CN102304073A - Method for preparing 4.4-dichlorodiphenyl sulfone by using sulfuric acid - Google Patents
Method for preparing 4.4-dichlorodiphenyl sulfone by using sulfuric acid Download PDFInfo
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- CN102304073A CN102304073A CN201110245951A CN201110245951A CN102304073A CN 102304073 A CN102304073 A CN 102304073A CN 201110245951 A CN201110245951 A CN 201110245951A CN 201110245951 A CN201110245951 A CN 201110245951A CN 102304073 A CN102304073 A CN 102304073A
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- sulfuric acid
- dichlorodiphenyl sulfone
- chlorobenzene
- diphenyl sulfone
- dichloro diphenyl
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Abstract
The invention discloses a method for preparing 4.4-dichlorodiphenyl sulfone by using sulfuric acid, which comprises the following steps: weighing concentrated sulfuric acid and chlorobenzene according to a molar ratio of 1:2.5, filling the concentrated sulfuric acid and chlorobenzene into a closed container respectively, and heating to 200 DEG C; under a condition that the reaction pressure is kept at 4.5*10<5>Pa, refluxing the reaction solution and heating to 240 DEG C; reacting for 6 to 8 hours under a condition that boric acid is used as a catalyst and the pressure is kept between 4.5*10<5>Pa and 5*10<5>Pa; and finishing the reaction, and separating 4.4-dichlorodiphenyl sulfone crystals by using ethanol. Therefore, the method can inhibit the production of byproducts including 2.4-dichlorodiphenyl sulfone and 3.4-dichlorodiphenyl sulfone and improve the yield of 4.4-dichlorodiphenyl sulfone to 73 percent; and compared with the prior art, the method greatly improves the utilization rate of raw materials.
Description
Technical field
The present invention relates to a kind of preparation method of 4.4-dichloro diphenyl sulfone, especially a kind of vitriol oil that adopts is the preparation method of the 4.4-dichloro diphenyl sulfone of one of raw material.
Background technology
4.4 the – dichloro diphenyl sulfone is called for short DDS, is white crystal, can distil, and is soluble in organic solvents such as benzene, chlorobenzene, DMF; Be slightly soluble in ethanol, methyl alcohol; Water insoluble.Its flash-point is 233 ℃, and boiling point then is 397 ℃.
4.4 the – dichloro diphenyl sulfone has purposes widely at engineering plastics and field of fine chemical, is the main raw material of engineering plastics such as preparation polysulfones, polyethersulfone, also is the intermediate of medicine, dyestuff, agricultural chemicals.
In the prior art; The method that adopts the vitriol oil to prepare the 4.4-dichloro diphenyl sulfone is: the chlorobenzene and the vitriol oil were reacted 24 hours in 200 degrees centigrade; To generate the 4.4-dichloro diphenyl sulfone; Subsidiary by product 2.4-dichlorobenzene sulfone, 3.4-dichlorobenzene sulfone, wherein, the yield of 4.4-dichloro diphenyl sulfone is no more than 43%; Hence one can see that; The quality product that this method obtains is bad, and yield is low, and waste of raw materials is serious.
Summary of the invention
The present invention is directed to the deficiency of prior art; A kind of sulfuric acid preparation method of 4.4-dichloro diphenyl sulfone is provided, and it adds catalyzer, improves existing reaction conditions in reaction process, thereby has improved the production yield of 4.4-dichloro diphenyl sulfone; Reduce the reaction times, improve quality product.
For realizing above technical purpose, the present invention will take following technical scheme:
A kind of sulfuric acid preparation method of 4.4-dichloro diphenyl sulfone may further comprise the steps: at first according to the mol ratio of the 1:2.5 metering vitriol oil and chlorobenzene, and the vitriol oil and chlorobenzene are put into be heated to 200 ℃ in the encloses container together respectively; Be controlled at 4.5*10 in reaction pressure
5Under the situation of Pa, back flow reaction liquid is warming up to 240 ℃; Be that catalyzer, pressure maintain 4.5-5*10 with boric acid at last
5Under the situation of Pa, reacted 6-8 hour; After the end, adopt ethanol that 4.4-dichloro diphenyl sulfone Crystallization Separation is gone out to get final product.
