CN115353496A - Continuous production process of 1, 2-benzisothiazolin-3-one - Google Patents
Continuous production process of 1, 2-benzisothiazolin-3-one Download PDFInfo
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- CN115353496A CN115353496A CN202210697378.6A CN202210697378A CN115353496A CN 115353496 A CN115353496 A CN 115353496A CN 202210697378 A CN202210697378 A CN 202210697378A CN 115353496 A CN115353496 A CN 115353496A
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- benzisothiazolin
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- DMSMPAJRVJJAGA-UHFFFAOYSA-N benzo[d]isothiazol-3-one Chemical compound C1=CC=C2C(=O)NSC2=C1 DMSMPAJRVJJAGA-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000010924 continuous production Methods 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 238000000605 extraction Methods 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 24
- 239000012074 organic phase Substances 0.000 claims abstract description 24
- 239000003960 organic solvent Substances 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims description 20
- 230000008020 evaporation Effects 0.000 claims description 17
- KXDAEFPNCMNJSK-UHFFFAOYSA-N Benzamide Chemical compound NC(=O)C1=CC=CC=C1 KXDAEFPNCMNJSK-UHFFFAOYSA-N 0.000 claims description 12
- 229920000858 Cyclodextrin Polymers 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 9
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000012295 chemical reaction liquid Substances 0.000 claims description 6
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 6
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 6
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LBEMXJWGHIEXRA-UHFFFAOYSA-N 2-[(2-carboxyphenyl)disulfanyl]benzoic acid Chemical compound OC(=O)C1=CC=CC=C1SSC1=CC=CC=C1C(O)=O LBEMXJWGHIEXRA-UHFFFAOYSA-N 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 5
- 229920001450 Alpha-Cyclodextrin Polymers 0.000 claims description 3
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 3
- 229910021595 Copper(I) iodide Inorganic materials 0.000 claims description 3
- 239000001116 FEMA 4028 Substances 0.000 claims description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- MCDLETWIOVSGJT-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O.CC(O)=O MCDLETWIOVSGJT-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- HFHDHCJBZVLPGP-RWMJIURBSA-N alpha-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO HFHDHCJBZVLPGP-RWMJIURBSA-N 0.000 claims description 3
- 229940043377 alpha-cyclodextrin Drugs 0.000 claims description 3
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 3
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 3
- 229960004853 betadex Drugs 0.000 claims description 3
- RFKZUAOAYVHBOY-UHFFFAOYSA-M copper(1+);acetate Chemical compound [Cu+].CC([O-])=O RFKZUAOAYVHBOY-UHFFFAOYSA-M 0.000 claims description 3
- LSXDOTMGLUJQCM-UHFFFAOYSA-M copper(i) iodide Chemical compound I[Cu] LSXDOTMGLUJQCM-UHFFFAOYSA-M 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 229960002089 ferrous chloride Drugs 0.000 claims description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 3
- 239000011790 ferrous sulphate Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- GDSRMADSINPKSL-HSEONFRVSA-N gamma-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO GDSRMADSINPKSL-HSEONFRVSA-N 0.000 claims description 3
- 229940080345 gamma-cyclodextrin Drugs 0.000 claims description 3
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 3
- 230000001502 supplementing effect Effects 0.000 claims description 2
- 239000007800 oxidant agent Substances 0.000 abstract description 4
- 230000001590 oxidative effect Effects 0.000 abstract description 4
- 229960001701 chloroform Drugs 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 230000002335 preservative effect Effects 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D275/00—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings
- C07D275/04—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings condensed with carbocyclic rings or ring systems
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Thiazole And Isothizaole Compounds (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a continuous production process of 1, 2-benzisothiazolin-3-one, which utilizes oxygen as an oxidant to improve the overall reaction efficiency and the production efficiency, can thoroughly extract an organic phase in a reaction solution during extraction, prevents the organic phase contained in an aqueous solution from being conveyed into a reaction kettle together, and can recover the 1, 2-benzisothiazolin-3-one in the aqueous solution and an organic solvent when the production is not needed.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a continuous production process of 1, 2-benzisothiazolin-3-one.
