of plant produced be example, NKA-2 is vinylbenzene-diethylbenzene structure) 10ml and adorn post, (pre-treatment: 60 ℃ handle with 3% sodium hydroxide solution down and washing to neutrality, flow velocity is 2BV/h.) above-mentioned clarified mother liquor is passed through strong polar macroporous adsorbent resin column, adsorption temp is 20 ℃, flow velocity 20BV/h, absorption effluent BIT concentration is 38mg/L, the recovery about 97%.Adsorbing saturated back use acetone is 40 ℃ in temperature, and flow velocity is to carry out desorption under the 2BV/h condition, obtains the BIT acetone soln, and fractionation by distillation obtains BIT and acetone, and desorption rate is 97.4%.
Embodiment 4
With BIT leaching mother liquor 500ml, to filter and obtain clarified mother liquor, BIT concentration is about 1000-1500mg/L, pH value of solution=5; Get nonpolar macroporous adsorption resin (on the south become civilized the H103 type of plant produced be example) 10ml and adorn post, (pre-treatment: 60 ℃ handle with 3% sodium hydroxide solution down and washing to neutrality, flow velocity is 2BV/h.) above-mentioned clarified mother liquor is passed through nonpolarity macroporous adsorptive resins chromatographic column, adsorption temp is 20 ℃, flow velocity 16BV/h, absorption effluent BIT concentration is 42mg/L, the recovery about 96.6%.Adsorbing saturated back use 3% sodium hydroxide solution is 25 ℃ in temperature, and flow velocity is to carry out desorption under the 3BV/h condition, obtains the BIT alkaline solution, and desorption rate is 98.6%.
Claims (4)
1. one kind is reclaimed 1 from mother liquor, and the method for 2-benzisothiazole-3-ketone is characterized in that it is made up of following steps:
Steps A: will contain 1, the mother liquor of 2-benzisothiazole-3-ketone adds acid or alkali and regulates pH to 1.5-5, filters, and obtains clarified mother liquor;
Step B: in adsorption column, pack into strong polarity or nonpolar macroporous adsorption resin; After conventional pre-treatment, the steps A gained contained 1, the clarified mother liquor of 2-benzisothiazole-3-ketone; It is under the 8-20BV/h condition with flow velocity that controlled temperature is 20-60 ℃; Through polymeric adsorbent, 1, the 2-benzisothiazole-3-ketone is adsorbed;
Step C: with the sig water is elutriant, and controlled temperature is 25-60 ℃, and flow velocity is 2-3BV/h, carries out desorption, obtains 1, and the alkaline solution of 2-benzisothiazole-3-ketone reclaims.
2. recovery 1 according to claim 1, the method for 2-benzisothiazole-3-ketone is characterized in that strong polarity described in the step B or nonpolar macroporous adsorption resin are NKA-2 type resin or H103 type resin.
3. recovery 1 according to claim 1, the method for 2-benzisothiazole-3-ketone is characterized in that the sig water described in the step C is the 2%-5% sodium hydroxide solution.
4. recovery 1 according to claim 1, the method for 2-benzisothiazole-3-ketone is characterized in that steps A is identical with step B, carries out following step C and step D then:
Step C: the elutriant sig water substitute with organic solvent ethanol or acetone, when adopting organic solvent ethanol or acetone as elutriant, eluting temperature is 40-60 ℃, flow velocity is 2-3BV/h,
Step D: the organic solvent desorption liquid of step C gained is gone out 1 through fractionation by distillation, and the 2-benzisothiazole-3-ketone reclaims organic solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101229154A CN101298441B (en) | 2008-06-20 | 2008-06-20 | Method for reclaiming 1,2- benzoisothiazoline-3-ketone from mother liquor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101229154A CN101298441B (en) | 2008-06-20 | 2008-06-20 | Method for reclaiming 1,2- benzoisothiazoline-3-ketone from mother liquor |
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| Publication Number | Publication Date |
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| CN101298441A CN101298441A (en) | 2008-11-05 |
| CN101298441B true CN101298441B (en) | 2012-07-25 |
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| CN2008101229154A Expired - Fee Related CN101298441B (en) | 2008-06-20 | 2008-06-20 | Method for reclaiming 1,2- benzoisothiazoline-3-ketone from mother liquor |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102726421A (en) * | 2011-03-31 | 2012-10-17 | 住友精化株式会社 | Method for producing 1,2-benzisothiazol-3-one waterborne compound |
| CN107686468B (en) * | 2017-09-30 | 2020-06-19 | 连云港市三联化工有限公司 | Method for recovering 1, 2-benzisothiazolin-3-ketone contained in solvent |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143452A (en) * | 1995-07-21 | 1997-02-26 | 希尔斯美国有限公司 | Liquid formulations of 1,2-benzisothiazolin-3-one |
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2008
- 2008-06-20 CN CN2008101229154A patent/CN101298441B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143452A (en) * | 1995-07-21 | 1997-02-26 | 希尔斯美国有限公司 | Liquid formulations of 1,2-benzisothiazolin-3-one |
Non-Patent Citations (2)
| Title |
|---|
| 倪越等.新工业防霉杀菌剂1 2- 苯并异噻唑啉- 3- 酮的研制.精细与专用化学品12 20.2004 |
| 倪越等.新工业防霉杀菌剂1,2- 苯并异噻唑啉- 3- 酮的研制.精细与专用化学品12 20.2004,12(20),21-22. * |
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Application publication date: 20081105 Assignee: Dafeng Yuelong Chemical Co., Ltd. Assignor: Nanjing University Contract record no.: 2015320010078 Denomination of invention: Method for reclaiming 1,2- benzoisothiazoline-3-ketone from mother liquor Granted publication date: 20120725 License type: Exclusive License Record date: 20150528 |
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