CN104725285A - Method for removing sulfate from sodium isopropyl benzenesulfonate - Google Patents
Method for removing sulfate from sodium isopropyl benzenesulfonate Download PDFInfo
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- CN104725285A CN104725285A CN201310733290.6A CN201310733290A CN104725285A CN 104725285 A CN104725285 A CN 104725285A CN 201310733290 A CN201310733290 A CN 201310733290A CN 104725285 A CN104725285 A CN 104725285A
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- sodium sulfonate
- cumene sodium
- saturated solution
- virahol
- vitriol
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Abstract
The invention provides a method for removing sulfate from sodium isopropyl benzenesulfonate, which comprises the following steps: (1) adding isopropanol or anhydrous ethanol into a sodium isopropyl benzenesulfonate saturated solution while stirring, wherein the volume ratio of the sodium isopropyl benzenesulfonate saturated solution to the isopropanol or anhydrous ethanol is 100:(30-40), and the addition rate is gradually reduced; when all the white floccules appear, stopping adding the isopropanol or anhydrous ethanol, filtering out the filtrate, and discarding a small amount of filter cake; and (2) concentrating the obtained filtrate, and crystallizing to obtain the sulfate-removed sodium isopropyl benzenesulfonate. The method can effectively remove sulfate from sodium isopropyl benzenesulfonate, and the impurity sulfate ion content is lowered from 3% to 0.5-0.05%.
Description
Technical field
The present invention relates to a kind of purification process of chemical reagent, in especially a kind of cumene sodium sulfonate, remove the method for vitriol.
Background technology
Cumene sodium sulfonate, No. CAS: 32073-22-6, molecular formula: C
9h
11naO
3s, main application is produce at sanitising agent and can work as solubility promoter, coupler and auxiliary agent in other industry; For organic synthesis, cosmetics of everyday use and chemical reagent.
But find in process of production, the vitriol that cumene sodium sulfonate generates in reaction process is not easily rejected, only rely on the production technique repeating crystallization, vitriol wherein also only can maintain about 3%, be difficult to the vitriol reduced further again in cumene sodium sulfonate, thus the quality product of cumene sodium sulfonate cannot be further enhanced.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method removing vitriol in cumene sodium sulfonate.
For solving the problems of the technologies described above, technical scheme of the present invention is:
Remove a method for vitriol in cumene sodium sulfonate, concrete preparation process is as follows:
(1) Virahol or dehydrated alcohol is added by under cumene sodium sulfonate saturated solution agitation condition, wherein, the volume ratio of described cumene sodium sulfonate saturated solution and Virahol or dehydrated alcohol is 100:30-40, slow after fast before adding speed, after White Flocculus is all gushed out, stop adding Virahol or dehydrated alcohol, filter, filtrate leached, a small amount of filter cake discards;
(2) gained filtrate concentrates post crystallization, obtains the cumene sodium sulfonate after removing vitriol.
Preferably, remove the method for vitriol in above-mentioned cumene sodium sulfonate, described in described step (1), the volume ratio of cumene sodium sulfonate saturated solution and Virahol or dehydrated alcohol is 100:30.
Preferably, the method of vitriol is removed in above-mentioned cumene sodium sulfonate, slowly refer in the cumene sodium sulfonate saturated solution of 60-70% after fast before adding speed in described step (1) and directly add Virahol or dehydrated alcohol, in the cumene sodium sulfonate saturated solution of 30-40%, add Virahol or dehydrated alcohol with the speed of 1 ± 0.5ml/s.
The invention has the beneficial effects as follows:
The method of vitriol is removed in above-mentioned cumene sodium sulfonate; simple to operate; can from cumene sodium sulfonate effective elimination vitriol; impurity sulfate ion content drops to 0.5%-0.05% by previous 3%; reliably easy through repeating experiment effect; quality product obviously rises, and is applicable to the needs that large-scale industrial is produced.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is further described.
Embodiment 1
Remove a method for vitriol in cumene sodium sulfonate, concrete preparation process is as follows:
(1) synthesizing iso-propylbenzene sodium sulfonate saturated solution is configured;
(2) Virahol is added under stirring, the volume ratio of described cumene sodium sulfonate saturated solution and Virahol is 100:30, slow after fast before adding speed, namely have in the cumene sodium sulfonate saturated solution of 60% and directly add Virahol or dehydrated alcohol, in the cumene sodium sulfonate saturated solution of 40%, add Virahol or dehydrated alcohol, after White Flocculus is all gushed out with the speed of about 1ml/s, stop adding Virahol, filter, filtrate leached, a small amount of filter cake discards;
(3) gained filtrate concentrates post crystallization, obtains the cumene sodium sulfonate after removing vitriol.
Vitriol inspection is carried out to gained cumene sodium sulfonate:
According to the method that GB/T602-2002 is contained, preparation 0.05,0.1,0.2,0.3,0.4,0.5mg/ml vitriol standardized solution (SO
4 2-).
Take 1g sample, be water-solublely diluted to 20mL, add 2mL hydrochloric acid soln (30%), shake up, drip 3mL barium chloride solution (250g/L), shake up, place 10min.Turbidimetry is adopted to judge sulphate content.