Background
1, 2-benzisothiazolin-3-one (BIT) is one of the most important novel industrial sterilization, mildew prevention and preservative at present. The 1, 2-benzisothiazolin-3-one has the outstanding function of inhibiting the breeding of microorganisms such as fungi, mould, bacteria, algae and the like in an organic medium, and is considered to be one of green, environment-friendly, sterilization, mildew prevention and preservative with slight toxicity, safety and no harm. The method for synthesizing 1, 2-benzisothiazolin-3-one of patent No. CN201510203295.7 utilizes air as an oxidant, although the cost is low, the reaction speed is slow, the production efficiency is influenced, and in the method, an organic phase in a reaction solution cannot be completely extracted during extraction, so that a lot of aqueous solution containing the organic phase is conveyed into a reaction kettle together with the organic phase, when the production is not needed, the organic phase is wasted, the aqueous solution in the method is directly returned into the reaction kettle, the aqueous solution contains a large amount of organic solvent, the organic solvent cannot be recycled into the extraction kettle, the extraction kettle needs to continuously supplement the organic solvent, when the organic solvent is removed by vacuum evaporation, the organic solvent cannot be condensed and recycled, the resource loss is caused, the reaction cost is increased, and when the production is not performed, the organic solvent and the 1, 2-benzisothiazolin-3-one residue in the aqueous solution cannot be removed and recycled; therefore, the continuous production process of the 1, 2-benzisothiazolin-3-one is provided.
Disclosure of Invention
The invention aims to solve the problems in the prior art by providing a continuous production process of 1, 2-benzisothiazolin-3-one.
In order to achieve the purpose, the invention provides the following technical scheme: a continuous production process of 1, 2-benzisothiazolin-3-ketone comprises the following specific steps:
s1: adding cyclodextrin, benzamide and water into a reaction kettle, heating and uniformly stirring, continuously adding a catalyst and sodium thiosulfate into the reaction kettle, stirring to be uniform, introducing oxygen for reaction, detecting by adopting HPLC (high performance liquid chromatography), and stopping introducing oxygen and heating when the product conversion rate reaches over 99% to obtain a reaction solution;
s2: introducing the reaction liquid into an extraction kettle, extracting the reaction liquid by using an organic solvent, separating an organic phase and a mixed liquid, then introducing the mixed liquid into the extraction kettle again, and extracting the mixed liquid by using the organic solvent until the organic phase is not extracted, wherein the mixed liquid becomes an aqueous solution;
s3: putting the organic phase obtained by multiple extractions into an evaporation tank, and evaporating the organic solvent on the organic phase to obtain 1, 2-benzisothiazolin-3-one;
s4: if the production of the 1, 2-benzisothiazolin-3-one is finished, mixing the aqueous solution obtained by extraction with the organic solution evaporated and condensed by an evaporation tank, and then changing the residual 1, 2-benzisothiazolin-3-one in the organic solution and the aqueous solution into dithiodibenzoic acid by adding alkali for neutralization, distillation and filtration;
s5: if the production is continued, the organic solution evaporated and condensed by the evaporation tank is conveyed into the extraction kettle, the organic solution obtained by rectifying and extracting the aqueous solution is conveyed into the extraction kettle, the catalyst and the water are conveyed into the reaction kettle, and the continuous production can be realized only by adding the benzamide and the sodium thiosulfate.
As a preferable technical scheme of the invention, the heating temperature in the S1 is 80-120 ℃, the stirring time is 1-1.5h, and oxygen is supplied by an oxygen supplementing machine.
In a preferred embodiment of the present invention, in S2, when the organic phase cannot be precipitated at the bottom of the extraction vessel, the introduction of the organic solvent into the extraction vessel is stopped.
As a preferable technical scheme of the invention, the evaporation temperature of the evaporation tank in S3 is 90-110 ℃, and the heating temperature of the evaporation tank in S4 is 60-90 ℃ when the 1, 2-benzisothiazolin-3-one remained in the organic solution and the aqueous solution is changed into dithiodibenzoic acid.
As a preferable technical solution of the present invention, the cyclodextrin includes α -cyclodextrin, β -cyclodextrin, γ -cyclodextrin and cyclodextrin derivatives.
As a preferable technical scheme of the invention, the catalyst comprises ferrous chloride, ferrous sulfate, ferrous acetate, ferrous nitrate, cuprous iodide, cuprous acetate and palladium dichloride.
As a preferred technical scheme of the invention, the organic solvent comprises ethyl acetate, butyl acetate, dichloromethane and trichloromethane.
The invention has the beneficial effects that: the invention uses oxygen as oxidant, improves the whole reaction efficiency and production efficiency, and the process can extract the organic phase in the reaction solution thoroughly during extraction, thereby avoiding the organic phase in the aqueous solution from being conveyed into a reaction kettle together, and recovering the 1, 2-benzisothiazolin-3-one in the aqueous solution and the organic solvent when the production is not needed.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention more readily understood by those skilled in the art, and thus will more clearly and distinctly define the scope of the invention.
