CN1059335A - The synthetic method of tetrachlorophthalic anhydride - Google Patents
The synthetic method of tetrachlorophthalic anhydride Download PDFInfo
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- CN1059335A CN1059335A CN 90107375 CN90107375A CN1059335A CN 1059335 A CN1059335 A CN 1059335A CN 90107375 CN90107375 CN 90107375 CN 90107375 A CN90107375 A CN 90107375A CN 1059335 A CN1059335 A CN 1059335A
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- tetrachlorophthalic anhydride
- synthetic method
- chlorine
- catalyzer
- chlorsulfonic acid
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Abstract
A kind of tetrachlorophthalic anhydride synthetic method that is used for fine chemistry industry industry is a reaction solvent with the chlorsulfonic acid, and iodine chloride or molybdenum are catalyzer, import chlorine, under normal pressure the phthalic anhydride chlorination is synthesized tetrachlorophthalic anhydride, it has solved general tetrachlorophthalic anhydride synthesis reaction temperature height, complicated operation, problems such as molar yield is low, simultaneously, make solvent and catalyst recovery yield height, reduced production cost, improve quality product, reduced the quantity discharged of " three wastes " significantly.
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 oxide 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 arranged side by side.
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, the outlet of 3,4 tail gas, 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 2,5 through 12,7 feed hot water or steam, and catalyzer is transferred in the reactor 9 automatically, again through 12,7 hot water or steam change cold water into, open valve 2,5, 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, chlorine, 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 a reactor, carry out building-up reactions.
2, according to claim 1 described tetrachlorophthalic anhydride synthetic method, it is characterized in that the cooperation ratio of phthalic anhydride, iodine chloride, chlorine, chlorsulfonic acid is 1: (0.01-0.25): (4-12): (2-15): (5-15) mole.Its temperature of reaction is 60-170 ℃, and carries out under normal pressure.
3,, it is characterized in that the recovery method of solvent (chlorsulfonic acid), catalyzer (iodine chloride, molybdenum, iodine) is a distillation method according to claim 1 described tetrachlorophthalic anhydride synthetic method.
4, tetrachlorophthalic anhydride synthetic method according to claim 1 is characterized in that reactor is connected with reactor body by the heat exchanger of 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 true CN1059335A (en) | 1992-03-11 |
| CN1029396C 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) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102414161A (en) * | 2009-04-28 | 2012-04-11 | 住友化学株式会社 | Process for producing phthalic acid compound including chlorinated aromatic ring |
| 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
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102414161A (en) * | 2009-04-28 | 2012-04-11 | 住友化学株式会社 | Process for producing phthalic acid compound including chlorinated aromatic ring |
| CN102414161B (en) * | 2009-04-28 | 2014-12-24 | 住友化学株式会社 | 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1029396C (en) | 1995-08-02 |
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