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A kind of preparation method of cyclohexyl (meth)acrylate

A technology of cyclohexyl acrylate and acrylic acid, which is applied in the field of synthesis of special acrylic acid esters through the addition and esterification of acrylic acid, which can solve the problems of long reaction time, short service life of catalysts, and high labor intensity, so as to reduce selectivity and improve selectivity , highly active effect

Active Publication Date: 2021-09-07
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yang Lei et al. In the study of the addition and esterification of acrylic acid and cyclohexene catalyzed by supported HSiW / SBA-15, Guangdong Chemical Industry, 2015, 42(1): 21-23. The kettle-type process method was used, and SBA-15 was used to support The silicotungstic acid catalyst can add and esterify acrylic acid and cyclohexene to synthesize cyclohexyl acrylate. The reaction temperature is 95°C, the reaction time is 9h, and the selectivity of cyclohexyl acrylate is 96.2%. The two synthetic process schemes are The atomic economy reaction process does not produce a large amount of waste water and waste liquid, and is environmentally friendly, but at the same time, they are all batch synthesis processes, with long reaction time, high labor intensity, short service life of the catalyst, and high production costs.

Method used

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  • A kind of preparation method of cyclohexyl (meth)acrylate
  • A kind of preparation method of cyclohexyl (meth)acrylate
  • A kind of preparation method of cyclohexyl (meth)acrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-5

[0064] The blank MCM-48 molecular sieve and the MCM-48 molecular sieve were loaded with phosphorus tungsten molybdenum vanadium zirconium heteropolyacid H 3 PW 6 Mo 4 VZrO 40 The catalyst is mixed evenly according to the dilution ratio of 2:1 (volume ratio), and then loaded into the upper section of the segmented fixed-bed tubular reactor 3, MCM-48 blank molecular sieve and MCM-48 molecular sieve phosphotungstomolybdenum vanadium zirconium heteropolyacid H 3 PW 6 Mo 4 VZrO 40 The catalyst is mixed evenly according to the dilution ratio of 1:1 (volume ratio), and then loaded into the lower section of the segmented fixed-bed tubular reactor 3, and the molar ratio of methacrylic acid and cyclohexene is added to the raw material in a ratio of 2:1. In the mixing tank 1, add the polymerization inhibitor cyclohexanol and hydroquinone to it again, the mass ratio of hydroquinone to (meth)acrylic acid is 0.005:1, and finally replenish the raw material mixing tank 1 through the firs...

Embodiment 6～10

[0068] The MCM-48 blank molecular sieve and the MCM-48 molecular sieve were loaded with phosphorus tungsten molybdenum vanadium zirconium heteropolyacid H 3 PW 6 Mo 4 VZrO 40 The catalyst is mixed evenly according to the dilution ratio of 1:1 (volume ratio), and then loaded into the lower section of the segmented fixed-bed tubular reactor 3, and the molar ratio of methacrylic acid and cyclohexene is added to the raw material in a ratio of 2:1. In the mixing tank 1, add polymerization inhibitor cyclohexanol and hydroquinone to it again, the mass ratio of hydroquinone to (meth)acrylic acid is 0.005:1, and the mass ratio of cyclohexanol to cyclohexene is 0.06 : 1, at last the raw material mixing tank 1 is supplemented with compressed air to 0.5MPaA through the first pipeline 5 and mixed uniformly, and the compressed air is supplemented to 0.5MPaA through the tenth pipeline 14 in the reaction liquid storage tank and the segmented fixed-bed reactor, Then through the diaphragm me...

Embodiment 11～15

[0072] The MCM-48 blank molecular sieve and the MCM-48 molecular sieve were loaded with phosphorus tungsten molybdenum vanadium zirconium heteropolyacid H 3 PW 6 Mo 4 VZrO 40 The catalyst is mixed evenly according to the dilution ratio of 2:1 (volume ratio), and then loaded into the upper section of the segmented fixed-bed tubular reactor 3, and the molar ratio of methacrylic acid and cyclohexene is added to the raw material in a ratio of 2:1. In the mixing tank 1, add polymerization inhibitor cyclohexanol and hydroquinone to it again, the mass ratio of hydroquinone to (meth)acrylic acid is 0.005:1, and the mass ratio of cyclohexanol to cyclohexene is 0.05 : 1, at last the raw material mixing tank 1 is supplemented with compressed air to 0.6MPaA through the first pipeline 5 and mixed uniformly, and the compressed air is supplemented to 0.6MPaA through the tenth pipeline 14 in the reaction liquid storage tank and the segmented fixed-bed reactor, Then through the diaphragm me...

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Abstract

The invention relates to a preparation method of cyclohexyl (meth)acrylate, comprising the following steps: mixing (meth)acrylic acid, cyclohexene, cyclohexanol, hydroquinone and / or derivatives thereof according to a certain proportion A segmented fixed-bed tubular reactor equipped with a molecular sieve-supported phosphorus-tungsten-molybdenum-vanadium-zirconium heteropolyacid catalyst is added to react to generate (meth)cyclohexyl acrylate. The method realizes the large-scale continuous production of cyclohexyl (meth)acrylate, the whole set of process steps is simple, continuous operation, low construction cost, no pollution, conforms to atomization economy, and at the same time, the selectivity and yield of the product are high.

Description

technical field [0001] The invention relates to a preparation method of cyclohexyl (meth)acrylate, which belongs to the field of synthesis of special esters of (meth)acrylic acid by addition esterification of acid alkenes. Background technique [0002] Cyclohexyl (meth)acrylate is a kind of acrylate with special structure. It contains cyclic groups and double bonds in its structure. It can be used as a monomer or comonomer for solution polymerization or suspension polymerization. Its polymerization products have High refractive index, excellent water resistance, abrasion resistance, chemical resistance, heat resistance, low shrinkage and high hardness, etc. Therefore, it has been widely used in automobile shells as a high-quality active crosslinking agent and diluent Coatings, solvent-based coatings, high-solid coatings, powder coatings, water-soluble resins, polymer flocculants, textile auxiliaries, petroleum depressants and medical materials, etc. [0003] Cyclohexyl (met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/04C07C67/62C07C69/54C07C69/013B01J31/18
CPCB01J27/199B01J29/0341B01J2229/18C07C67/04C07C67/62C07C2601/14C07C69/54C07C69/013
Inventor 郑京涛李晶鞠昌迅郭华黎源陆国太姜庆梅李付国程英丰茂英孙烨刘照刘岩
Owner WANHUA CHEM GRP CO LTD
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