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A kind of method that transesterification prepares phthalic acid higher carbon alcohol ester

A technology of dimethyl phthalate and phthalic acid, which is applied in the field of transesterification to prepare higher alcohol phthalate, can solve the problems of many side reactions, less side reactions, low consumption of raw materials, etc. Low corrosiveness, mild reaction conditions, clean process and energy saving effect

Active Publication Date: 2018-01-02
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the process of preparing DIDP, DINP, DPHP and other high-carbon alcohol esters of phthalic acid by the current phthalic anhydride esterification process, process wastewater will be generated. The raw material phthalic anhydride has poor storage and transportation stability, inconvenient feeding, strong irritation to the human body, and catalyst corrosion. Strong, side reaction is many, and raw material consumption is high outstanding problem, the purpose of the invention is: develop a kind of method for transesterification preparation phthalate higher carbon alcohol esters such as DIDP, DINP and DPHP, have following advantage: (1) process is clean Energy saving: no water is generated in the reaction, which can not only reduce the energy consumption of water separation, but also avoid the production and discharge of process wastewater; Carbon alcohol ester replaces phthalic anhydride, which has good storage and transportation stability and convenient reaction feeding; (3) The researched and developed transesterification catalyst has little or no corrosion to the device, mild reaction conditions, less side reactions, and lower raw material consumption

Method used

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  • A kind of method that transesterification prepares phthalic acid higher carbon alcohol ester
  • A kind of method that transesterification prepares phthalic acid higher carbon alcohol ester
  • A kind of method that transesterification prepares phthalic acid higher carbon alcohol ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 19.4 grams of dimethyl phthalate (DMP for short, 0.1 mol), 47.5 grams of 2-propylheptanol (0.3 mol), and 0.2 grams of potassium titanium oxalate (1.0% of the mass of DMP) into 100 ml of In the two-necked round-bottomed flask of the water dispenser, connect the condenser to the water separator, stir evenly, and heat up to 200 ° C for 5 hours. After the reaction, the mixture is qualitatively analyzed by gas chromatography-mass spectrometry, and quantitatively analyzed by gas chromatography. Both the conversion rate of DMP and the selectivity of DPHP are above 99%.

Embodiment 2

[0024] Catalyst blank experiment: no catalyst was added, other conditions were the same as in Example 1, the conversion rate of DMP only reached 50%, and the selectivity of DPHP was only 5%.

Embodiment 3～21

[0026] The specific method of Examples 3-21 is similar to that of Example 1, and the specific reaction conditions and results are shown in Table 1.

[0027] It can be seen from the catalyst blank experiment that DMP and 2-propylheptanol were heated and reacted at 200° C. for 5 hours, and the conversion rate of DMP and the selectivity of DPHP were all very low (embodiment 2). Concentrated sulfuric acid has a good catalytic effect on the preparation of DPHP by the esterification reaction of 2-propylheptanol and phthalic anhydride, and the conversion rate of phthalic anhydride and the selectivity of DPHP can reach more than 99%. Yet, the vitriol oil is used to catalyze the transesterification reaction of DMP and 2-propylheptanol, although the DMP conversion rate can reach more than 99%, but the DPHP selectivity only has 80% (embodiment 3). Trying to use tin titanate as a catalyst, the reaction result under the same conditions is the same as that of the catalyst blank experiment (...

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Abstract

The invention relates to a method for preparing phthalic acid higher alcohol esters by transesterification. High carbon alcohols such as decyl alcohol and 2-propylheptanol are used as raw materials, and potassium titanium oxalate, aluminum titanate, potassium titanate, magnesium titanate, calcium titanate, zirconium titanate, barium titanate, aluminum trichloride, One or more of antimony trichloride, titanium tetrachloride, zirconium tetrachloride, titanium tetramethoxide, titanium tetrakis (2-propylheptyl alcohol), titanium tetraisonononoxide, and titanium tetraisodecyl alcohol are Catalyst, react at 160-200 DEG C for 2-6 hours, the conversion rate of low-carbon alcohol phthalate and the selectivity of high-carbon alcohol phthalate can reach up to more than 99%. The invention has the advantages of clean process and energy saving, good stability of raw material storage and transportation, convenient feeding, low catalyst corrosion, mild reaction conditions, less side reactions, low raw material consumption and the like.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a method for preparing higher alcohol phthalates by transesterification. Background technique [0002] Plasticizer is an indispensable additive for the production of plastics, rubber and polyester products. Its function is to weaken the intermolecular force of polymers, increase the mobility of molecular chains, reduce crystallinity, improve the processability, plasticity, Comprehensive properties such as flexibility and stretchability. [0003] my country mainly uses low-end plasticizers such as dibutyl phthalate (DBP for short) and dioctyl phthalate (DOP for short). These plasticizers will migrate and precipitate, and have a great environmental impact. They have been restricted in production and use in the United States, Japan, the European Union and other places. They have been mainly used by diisononyl phthalate (DINP for short), diisodecyl phthalate, etc. Alcoh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/80C07C67/293
Inventor 黄义争徐杰高进苗虹孙颖马红
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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