CN204779430U - Primary raw material neighbour p toluene sulfonyl chloride's of neighbour / para toluene sulfonamide purification equipment - Google Patents
Primary raw material neighbour p toluene sulfonyl chloride's of neighbour / para toluene sulfonamide purification equipment Download PDFInfo
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- CN204779430U CN204779430U CN201520349333.5U CN201520349333U CN204779430U CN 204779430 U CN204779430 U CN 204779430U CN 201520349333 U CN201520349333 U CN 201520349333U CN 204779430 U CN204779430 U CN 204779430U
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- neighbour
- tosyl chloride
- film evaporator
- purification
- receiving tank
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Abstract
The utility model discloses a neighbour p toluene sulfonyl chloride's purification equipment, including the washing that connects gradually dissolve that cauldron, film evaporator, height boil that the thing is received jar, stills and purification thing receive jar, the stills top is equipped with the distillation column, the distillation column passes through condenser and purification thing to be received and jar is connected, the film evaporator top is connected with solvent naphtha recovery jar. According to the characteristic of accessory substance, this purification method and purification equipment adopt the differential distillation tower to carry out the distilling mode of negative pressure and purify, obtain the higher adjacent p toluene sulfonyl chloride of purity, and content can reach 98-99%, and the range of application increases greatly.
Description
Technical field
The utility model relates to a kind of equipment for purifying of raw material neighbour/Tosyl chloride of neighbour/para toluene sulfonamide.
Background technology
Neighbour/Tosyl chloride is the main raw material of neighbour/para toluene sulfonamide, the main production of current industrial production neighbour/Tosyl chloride is by toluene and chlorsulfonic acid sulfonation under cryogenic, neighbour/Tosyl chloride and sulfuric acid mixture is obtained again with after the excessive chlorsulfonic acid of water decomposition, Tosyl chloride comprising about 70% and about 30% o-toluenesulfonyl chloride, after centrifugation about 50% Tosyl chloride, containing neighbour/Tosyl chloride crude product in by product sulfuric acid in centrifuge mother liquor, general 20% Tosyl chloride and 30% o-toluenesulfonyl chloride, mix the neighbour/Tosyl chloride into about 50%.The neighbour that this production technique obtains/Tosyl chloride crude product crude product water content is higher, free acid >=1%, and content can only reach 92 ~ 94%, can not reach the needs of downstream application far away.
In addition cause the major cause that neighbour/tolysulfonyl cl content is lower to be in sulfonation process, product SULPHURYL CHLORIDE can be carried out friedel-crafts reaction with toluene and be produced by product ditolyl sulfone, and this by product can be dissolved in product neighbour/Tosyl chloride.
Utility model content
For solving the problems of the technologies described above, the utility model provides a kind of equipment for purifying of neighbour/Tosyl chloride effectively can reduce moisture content in neighbour/Tosyl chloride, free acid and by product, improves purity.
The utility model is by the following technical solutions: a kind of equipment for purifying of neighbour/Tosyl chloride, comprise the washing dissolution kettle, thin-film evaporator, high boiling material receiving tank, still kettle and the purification thing receiving tank that connect successively, described still kettle top is provided with distillation tower, described distillation tower is connected with purification thing receiving tank by condenser, and described thin-film evaporator top is connected with solvent oil withdrawing can.
Described purification thing receiving tank is the thin-film evaporator that top is connected to vacuum pump.To be purified by aforesaid device the method for neighbour/Tosyl chloride, comprise the following steps, first with solvent oil, the Tosyl chloride crude product in washing dissolution kettle is fully dissolved rear leaving standstill, lower aqueous layer is separated, removing free acid, solvent oil withdrawing can is recycled to through condensation after being evaporated by solvent oil under negative pressure state by thin-film evaporator again, neighbour/Tosyl chloride proceeds to high boiling material receiving tank, again high boiling material neighbour/Tosyl chloride is proceeded in still kettle, steamed by distillation tower under negative pressure state, after condenser condenses, be placed in purification thing receiving tank, and by product ditolyl sulfone is because boiling point is left in still kettle far above neighbour/Tosyl chloride.
Hydrogenchloride and tosic acid is obtained because neighbour/Tosyl chloride at high temperature can be hydrolyzed with water.Therefore use 120# solvent oil neighbour/Tosyl chloride crude product fully to be dissolved rear leaving standstill, lower aqueous layer be separated, finally intercept cut according to distillation tower top temperature and obtain the higher neighbour/Tosyl chloride of purity, content can reach 98 ~ 99%.
