Removal method for titanate from esterified product

A technology of titanate and catalyst, which is applied in the field of removal of ester substances in esterification products, can solve the problems of mechanical impurities, difficulties, and difficulty in industrial production, and achieve the goals of short filtration time, perfect production process, and shortened production cycle Effect

Inactive Publication Date: 2006-11-08
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although this method has a certain removal effect on titanate (tetrabutyl titanate) catalyst, activated clay, activated carbon and titanate (tetrabutyl titanate) need to form a filter cake and have a large viscosity. Filtration needs to be carried out under vacuum conditions; if the pilot test is carried out, press filtration is required, and it is very difficult and not easy for industrial production, and the product contains mechanical impurities, which affects product quality and its application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0018] This example is a method for removing tetrabutyl titanate remaining in the esterification product of saturated aliphatic dicarboxylic acid and higher alcohol.

[0019] Add 146.1 g of adipic acid and 255.5 g of n-hexanol into a 1000 ml four-neck flask equipped with a stirrer, a thermometer, and a condensing water separator, stir to raise the temperature, add catalyst tetrabutyl titanate 0.3 ml at 110 ° C, and reflux at 155 ° C. Water began to record time, and the esterification was completed after 5 hours of reaction.

[0020] Cool the crude product of esterification to 40°C, start decompression to remove excess n-hexanol, keep the pressure at -0.095Mpa, slowly raise the temperature to extract excess n-hexanol, about 220°C, until no n-hexanol is recovered. Cool down to 50°C under vacuum, add sodium percarbonate (2Na 2 CO 3 .3H 2 o 2 ) 5.0 g, yellow flocs appeared after stirring for 2 hours, the temperature was lowered to 20° C., the yellow flocs were filtered off und...

example 2

[0027] This example removes the method for tetrabutyl titanate in the esterification product of ortho (iso, tere) phthalate.

[0028] Add 148.0g of phthalic anhydride and 255.5g of n-hexanol into a 1000ml four-neck flask equipped with a stirrer, a thermometer, and a condensing water separator, stir to raise the temperature, add 0.3ml of catalyst tetrabutyl titanate at 110°C, and start to reflux at 155°C for water collection Timing, reaction 5 hours esterification finishes.

[0029] Cool the crude product of esterification to 40°C, start decompression to remove excess n-hexanol, keep the pressure at -0.095Mpa, slowly raise the temperature to extract excess n-hexanol, stop when there is no n-hexanol at about 220°C, and then cool down to 50°C in vacuum ℃, adding sodium percarbonate (2Na 2 CO 3 .3H 2 o 2 ) 5.0 g, yellow flocs appeared after stirring for 2 hours, the temperature was lowered to 20° C., the yellow flocs were filtered off under normal pressure, and the filtrate wa...

example 3

[0036] In the thick ester product of example 1, add sodium carbonate Na 2 CO 3 3.4 grams, 4.57 grams of hydrogen peroxide aqueous solution (35%) (containing 1.6 grams of hydrogen peroxide), kept at 50 ° C, stirred for 2 hours, yellow flocs appeared, cooled to 20 ° C, filtered off the yellow flocs under normal pressure, get the product.

[0037] Sodium carbonate (Na 2 CO 3 ) chemically pure, CNPC Jilin Petrochemical Company

[0038] Hydrogen peroxide aqueous solution (35%) chemically pure, Jilin Chemical Industry Company Reagent Factory.

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Abstract

The invention provides a method for removing the titanate catalyst in the esterification product, by adding sodium percarbonate or a mixture of sodium carbonate and hydrogen peroxide or a mixture of sodium bicarbonate and hydrogen peroxide to accelerate the hydrolysis of titanate, Complexation, the formed flocculent precipitate can be removed by normal pressure filtration, the filtration time is short, and the final esterification product obtained has no mechanical impurities. The problem that the titanate catalyst remains in the esterification product and the separation is difficult is solved, and the method improves the production process of the titanate catalyzed esterification, and can shorten the production cycle.

Description

technical field [0001] The invention relates to a method for removing ester substances in esterification products. Background technique [0002] Titanate is a colorless to light yellow liquid. It is a non-acidic esterification catalyst with excellent performance. When it is used as an esterification reaction catalyst, except for wastewater, almost no esterification by-products are produced. The obtained esterification The product quality is good, and its appearance, color, and stability are superior to those produced by the acid catalyst process, and the process using this type of catalyst has less "three wastes", and the recovered alcohol is of good quality and can be directly reused. However, titanate is easily decomposed when exposed to water, and can be dissolved in most organic solvents except ketones. Therefore, titanate is unstable in esterification products, easy to hydrolyze, and can slowly form hydrolysis intermediate product polycondensation titanate, and finally...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/60
Inventor 张成业石大川
Owner PETROCHINA CO LTD
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