Method for preparing paraphthaloyl chloride

A technology of terephthaloyl chloride and terephthalic acid, which is applied in the field of chemical raw material preparation, can solve the problems of high cost and low catalyst activity, and achieve the effect of simple and convenient reaction operation and high product yield

Active Publication Date: 2015-07-01
河南能源集团研究总院有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the outstanding problems of low catalyst activity and high cost in the preparation of terephthaloyl chloride by the current thionyl chloride method, the purpose of the present invention is to develop a catalyst system with low price, high activity and high selectivity, which is used to catalyze Terephthaloyl dichloride reacts with thionyl chloride to produce terephthaloyl dichloride in high yield

Method used

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  • Method for preparing paraphthaloyl chloride
  • Method for preparing paraphthaloyl chloride
  • Method for preparing paraphthaloyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 10 grams of terephthalic acid (PTA), 50 grams of thionyl chloride (SOCl 2 ) and 0.02 grams of iron powder were added to a 100ml two-neck round bottom flask, stirred evenly, and heated to 90 o C reacted for 16 hours, the generated HCl and SO 2 The mixed gas was first absorbed with water, and then absorbed with 30% NaOH solution. After the reaction was over, the excess thionyl chloride was recovered by distillation, and then 9.7 g of terephthaloyl chloride (TPC) was obtained by distillation under reduced pressure. The isolated yield of the product was 79%. The product was qualitatively analyzed by gas chromatography-mass spectrometry, hydrogen nuclear magnetic resonance spectrum, and carbon spectrum, and the purity detected by gas chromatography was higher than 99%.

Embodiment 2~27

[0017] The concrete method of embodiment 2~27 is similar to embodiment 1, and specific reaction condition and result are listed in table 1.

[0018] According to Example 1, it can be seen that iron powder can catalyze the reaction of PTA and thionyl chloride to prepare TPC. Embodiment 2 shows that catalyst plays a vital role in this reaction, and when there is no catalyst, product TPC cannot be obtained. Embodiment 3~5 shows that trying to catalyze this reaction with metals such as copper powder, aluminum powder, zinc powder can not obtain product TPC. Embodiment 6~7 shows that salts such as cupric chloride, nickel chloride also can not catalyze this reaction. Examples 8 to 27 show that iron salts such as ferric chloride, ferrous chloride, ferric sulfate, ferrous sulfate, ferric nitrate, ferrous nitrate, ferric phosphate, ferrous phosphate and iron acetylacetonate, ferrous oxalate, ferrous lactate Iron, ferric citrate, ferrous tartrate, ferric malate, ferrous gluconate, ferr...

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Abstract

The invention relates to a method for preparing paraphthaloyl chloride. The method comprises the steps of mixing thionyl chloride and terephthalic acid according to the mass ratio of (2:1)-(5:1) by taking one or more of iron powder, iron salt and an iron-containing compound which is 0.2-5 percent of the mass of the terephthalic acid as a catalyst, generating reaction under the temperature of 70-120 DEG C for 4-16 hours, performing distillation to recycle the excessive thionyl chloride, and performing decompressed distillation to obtain the paraphthaloyl chloride. The yield can be up to 96 percent at most, and the purity is higher than 99 percent. The method has the advantages that the catalyst is low in cost and readily available, the product is high in yield, and the reaction operation is simple and convenient and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical raw material preparation, and relates to a method for preparing terephthaloyl dichloride. Background technique [0002] Terephthaloyl chloride is an important organic chemical raw material, which can be used to synthesize polyamide, polyarylamide, polyester, polyarylate, polyarylsulfone and other high-temperature-resistant and high-strength polymer materials. For example, aramid 1414 is a polymer of terephthaloyl chloride and p-phenylenediamine, its toughness and strength can reach 2 times and 6 times that of high-quality steel, respectively, and it is resistant to high temperature, chemical corrosion, heat shrinkage and creep. , Widely used in aircraft, rockets, missiles and bulletproof equipment. As another example, polyarylsulfone fiber is a polymer of terephthaloyl chloride, 4,4'-diaminodiphenylsulfone and 3,3'-diaminodiphenylsulfone, which has good thermal stability and can be used at 250 ...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07C63/30C07C51/60
CPCY02P20/52
Inventor黄义争付瑶徐杰宋灿高进魏灵朝苗虹蒋元力
Owner河南能源集团研究总院有限公司