CN1029396C - Synthesizing method of tetrachloroquinone anhydride - Google Patents
Synthesizing method of tetrachloroquinone anhydride Download PDFInfo
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- CN1029396C CN1029396C CN 90107375 CN90107375A CN1029396C CN 1029396 C CN1029396 C CN 1029396C CN 90107375 CN90107375 CN 90107375 CN 90107375 A CN90107375 A CN 90107375A CN 1029396 C CN1029396 C CN 1029396C
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- anhydride
- tetrachlorophthalic anhydride
- chlorine
- synthetic method
- iodine chloride
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Abstract
The present invention relates to a method for synthesizing tetrachlorobenzene anhydride for fine chemical industry. Chlorosulfonic acid is used as a reaction solvent. Iodine chloride or molybdenum is used as a catalyst. Benzoic anhydride is chlorinated to be synthesized into the tetrachlorophthalic anhydride by leading chlorine gas in at normal pressure. The method solves the problems of a general method for synthesizing the tetrachlorophthalic anhydride of high reaction temperature, complicated operation, low mole yield, etc., and simultaneously, enables the recovery rates of the reaction solvent and the catalyst to be enhanced; the production cost is reduced; the product quality is enhanced; the discharge amount of three waste is greatly reduced.
Description
The invention belongs to the synthetic method in the fine chemistry industry.
At present, the synthetic method of international tetrachlorophthalic anhydride, mainly be: 1. be solvent with the oleum, with iodine or iodine chloride is the solvent method of catalyzer, this method solvent load is big and can only disposablely use, and the cost height can also produce a large amount of spent acid, solvent energy recycling use in some solvent method, but molar yield is low.2. the fusion phthalic anhydride chlorination process under molybdenum chloride catalysis, this method make the phthalic anhydride distillation serious, and operation and quality product are restive.3. adopting Lewis acid such as iron(ic) chloride or cobalt chloride is the gas phase chlorination method of catalyzer, this method reaction temperature height, and quality product is bad, and is technical not mature enough.So the synthetic method of existing tetrachlorophthalic anhydride all can not satisfy the actual demand of producing.
The objective of the invention is to improve the synthetic quality of tetrachlorophthalic anhydride and reduce production costs, reduce temperature of reaction, make simple to operate, reliable operation, simultaneously, simplify complicated technological process.
Basic design of the present invention is in a custom-designed reactor, phthalic anhydride to be dissolved in the chlorsulfonic acid, in the presence of iodine chloride, feed chlorine and react, be reflected under the normal pressure and carry out, after reaction is finished, steaming desolventizes and catalyzer, and residuum promptly obtains tetrachlorophthalic anhydride through washing, oven dry.Recovered solvent and catalyzer needn't be made with extra care, and can reuse.For making the catalyst recovery yield height, adopt double-heat exchanger in parallel.
Advantage of the present invention is that temperature of reaction is low, smooth operation, simple, and " three wastes " generation is few, and solvent and catalyzer are recyclable to be recycled, and production cost is reduced, and quality product improves.
As shown in drawings, 1,6 heat exchangers, 2,5 stopping valve, 3,4 tail gas outlet, 7,12 cold water inlets, 8 chlorine conduits, 9 reactors, 10 chlorine gas distribution plates, 11 discharge ports, 13,14 cooling water outlets.
Be to state an embodiment who chats with reference to the accompanying drawings in detail below:
In the reactor 9 of 300-500 milliliter, the chlorsulfonic acid that adds the 250-350 milliliter, the iodine or the iodine chloride of the phthalic anhydride of 60-100 gram and 5-10 gram, chlorine imports through the speed of chlorine conduit 8 with the 10-16 Grams Per Minute, control reaction temperature is 60-150 ℃, progressively heat up, cold water is through 12,7, delivery heat exchanger 1, in 6, in the reaction, catalyzer distillation crystallization is arranged at heat exchanger 1, in 6, at this moment shut-off valve 2 or 5 feeds hot water or steam through 12 or 7, catalyzer is transferred in the reactor 9 automatically, again hot water or steam through 12 or 7 are changed into cold water, open valve 2 or 5, just can react normally.Reaction is transferred to reaction mixture in the general distiller after finishing, and steams to desolventize with catalyzer and reclaim to be provided with back preparation usefulness, and residuum washes with water, and oven dry then promptly obtains tetrachlorophthalic anhydride 110-193 gram.
Claims (4)
1, a kind of tetrachlorophthalic anhydride synthetic method that is used for fine chemistry industry industry, main raw material phthalic anhydride, iodine chloride, the chlorsulfonic acid etc. of adopting, it is characterized in that with the chlorsulfonic acid being that reaction solvent, iodine chloride or molybdenum are catalyzer, add chlorine, in the reactor of the heat exchanger that has two parallel connections, carry out building-up reactions.
2, tetrachlorophthalic anhydride synthetic method according to claim 1, the cooperation ratio that it is characterized in that phthalic anhydride, iodine chloride, chlorine, chlorsulfonic acid is 1: (0.01-0.25): (4-12): (2-15) mole, its temperature of reaction is 60-170 ℃ and carries out under normal pressure.
3, tetrachlorophthalic anhydride synthetic method according to claim 1, the recovery method of its feature solvent (chlorsulfonic acid), catalyzer (iodine chloride, molybdenum, iodine) is a distillation method.
4, tetrachlorophthalic anhydride synthetic method according to claim 1 is characterized in that using the reactor of the heat exchanger that has two parallel connections, is provided with chlorine gas distribution plate in the reactor body, and chlorine tube and reactor body link.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90107375 CN1029396C (en) | 1990-08-28 | 1990-08-28 | Synthesizing method of tetrachloroquinone anhydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90107375 CN1029396C (en) | 1990-08-28 | 1990-08-28 | Synthesizing method of tetrachloroquinone anhydride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1059335A CN1059335A (en) | 1992-03-11 |
| CN1029396C true CN1029396C (en) | 1995-08-02 |
Family
ID=4880505
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90107375 Expired - Fee Related CN1029396C (en) | 1990-08-28 | 1990-08-28 | Synthesizing method of tetrachloroquinone anhydride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1029396C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120035395A1 (en) * | 2009-04-28 | 2012-02-09 | Sumitomo Chemical Company, Limited | Process for producing phthalic acid compound including chlorinated aromatic ring |
| CN102079734A (en) * | 2009-11-26 | 2011-06-01 | 浙江启明药业有限公司 | Circulating economic comprehensive treatment method for industrial production of tetrachlorophthalic anhydride |
| CN114933579A (en) * | 2022-04-26 | 2022-08-23 | 河北海力香料股份有限公司 | Preparation method of tetrachlorophthalic anhydride |
-
1990
- 1990-08-28 CN CN 90107375 patent/CN1029396C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1059335A (en) | 1992-03-11 |
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| C14 | Grant of patent or utility model | ||
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| CF01 | Termination of patent right due to non-payment of annual fee |