Referring to fig. 1, the present invention provides a technical solution: a continuous production process of 1, 2-benzisothiazolin-3-ketone comprises the following specific steps:
s1: adding cyclodextrin, benzamide and water into a reaction kettle, heating, uniformly stirring, continuously adding a catalyst and sodium thiosulfate into the reaction kettle, stirring uniformly, introducing oxygen for reaction, detecting by using HPLC (high performance liquid chromatography), stopping introducing oxygen and heating when the product conversion rate reaches over 99 percent to obtain a reaction solution, wherein the heating temperature is 80-120 ℃, the stirring time is 1-1.5 hours, and the oxygen is supplied by using an oxygenator;
s2: introducing the reaction liquid into an extraction kettle, extracting the reaction liquid by using an organic solvent, separating an organic phase and a mixed liquid, then introducing the mixed liquid into the extraction kettle again, and extracting the mixed liquid by using the organic solvent until the organic phase cannot be extracted, wherein the mixed liquid becomes an aqueous solution;
s3: putting the organic phase obtained by multiple extractions into an evaporation tank, and evaporating the organic solvent on the organic phase to obtain the 1, 2-benzisothiazolin-3-one, wherein the evaporation temperature of the evaporation tank is 90-110 ℃;
s4: if the production of the 1, 2-benzisothiazolin-3-one is finished, mixing the aqueous solution obtained by extraction with the organic solution evaporated and condensed by an evaporation tank, and then adding alkali for neutralization, distillation and filtration to change the residual 1, 2-benzisothiazolin-3-one in the organic solution and the aqueous solution into dithiodibenzoic acid;
s5: if the production is continued, the organic solution evaporated and condensed by the evaporation tank is conveyed into the extraction kettle, the organic solution obtained by rectifying and extracting the aqueous solution is conveyed into the extraction kettle, the catalyst and the water are conveyed into the reaction kettle, and the continuous production can be realized only by adding the benzamide and the sodium thiosulfate.
The cyclodextrin includes alpha-cyclodextrin, beta-cyclodextrin, gamma-cyclodextrin and cyclodextrin derivatives.
The catalyst comprises ferrous chloride, ferrous sulfate, ferrous acetate, ferrous nitrate, cuprous iodide, cuprous acetate and palladium dichloride.
Organic solvents include ethyl acetate, butyl acetate, dichloromethane and chloroform.
The invention uses oxygen as oxidant, improves the whole reaction efficiency and production efficiency, and the process can extract the organic phase in the reaction solution thoroughly during extraction, thereby avoiding the organic phase in the aqueous solution from being conveyed into a reaction kettle together, and recovering the 1, 2-benzisothiazolin-3-one in the aqueous solution and the organic solvent when the production is not needed.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention.
Claims (7)
1. A continuous production process of 1, 2-benzisothiazolin-3-one is characterized by comprising the following steps: the method comprises the following specific steps:
s1: adding cyclodextrin, benzamide and water into a reaction kettle, heating and uniformly stirring, continuously adding a catalyst and sodium thiosulfate into the reaction kettle, stirring to be uniform, introducing oxygen for reaction, detecting by adopting HPLC (high performance liquid chromatography), and stopping introducing oxygen and heating when the product conversion rate reaches over 99% to obtain a reaction solution;
s2: introducing the reaction liquid into an extraction kettle, extracting the reaction liquid by using an organic solvent, separating an organic phase and a mixed liquid, then introducing the mixed liquid into the extraction kettle again, and extracting the mixed liquid by using the organic solvent until the organic phase is not extracted, wherein the mixed liquid becomes an aqueous solution;
s3: putting the organic phase obtained by multiple extractions into an evaporation tank, and evaporating the organic solvent on the organic phase to obtain 1, 2-benzisothiazolin-3-one;
s4: if the production of the 1, 2-benzisothiazolin-3-one is finished, mixing the aqueous solution obtained by extraction with the organic solution evaporated and condensed by an evaporation tank, and then adding alkali for neutralization, distillation and filtration to change the residual 1, 2-benzisothiazolin-3-one in the organic solution and the aqueous solution into dithiodibenzoic acid;
s5: if the production is continued, the organic solution evaporated and condensed by the evaporation tank is conveyed into the extraction kettle, the organic solution obtained by rectifying and extracting the aqueous solution is conveyed into the extraction kettle, the catalyst and the water are conveyed into the reaction kettle, and the continuous production can be realized only by adding the benzamide and the sodium thiosulfate.
2. The continuous process of claim 1, 2-benzisothiazolin-3-one, wherein the process comprises the steps of: the heating temperature in the S1 is 80-120 ℃, the stirring time is 1-1.5h, and oxygen is supplied by an oxygen supplementing machine.
3. The continuous production process of 1, 2-benzisothiazolin-3-one according to claim 1, comprising the following steps: and (3) stopping adding the organic solvent into the extraction kettle when the organic phase cannot be separated out from the bottom of the extraction kettle in the S2.