Detected result: vitriol≤0.05%
Embodiment 2
Remove a method for vitriol in cumene sodium sulfonate, concrete preparation process is as follows:
(1) synthesizing iso-propylbenzene sodium sulfonate saturated solution is configured;
(2) Virahol is added under stirring, the volume ratio of described cumene sodium sulfonate saturated solution and Virahol is 100:40, slow after fast before adding speed, namely have in the cumene sodium sulfonate saturated solution of 70% and directly add Virahol or dehydrated alcohol, in the cumene sodium sulfonate saturated solution of 30%, add Virahol or dehydrated alcohol, after White Flocculus is all gushed out with the speed of about 1ml/s, stop adding Virahol, filter, filtrate leached, a small amount of filter cake discards;
(3) gained filtrate concentrates post crystallization, obtains the cumene sodium sulfonate after removing vitriol.
Embodiment 3
Remove a method for vitriol in cumene sodium sulfonate, concrete preparation process is as follows:
(1) synthesizing iso-propylbenzene sodium sulfonate saturated solution is configured;
(2) Virahol is added under stirring, the volume ratio of described cumene sodium sulfonate saturated solution and Virahol is 100:35, slow after fast before adding speed, namely have in the cumene sodium sulfonate saturated solution of 65% and directly add Virahol or dehydrated alcohol, in the cumene sodium sulfonate saturated solution of 35%, add Virahol or dehydrated alcohol, after White Flocculus is all gushed out with the speed of about 1ml/s, stop adding Virahol, filter, filtrate leached, a small amount of filter cake discards;
(3) gained filtrate concentrates post crystallization, obtains the cumene sodium sulfonate after removing vitriol.
Embodiment 4
Remove a method for vitriol in cumene sodium sulfonate, concrete preparation process is as follows:
(1) synthesizing iso-propylbenzene sodium sulfonate saturated solution is configured;
(2) Virahol is added under stirring, the volume ratio of described cumene sodium sulfonate saturated solution and Virahol is 100:30, slow after fast before adding speed, namely have in the cumene sodium sulfonate saturated solution of 67% and directly add Virahol or dehydrated alcohol, in the cumene sodium sulfonate saturated solution of 33%, add Virahol or dehydrated alcohol, after White Flocculus is all gushed out with the speed of about 1ml/s, stop adding Virahol, filter, filtrate leached, a small amount of filter cake discards;
(3) gained filtrate concentrates post crystallization, obtains the cumene sodium sulfonate after removing vitriol.
The described reactant of one of embodiment 1-4 is commercially available prod, is increased by its consumption or reduces, all belong to protection scope of the present invention according to same ratio.
Above-mentioned detailed description of the method removing vitriol in this kind of cumene sodium sulfonate being carried out with reference to embodiment; illustrative instead of determinate; several embodiments can be listed according to institute's limited range; therefore in the change do not departed under general plotting of the present invention and amendment, should belong within protection scope of the present invention.
Claims (3)
1. remove a method for vitriol in cumene sodium sulfonate, it is characterized in that: concrete preparation process is as follows:
(1) Virahol or dehydrated alcohol is added by under cumene sodium sulfonate saturated solution agitation condition, wherein, the volume ratio of described cumene sodium sulfonate saturated solution and Virahol or dehydrated alcohol is 100:30-40, slow after fast before adding speed, after White Flocculus is all gushed out, stop adding Virahol or dehydrated alcohol, filter, filtrate leached, a small amount of filter cake discards;
(2) gained filtrate concentrates post crystallization, obtains the cumene sodium sulfonate after removing vitriol.
2. remove the method for vitriol in cumene sodium sulfonate according to claim 1, it is characterized in that: described in described step (1), the volume ratio of cumene sodium sulfonate saturated solution and Virahol or dehydrated alcohol is 100:30.
3. in cumene sodium sulfonate according to claim 1, remove the method for vitriol, it is characterized in that: refer to slowly in the cumene sodium sulfonate saturated solution of 60-70% after fast before adding speed in described step (1) and directly add Virahol or dehydrated alcohol, in the cumene sodium sulfonate saturated solution of 30-40%, add Virahol or dehydrated alcohol with the speed of 1 ± 0.5ml/s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310733290.6A CN104725285A (en) | 2013-12-23 | 2013-12-23 | Method for removing sulfate from sodium isopropyl benzenesulfonate |
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|---|---|---|---|
| CN201310733290.6A CN104725285A (en) | 2013-12-23 | 2013-12-23 | Method for removing sulfate from sodium isopropyl benzenesulfonate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105330573A (en) * | 2015-11-19 | 2016-02-17 | 江南大学 | Sodium cumenesulfonate solution and preparation method thereof |
| CN115850124A (en) * | 2022-12-08 | 2023-03-28 | 吴赣药业（苏州）有限公司 | Preparation method of sodium xylene sulfonate |
| CN116023306A (en) * | 2022-12-19 | 2023-04-28 | 吴赣药业（苏州）有限公司 | Method for removing inorganic sulfate from sodium cumene sulfonate |
-
2013
- 2013-12-23 CN CN201310733290.6A patent/CN104725285A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105330573A (en) * | 2015-11-19 | 2016-02-17 | 江南大学 | Sodium cumenesulfonate solution and preparation method thereof |
| CN115850124A (en) * | 2022-12-08 | 2023-03-28 | 吴赣药业（苏州）有限公司 | Preparation method of sodium xylene sulfonate |
| CN115850124B (en) * | 2022-12-08 | 2023-12-19 | 吴赣药业（苏州）有限公司 | Preparation method of sodium xylenesulfonate |
| CN116023306A (en) * | 2022-12-19 | 2023-04-28 | 吴赣药业（苏州）有限公司 | Method for removing inorganic sulfate from sodium cumene sulfonate |
| CN116023306B (en) * | 2022-12-19 | 2024-02-02 | 吴赣药业（苏州）有限公司 | Method for removing inorganic sulfate from sodium cumene sulfonate |
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