According to above technical scheme, can realize following beneficial effect:
It is raw material that the present invention adopts the vitriol oil and excessive chlorobenzene; Under high pressure-temperature; With boric acid is that catalyzer carries out condensation reaction, after reaction finishes, adopts ethanol to carry out 4.4-dichloro diphenyl sulfone Crystallization Separation; Therefore; The present invention can suppress by product 2.4-dichlorobenzene sulfone, 3.4-dichlorobenzene sulfone in condensation reaction, improve the yield of 4.4-dichloro diphenyl sulfone, can be up to 73%; Compared with prior art, greatly improved raw material availability.
Embodiment
Below will combine embodiment that technical scheme of the present invention at length is described.
The sulfuric acid preparation method of 4.4-dichloro diphenyl sulfone of the present invention, the reagent that is adopted has: mass concentration is 92% vitriol oil, chlorobenzene, boric acid and ethanol; Its preparation method may further comprise the steps: at first according to the mol ratio of the 1:2.5 metering vitriol oil and chlorobenzene, and the vitriol oil and chlorobenzene are put into be heated to 200 ℃ in the encloses container together respectively; Be controlled at 4.5*10 in reaction pressure
5Under the situation of Pa, back flow reaction liquid is warming up to 240 ℃; Be that catalyzer, pressure maintain 4.5-5*10 with boric acid at last
5Under the situation of Pa, reacted 6-8 hour; After the end, adopt ethanol that 4.4-dichloro diphenyl sulfone Crystallization Separation is gone out to get final product.
Claims (1)
1. the sulfuric acid preparation method of a 4.4-dichloro diphenyl sulfone is characterized in that, may further comprise the steps: at first according to the mol ratio of the 1:2.5 metering vitriol oil and chlorobenzene, and the vitriol oil and chlorobenzene are put into be heated to 200 ℃ in the encloses container together respectively; Be controlled at 4.5*10 in reaction pressure
5Under the situation of Pa, back flow reaction liquid is warming up to 240 ℃; Be that catalyzer, pressure maintain 4.5-5*10 with boric acid at last
5Under the situation of Pa, reacted 6-8 hour; After the end, adopt ethanol that 4.4-dichloro diphenyl sulfone Crystallization Separation is gone out to get final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110245951A CN102304073A (en) | 2011-08-25 | 2011-08-25 | Method for preparing 4.4-dichlorodiphenyl sulfone by using sulfuric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110245951A CN102304073A (en) | 2011-08-25 | 2011-08-25 | Method for preparing 4.4-dichlorodiphenyl sulfone by using sulfuric acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102304073A true CN102304073A (en) | 2012-01-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110245951A Pending CN102304073A (en) | 2011-08-25 | 2011-08-25 | Method for preparing 4.4-dichlorodiphenyl sulfone by using sulfuric acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102304073A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4983773A (en) * | 1988-10-19 | 1991-01-08 | Basf Aktiengesellschaft | Preparation of bis-(4-chlorophenyl) sulfone |
| CN1623982A (en) * | 2003-12-02 | 2005-06-08 | 马炳荣 | Method for preparing 4,4'-dichloride diphenyl sulfone |
-
2011
- 2011-08-25 CN CN201110245951A patent/CN102304073A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4983773A (en) * | 1988-10-19 | 1991-01-08 | Basf Aktiengesellschaft | Preparation of bis-(4-chlorophenyl) sulfone |
| CN1623982A (en) * | 2003-12-02 | 2005-06-08 | 马炳荣 | Method for preparing 4,4'-dichloride diphenyl sulfone |
Non-Patent Citations (3)
| Title |
|---|
| 《天津化工》 20050331 孟翠敏 4,4'-二氯二苯砜的合成与应用 第41-42页 1 第19卷, 第2期 * |
| 孟翠敏: "4,4’-二氯二苯砜的合成与应用", 《天津化工》, vol. 19, no. 2, 31 March 2005 (2005-03-31), pages 41 - 42 * |
| 赵玉英等: "4,4＇-二氯二苯砜", 《山西化工》, no. 1, 31 December 1997 (1997-12-31), pages 54 - 2 * |
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Application publication date: 20120104 |