4. The continuous production process of 1, 2-benzisothiazolin-3-one according to claim 1, comprising the following steps: the evaporation temperature of the evaporation tank in the S3 is 90-110 ℃, and the heating temperature of the evaporation tank in the S4 is 60-90 ℃ when the 1, 2-benzisothiazolin-3-one remained in the organic solution and the aqueous solution is changed into the dithiodibenzoic acid.
5. The continuous process of claim 1, 2-benzisothiazolin-3-one, wherein the process comprises the steps of: the cyclodextrin includes alpha-cyclodextrin, beta-cyclodextrin, gamma-cyclodextrin and cyclodextrin derivatives.
6. The continuous production process of 1, 2-benzisothiazolin-3-one according to claim 1, comprising the following steps: the catalyst comprises ferrous chloride, ferrous sulfate, ferrous acetate, ferrous nitrate, cuprous iodide, cuprous acetate and palladium dichloride.
7. The continuous process of claim 1, 2-benzisothiazolin-3-one, wherein the process comprises the steps of: the organic solvent includes ethyl acetate, butyl acetate, dichloromethane and chloroform.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB758076A (en) * | 1954-10-04 | 1956-09-26 | Ici Ltd | An improvement in or relating to the manufacture of a pyridine homologue |
| KR20000018793A (en) * | 1998-09-04 | 2000-04-06 | 조민호 | Method for manufacturing 1,2-benzisothiazolones-3-one |
| US20130150239A1 (en) * | 2010-01-07 | 2013-06-13 | Raman Premachandran | Aqueous-miscible or aqueous-dispersible, voc-free biocidal compositions for the enhanced inhibition of gram-negative bacterial strains, and method of preparing the same |
| CN104817517A (en) * | 2015-04-24 | 2015-08-05 | 大丰跃龙化学有限公司 | Synthetic method of 1, 2-benzisothiazolin-3-one |
| CN110467584A (en) * | 2019-09-09 | 2019-11-19 | 大连百傲化学股份有限公司 | A kind of continuous production method of 1,2- benzisothiazole-3-ketone |
| CN110483438A (en) * | 2019-09-09 | 2019-11-22 | 大连百傲化学股份有限公司 | A kind of duct type continuous production method of 3- iso thiazoline ketone compound |
| CN113200937A (en) * | 2021-05-14 | 2021-08-03 | 郑州大学 | Method for preparing 1, 2-benzisothiazolin-3-one by catalytic oxidation |
-
2022
- 2022-06-20 CN CN202210697378.6A patent/CN115353496A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB758076A (en) * | 1954-10-04 | 1956-09-26 | Ici Ltd | An improvement in or relating to the manufacture of a pyridine homologue |
| KR20000018793A (en) * | 1998-09-04 | 2000-04-06 | 조민호 | Method for manufacturing 1,2-benzisothiazolones-3-one |
| US20130150239A1 (en) * | 2010-01-07 | 2013-06-13 | Raman Premachandran | Aqueous-miscible or aqueous-dispersible, voc-free biocidal compositions for the enhanced inhibition of gram-negative bacterial strains, and method of preparing the same |
| CN104817517A (en) * | 2015-04-24 | 2015-08-05 | 大丰跃龙化学有限公司 | Synthetic method of 1, 2-benzisothiazolin-3-one |
| CN110467584A (en) * | 2019-09-09 | 2019-11-19 | 大连百傲化学股份有限公司 | A kind of continuous production method of 1,2- benzisothiazole-3-ketone |
| CN110483438A (en) * | 2019-09-09 | 2019-11-22 | 大连百傲化学股份有限公司 | A kind of duct type continuous production method of 3- iso thiazoline ketone compound |
| CN113200937A (en) * | 2021-05-14 | 2021-08-03 | 郑州大学 | Method for preparing 1, 2-benzisothiazolin-3-one by catalytic oxidation |
Non-Patent Citations (4)
| Title |
|---|
| 张正儒: "杀菌防霉剂1, 2-苯并异噻唑啉-3-酮的合成", 东西南北:教育, vol. 11, no. 26, pages 1 - 4 * |
| 王向辉，等: "异噻唑啉酮类衍生物的合成及应用研究进展", 海南大学学报(自然科学版), vol. 12, no. 04, pages 147 - 151 * |
| 石森昊，等: "聚苯硫醚生产用N-甲基吡咯烷酮溶剂萃取回收研究", 四川化工, vol. 08, no. 02, pages 122 - 129 * |
| 童国通，等: "抑菌剂1, 2-苯并异噻唑啉-3-酮(BIT)的合成研究", 化学世界, vol. 12, no. 04, pages 1 - 5 * |
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