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Preparation method of phthalic acid esters

A technology of phthalic acid ester and phthalic anhydride, which is applied in the field of preparation of phthalic acid ester, can solve the problems of difficult separation, environmental pollution, difficult industrial realization, etc., and can reduce the reaction temperature and shorten the reaction time. effect of time, high reaction selectivity

Inactive Publication Date: 2013-12-11
ZHEJIANG HUANGMA TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] "Journal of Beijing Institute of Petrochemical Technology" reported that Liu Xia and others used sodium bisulfate as a catalyst to synthesize diisooctyl phthalate, and used xylene as a water-carrying agent. Xylene is a toxic solvent and pollutes the environment.
"Journal of Lanzhou University of Technology" reported Li Jizhong's synthesis of di-octyl phthalate and di-n-octyl phthalate, using toxic solvent toluene with water, although the equipment is less corrosive and easy to operate, but it pollutes the environment It cannot be ignored, and it is also very harmful to the operator's body
"Chemical Reagents" has reported Liu Xia's method of synthesizing diisooctyl phthalate by transesterification, but it brings troubles in the separation of methanol and isooctyl alcohol, which is difficult to realize industrially.
"Western Leather" reported that Zhang Rongli's solid QR catalyst catalyzes the production process of dioctyl phthalate. The ratio of alcohol to acid is 2.5:1. When the reaction starts, there is more water and alcohol, and the water will be divided in time. However, there is not much alcohol left after the water is reduced, and it is difficult to separate the water in time. A small amount of alcohol is difficult to bring out the water in time, and the reaction is difficult to proceed.
"Journal of Natural Sciences of Hunan Normal University" reported that in Li Juren's non-acid solid catalyzed synthesis of di-octyl phthalate, the amount of octanol is insufficient, and the esterification rate of phthalic anhydride is difficult to reach 99.0 within a certain period of time. %above

Method used

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  • Preparation method of phthalic acid esters
  • Preparation method of phthalic acid esters
  • Preparation method of phthalic acid esters

Examples

Experimental program
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Embodiment 1

[0022] A kind of preparation method of phthalic acid ester of the present embodiment comprises the following steps: 1) esterification reaction: add 148kg phthalic anhydride, 390kg isooctyl alcohol (phthalic anhydride and phthalic anhydride and The molar ratio of iso-octanol is 1:3.0), add 0.2152kg (0.4‰ of the total weight of phthalic anhydride and iso-octanol) of non-acid catalyst stannous chloride, blow nitrogen, start stirring, and heat up to 140°C-150°C, react under reflux for 1 hour, 2) then raise the temperature to 180°C-190°C, react under reflux for 2 hours to obtain the crude esterified product, and use the neutralization titration method to determine the acid value of the crude esterified product 0.05mgKOH / g; the esterification rate of phthalic anhydride is 99.98% 3) dealcoholization treatment: cool down the esterified crude product obtained in step 2) to 150°C, dealcoholize under vacuum ≤ -0.098MPa for 1h, Cool down to 100°C, decolorize with activated carbon for 1 ho...

Embodiment 2

[0026] The preparation method of a kind of phthalic acid ester of present embodiment comprises the following steps: 1) Esterification reaction: add 148kg phthalic anhydride, 403kg normal C8 alcohol (phthalic anhydride and normal The molar ratio of C8 alcohol is 1:3.1), add 0.2204kg (0.4‰ of the total weight of phthalic anhydride and n-C8 alcohol) of non-acid catalyst stannous oxide, blow nitrogen, start stirring, and raise the temperature to 130℃~ 140°C, react under reflux for 1 hour, 2) then raise the temperature to 170°C ~ 180°C, react under reflux for 2 hours to obtain the crude esterified product, and measure the acid value of the crude esterified product by neutralization titration method: 0.06mgKOH / g, the esterification rate of phthalic anhydride is 99.97% 3) dealcoholization treatment: cool down the esterification crude product obtained in step 2) to 160°C, dealcoholize under vacuum ≤ -0.098MPa for 2h, and cool down to 100 °C, decolorize with activated carbon for 1 hou...

Embodiment 3

[0030] A kind of preparation method of phthalic acid ester of the present embodiment comprises the following steps: 1) esterification reaction: add 148kg phthalic anhydride, 503kg isodecyl alcohol (phthalic anhydride and phthalic anhydride and The molar ratio of isodecyl alcohol is 1:3.2), add 0.3255kg (the amount is 0.5‰ of the total weight of phthalic anhydride and isodecyl alcohol) of non-acid catalyst stannous chloride, blow nitrogen, start stirring, and heat up to 140°C-150°C, react under reflux for 1 hour, 2) then raise the temperature to 190°C-200°C, react under reflux for 3 hours to obtain the crude esterified product, and use the neutralization titration method to determine the acid value of the crude esterified product is 0.04mgKOH / g, and the esterification rate of phthalic anhydride is 99.98%. Decolorize with activated carbon for 1 hour at 100°C, cool down and filter to obtain the product diisodecyl phthalate.

[0031] The ester content of the diisodecyl phthalate ...

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Abstract

The invention discloses a preparation method of phthalic acid esters, which is characterized by comprising the following steps: performing esterification reaction under the action of a non-acid catalyst by using phthalic anhydride and monohydric C<4-15> fatty alcohol as raw materials, then performing dealcoholization and decolouration, and finally filtering to obtain the phthalic acid esters. With the adoption of the preparation method, the production process is simplified and the impurity of the product is improved.

Description

technical field [0001] The invention relates to a preparation method of phthalic acid ester, which belongs to the technical field of synthesis of ester compounds in organic chemistry. Background technique [0002] Phthalate, also known as phthalate, abbreviated as PAE, is a general term for esters formed by phthalic anhydride. When used as a plastic plasticizer, it generally refers to the ester of phthalic acid and alcohols with 4 to 15 carbons. Among them, dioctyl phthalate is the most important species. Phthalates are a class of chemicals that act as softeners. It is commonly used in hundreds of products including vinyl flooring, wallpaper, cleaners, nail polish, sprays, shampoos and body washes. Phthalates have excellent comprehensive processing properties, high plasticizing efficiency, low volatility, and good cold resistance, flexibility, and electrical properties. It is mainly used as a plasticizer for polyvinyl chloride, vinyl chloride copolymer and cellulose resi...

Claims

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Application Information

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IPC IPC(8): C07C69/80C07C67/08
Inventor 刘志湘王胜利万庆梅金一丰谢专
Owner ZHEJIANG HUANGMA TECH