Method for synthesizing phthalate compounds

Abstract

The invention provides a method for synthesizing phthalate compounds. By taking a weak acid as a main catalyst assisted by a composite catalyst formed by other co-catalysts, the phthalate compounds are synthesized. The method specifically comprises the following steps: adding phthalic anhydride, alcohol and the composite catalyst into a reactor, wherein the molar ratio of phthalic anhydride and alcohol is 1: (2.1-5.0) and the addition of the composite catalyst is 0.2-10wt% of phthalic anhydride; and sealing the reactor, raising the temperature till boiling, reacting for 0.5-2 hours and rectifying to obtain a product. The method not only can realize a catalytic effect of concentrated sulfuric acid, but also overcome the defects. Moreover, the used catalyst can be separated and reused by using a conventional method, so that the separating flow is greatly simplified and continuous production is facilitated.

Description

technical field

[0001] The invention belongs to the technical field of chemical synthesis, and relates to a method for synthesizing phthalates. Background technique

[0002] Phthalate, also known as phthalate, abbreviated as PAE, is a general term for esters formed by phthalic anhydride. Phthalates have excellent comprehensive processing properties, high plasticizing efficiency, low volatility, and good cold resistance, flexibility, and electrical properties. Phthalates, mainly used as plasticizers (plasticizers), are added to plastics to enhance elasticity, transparency, durability and longevity, and are widely used in a variety of products, such as pills and nutritional supplements casings, viscosity agents, gelling agents, membrane aids, stabilizers, dispersants, lubricants, binders, emulsifiers and suspending agents, etc.

[0003] When phthalates are used as plastic plasticizers, they generally refer to esters formed between phthalic acid and alcohols containing 1 to 1...

Examples

Embodiment 1

[0024] Add 50 grams of phthalic anhydride in the 250 milliliter three-necked flask with stirring, water separator and reflux condenser, the addition of n-butanol is 2.4 times of the molar number of phthalic anhydride, 0.25 grams of catalyst (by weight In percent, sodium bisulfate: tetrabutylammonium bromide: Polyethylene Glycol=10:1.0:0.1), after heating up to boiling reaction 1h, obtain the catalytic performance of this catalyst with chromatographic analysis: phthalic anhydride conversion ratio The yield of dibutyl phthalate was 99.1%, and the yield of dibutyl phthalate was 98.0%.

Embodiment 2

[0026] Add 50 grams of phthalic anhydride to a 250-milliliter three-neck flask with stirring, water separator and reflux condenser, the addition of n-butanol is 4.0 times the molar number of phthalic anhydride, and 2.0 grams of catalyst (by weight Percentage, potassium hydrogensulfate:polyethylene glycol=10:0.1), after heating up to boiling reaction 2h, obtain the catalytic performance of this catalyst with chromatographic analysis: phthalic anhydride conversion rate is 93.5%, phthalic acid di Butyl ester yield was 93.2%.

Embodiment 3

[0028] Add 50 grams of phthalic anhydride in a 250 ml three-necked flask with stirring, water separator and reflux condenser, the addition of n-butanol is 2.4 times the molar number of phthalic anhydride, 2.5 grams of catalyst (by weight Percentage, sodium bisulfate: tetrabutylammonium bromide=10:0.8), be warming up to boiling reaction after 0.5h, obtain the catalytic performance of this catalyst with chromatographic analysis: phthalic anhydride conversion rate is 94.6%, o-phthalic anhydride The yield of dibutyl dicarboxylate was 94.2%.

technical field

[0001] The invention belongs to the technical field of chemical synthesis, and relates to a method for synthesizing phthalates. Background technique

[0002] Phthalate, also known as phthalate, abbreviated as PAE, is a general term for esters formed by phthalic anhydride. Phthalates have excellent comprehensive processing properties, high plasticizing efficiency, low volatility, and good cold resistance, flexibility, and electrical properties. Phthalates, mainly used as plasticizers (plasticizers), are added to plastics to enhance elasticity, transparency, durability and longevity, and are widely used in a variety of products, such as pills and nutritional supplements casings, viscosity agents, gelling agents, membrane aids, stabilizers, dispersants, lubricants, binders, emulsifiers and suspending agents, etc.

[0003] When phthalates are used as plastic plasticizers, they generally refer to esters formed between phthalic acid and alcohols containing 1 to 1...

Examples

Embodiment 1

[0024] Add 50 grams of phthalic anhydride in the 250 milliliter three-necked flask with stirring, water separator and reflux condenser, the addition of n-butanol is 2.4 times of the molar number of phthalic anhydride, 0.25 grams of catalyst (by weight In percent, sodium bisulfate: tetrabutylammonium bromide: Polyethylene Glycol=10:1.0:0.1), after heating up to boiling reaction 1h, obtain the catalytic performance of this catalyst with chromatographic analysis: phthalic anhydride conversion ratio The yield of dibutyl phthalate was 99.1%, and the yield of dibutyl phthalate was 98.0%.

Embodiment 2

[0026] Add 50 grams of phthalic anhydride to a 250-milliliter three-neck flask with stirring, water separator and reflux condenser, the addition of n-butanol is 4.0 times the molar number of phthalic anhydride, and 2.0 grams of catalyst (by weight Percentage, potassium hydrogensulfate:polyethylene glycol=10:0.1), after heating up to boiling reaction 2h, obtain the catalytic performance of this catalyst with chromatographic analysis: phthalic anhydride conversion rate is 93.5%, phthalic acid di Butyl ester yield was 93.2%.

Embodiment 3

[0028] Add 50 grams of phthalic anhydride in a 250 ml three-necked flask with stirring, water separator and reflux condenser, the addition of n-butanol is 2.4 times the molar number of phthalic anhydride, 2.5 grams of catalyst (by weight Percentage, sodium bisulfate: tetrabutylammonium bromide=10:0.8), be warming up to boiling reaction after 0.5h, obtain the catalytic performance of this catalyst with chromatographic analysis: phthalic anhydride conversion rate is 94.6%, o-phthalic anhydride The yield of dibutyl dicarboxylate was 94.2%.

Images