The utility model has the advantages that: according to the characteristic of by product, the mode that this method of purification and equipment for purifying adopt simple distillation tower to carry out vacuum distillation is purified, obtain neighbour/Tosyl chloride that purity is higher, content can reach 98 ~ 99%, and range of application increases greatly.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model;
Wherein, 1, washing dissolution kettle, 2, thin-film evaporator, 3, high boiling material receiving tank, 4, still kettle, 5, purification thing receiving tank, 6, distillation tower, 7, condenser, 8, solvent oil withdrawing can, 9, vacuum pump.
Embodiment
Below in conjunction with the drawings and specific embodiments, the technical solution of the utility model is further described, but protection domain of the present utility model is not limited thereto.
As shown in Figure 1, a kind of equipment for purifying of neighbour/Tosyl chloride, comprise the washing dissolution kettle 1, thin-film evaporator 2, high boiling material receiving tank 3, still kettle 4 and the purification thing receiving tank 5 that connect successively, still kettle 4 top is provided with distillation tower 6, distillation tower 6 is connected with purification thing receiving tank 5 by condenser 7, and thin-film evaporator 2 top is connected with solvent oil withdrawing can 8.Purification thing receiving tank 5 is preferably the thin-film evaporator that top is connected to vacuum pump 9.
The method of this equipment purification neighbour/Tosyl chloride is used to be: to wash in dissolution kettle at 3000L and add 120# solvent oil 1500kg, again 1500kg neighbour/Tosyl chloride crude product is added in washing dissolution kettle, stirring 30min makes material fully dissolve, leave standstill and lower aqueous layer was divided in 30 minutes, then leave standstill point sub-cloud washing water after adding 100kg water agitator treating.Again material is proceeded to thin-film evaporator at 90 ~ 100 DEG C, carrying out precipitation treatment is carried out under vacuum tightness-0.04 ~ 0.06MPa condition, 120# solvent oil is recycled to solvent oil withdrawing can through condensation after evaporating under high temperature condition of negative pressure, high boiling material neighbour/Tosyl chloride puts into high boiling material receiving tank, and then high boiling material is proceeded in 2000L still kettle, by diameter 400mm, the distillation tower of height 6m, under negative pressure 15mmHg condition, by temperature to 145 ~ 150 DEG C in still kettle, neighbour/Tosyl chloride 1430kg is obtained lower than intercepting cut when 130 DEG C in tower top temperature, content 98.76%, moisture content 0.03%, free acid 0.19%.
Claims (2)
1. the equipment for purifying of the main raw material neighbour/Tosyl chloride of neighbour/para toluene sulfonamide, it is characterized in that, comprise the washing dissolution kettle, thin-film evaporator, high boiling material receiving tank, still kettle and the purification thing receiving tank that connect successively, described still kettle top is provided with distillation tower, described distillation tower is connected with purification thing receiving tank by condenser, and described thin-film evaporator top is connected with solvent oil withdrawing can.
2. the equipment for purifying of the main raw material neighbour/Tosyl chloride of a kind of neighbour/para toluene sulfonamide according to claim 1, is characterized in that, described purification thing receiving tank is the thin-film evaporator that top is connected to vacuum pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520349333.5U CN204779430U (en) | 2015-05-27 | 2015-05-27 | Primary raw material neighbour p toluene sulfonyl chloride's of neighbour / para toluene sulfonamide purification equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520349333.5U CN204779430U (en) | 2015-05-27 | 2015-05-27 | Primary raw material neighbour p toluene sulfonyl chloride's of neighbour / para toluene sulfonamide purification equipment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN204779430U true CN204779430U (en) | 2015-11-18 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201520349333.5U Expired - Fee Related CN204779430U (en) | 2015-05-27 | 2015-05-27 | Primary raw material neighbour p toluene sulfonyl chloride's of neighbour / para toluene sulfonamide purification equipment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN204779430U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106986793A (en) * | 2017-05-09 | 2017-07-28 | 张建 | A kind of paratoluensulfonyl chloride purification system |
| CN108440346A (en) * | 2018-05-07 | 2018-08-24 | 浙江嘉化新材料有限公司 | O-toluenesulfonyl chloride method of purification |
-
2015
- 2015-05-27 CN CN201520349333.5U patent/CN204779430U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106986793A (en) * | 2017-05-09 | 2017-07-28 | 张建 | A kind of paratoluensulfonyl chloride purification system |
| CN108440346A (en) * | 2018-05-07 | 2018-08-24 | 浙江嘉化新材料有限公司 | O-toluenesulfonyl chloride method of purification |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20151118 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |