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Method used for preparing higher aliphatic phthalates via ester exchange

A technology of phthalic acid and higher alcohol esters, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of many side reactions, low raw material consumption, and few side reactions, and achieve The catalyst is less corrosive, the process is clean and energy-saving, and the effect of mild reaction conditions

Active Publication Date: 2016-06-08
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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  • Method used for preparing higher aliphatic phthalates via ester exchange
  • Method used for preparing higher aliphatic phthalates via ester exchange
  • Method used for preparing higher aliphatic phthalates via ester exchange

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 19.4 grams of dimethyl phthalate (abbreviated as DMP, 0.1mol), 47.5 grams of 2-propylheptanol (0.3mol), and 0.2 grams of potassium titanium oxalate (1.0% of the mass of DMP) into 100ml of water separator In the two-necked round-bottomed flask of the device, the condenser was connected to the water separator, stirred evenly, and the temperature was raised to 200 ° C for 5 hours. After the reaction, the mixture was qualitatively analyzed by gas chromatography-mass spectrometry, and quantitatively analyzed by gas chromatography. DMP Both conversion rate and DPHP selectivity 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 used for preparing higher aliphatic phthalates via ester exchange. According to the method, lower aliphatic phthalates such as dimethyl phthalate, diethyl ester, and dibutyl ester, and high alcohols such as isononyl alcohol, isodecanol, and 2-propyI-1-heptanol are taken as raw materials, one or a mixture of more than one ingredient selected from titanium potassium oxalate, aluminium titanate, potassium titanate, magnesium titanate, calcium titanate, zirconium titanite, barium titanate, aluminium trichloride, antimony trichloride, titanium tetrachloride, zirconium tetrachloride, titanium methoxide, tetra(2-propyl heptanol)titanium, tetra isononanol titamium, and tetra isodecanol titamium is taken as a catalyst; reaction is carried out for 2 to 6h at 160 to 200 DEG C; and the highest lower aliphatic phthalate conversion rate and the highest higher aliphatic phthalate selectivity are higher than 99%. The production process is clean; energy is saved; raw material storage and transportation stability is high; feeding is convenient; catalyst corrosivity is less; reaction conditions are mild; less side effect is caused; and raw material consumption is low.

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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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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