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Circular type esterification reaction polymer catalyst and preparation method and application thereof

A technology of esterification reaction and catalyst, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, carboxylate preparation, etc. It can solve the problems of limited number of effective catalysis, limited fixation effect, high toxicity, etc., and achieve good catalysis effect of effect

Inactive Publication Date: 2009-12-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the former, because the catalyst is adsorbed on the carrier, its immobilization effect is limited, and the catalyst is relatively easy to get out of it, so the number of times it can achieve effective catalysis is very limited, while the price and synthesis process of the latter are complicated. The degree is relatively high, and it mostly uses noble metal ions as the center ion, and its toxicity is also relatively high, so its application prospect is poor

Method used

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  • Circular type esterification reaction polymer catalyst and preparation method and application thereof
  • Circular type esterification reaction polymer catalyst and preparation method and application thereof
  • Circular type esterification reaction polymer catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1: Dispersion polymerization method

[0024] (1) Under the protection of nitrogen, add 2.58 g of sodium styrene sulfonate and 1.08 g of vinyl acetate into a three-necked flask containing 100 mL of dimethyl sulfoxide reaction solvent, and then add 0.0183 g of divinylbenzene Crosslinking agent, 0.0037g initiator benzoyl peroxide and 0.02g polyvinylpyrrolidone as dispersants, and then polymerized at 100℃ with stirring for 2 hours to obtain the dispersion of crosslinked polymer microspheres The system is centrifuged to obtain white solid microspheres of cross-linked polymer.

[0025] (2) Soak the above cross-linked polymer microspheres in saturated saline with twice the volume of the processed cross-linked polymer microspheres for 12 hours, rinse with water for 3 times, and then use 2% sodium hydroxide by mass Soak the solution for 6 hours, rinse the cross-linked polymer microspheres until the drained water is close to neutral, and then soak for 8 hours with a 3% hydroc...

Embodiment 2

[0028] Example 2: Dispersion polymerization method

[0029] (1) Under the protection of nitrogen, add 25.75g of sodium styrene sulfonate and 10.75g of vinyl acetate into a three-necked flask containing 100mL of N-methylpyrrolidone reaction solvent, and then add 5.47g of diethylene glycols Diacrylate (DEGDA) crosslinking agent, 3.65g initiator azobisisobutyronitrile and 2.92g polyvinylpyrrolidone as dispersants, and then polymerize at 80°C for 6 hours with stirring to obtain crosslinking The dispersion system of linked polymer microspheres is centrifuged to obtain white solid microspheres of crosslinked polymer.

[0030] (2) Soak the above cross-linked polymer microspheres in saturated saline with twice the volume of the processed cross-linked polymer microspheres for 20 hours, rinse with water for 5 times, and then use sodium hydroxide with a mass concentration of 10%. Soak the solution for 3 hours, rinse the cross-linked polymer microspheres until the drained water is close to neut...

Embodiment 3

[0032] Example 3: Dispersion polymerization method

[0033] (1) Under the protection of nitrogen, add 5.15g of sodium styrene sulfonate and 2.15g of vinyl acetate into a three-necked flask containing 100mL of N-methylpyrrolidone reaction solvent, and then add 1.09g of polyethylene glycol (600 ) Acrylate (PEG(600)DA) crosslinking agent, 0.73g initiator lauryl peroxide and 5.60g hydroxymethyl cellulose as dispersant, and then polymerize at 110°C with stirring After 4 hours, a dispersion system of cross-linked polymer microspheres was obtained, and then centrifuged to obtain white solid microspheres of cross-linked polymer.

[0034] (2) Soak the above cross-linked polymer microspheres in saturated saline with twice the volume of the processed cross-linked polymer microspheres for 16 hours, rinse with water for 4 times, and then use sodium hydroxide with a mass concentration of 6%. Soak the solution for 5 hours, rinse the cross-linked polymer microspheres until the drained water is cl...

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Abstract

The invention relates to a circular type esterification reaction polymer catalyst, belonging to the field of environmentally friendly macromolecule; the solid macromolecule obtained by synthesis can not only serve as catalyst which can be applied to esterification reaction but also achieve the purposes of recycling and easy separation. The polymer catalyst has the structural formula as shown in the right, wherein f, m is any integer from 1 to 1000, R1 is selected from -C6H4-,-COO(CH2CH2O)nOCO-,-COO(CH2CHCH3O)nOCO- or -COOCH2CH2OCOC6H4COOCH2CH2OCO-, and n is any integer from 2 to 10. R2 is selected from -H or -CH3, R3 is selected from -OCOCH3, -COOCH2C2H3O, -COOR4 or -COOR5OH, and R4 and R5 are both alkyl groups with 1-12 carbon atoms.

Description

Technical field [0001] The invention belongs to the environment-friendly polymer and its application field. Background technique [0002] Carboxylate is an important organic compound. It can be used not only as a raw material for organic synthesis, but also an important fine chemical product. It is widely used in perfumes, daily chemicals, food, medicine, rubber, coatings and other industries. However, in the preparation process of these ester compounds, the esterification reaction between the hydroxyl-containing compound and the carboxylic acid is an indispensable step. In this reaction process, a catalyst is necessary. But because the esterification reaction is a highly reversible reaction, if there is no suitable catalyst to participate, the reaction speed is very slow. From the analysis of its reaction mechanism, acidic or basic compounds can play a catalytic role, but Acidic compounds are generally used in actual production, such as concentrated sulfuric acid and p-toluenesu...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J37/00C08F2/14C08F2/16C08F218/08C08F220/18C08F220/32C08F220/14C07C67/08C07C69/54C07C69/24
Inventor 聂俊梁鹏总何勇
Owner BEIJING UNIV OF CHEM TECH
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