Method for preparing methoxyethyl acrylate and methoxyethyl methacrylate

A technology of methoxyethyl methacrylate and methoxyethyl acrylate, which is applied in the field of chemical product preparation, can solve problems such as a large amount of waste water, troublesome post-treatment, poor product quality, etc., so as to improve use efficiency and reduce recycling Equipment, the effect of content reduction

Active Publication Date: 2013-01-02
苏州和创化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This patent also needs to go through processes such as alkaline water washing and desolventization. The process flow is complicated, and it is all batch production, which is not suitable for large-scale industrial production. The water content of the product produced by the esterification method is also high, and the product quality is poor.
[0004] Chinese patent 200810053581.X introduces a method for preparing methoxyethyl (meth)acrylate by esterification, using water washing instead of decompression refining, and adding an adsorbent to deactivate methoxyethyl (meth)acrylate Adsorption separation of monomers and dimers of esters, where the adsorption process takes one day, the post-treatment efficiency is low, and it is not suitable for large-scale production
[0005] Chinese patent 200810053579.2 introduces the post-esterification treatment process, which uses a three-step washing process, first using salt water, then using alkaline water, and finally adding water washing, which not only produces a large amount of waste water, but also consumes salt and alkali
[0006] Chinese patent 201110242202.3 introduces a

Method used

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  • Method for preparing methoxyethyl acrylate and methoxyethyl methacrylate
  • Method for preparing methoxyethyl acrylate and methoxyethyl methacrylate
  • Method for preparing methoxyethyl acrylate and methoxyethyl methacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 5 liters of reactor, the rectification tower on the reactor is Φ50×2.5mm, and the height of the tower is 1000mm.

[0044] The catalyst is dibutyltin sulfide, and the polymerization inhibitor is poly{[6-[(1,1,3,3-tetramethylbutyl)amino]]-1,3,5-triazine-2,4-bis [(2,2,6,6,-tetramethyl-piperidinyl)imino]-1,6-hexanediamine[(2,2,6,6-tetramethyl-4-piperidinyl) Imino]}, the entrainer is n-hexane.

[0045] In the reactor, 2451 g of methyl acrylate and 1444 g of ethylene glycol-methyl ether were added according to the weight ratio of substances of 1.5:1, 78 g of catalyst and 7.8 g of polymerization inhibitor were added.

[0046] The reaction kettle is heated up, and when the bottom temperature of the rectification column on the reaction kettle rises to 50°C, the top reflux pump of the rectification tower is turned on, and the entrainer is refluxed according to a certain flow rate. The top temperature was 49°C. After 6 hours of reaction, the temperature of the reactor was 110°C....

Embodiment 2

[0051] 5 liters of reactor, the rectification tower on the reactor is Φ50×2.5mm, and the height of the tower is 1000mm.

[0052] The catalyst is dibutyltin sulfide, and the polymerization inhibitor is poly{[6-[(1,1,3,3-tetramethylbutyl)amino]]-1,3,5-triazine-2,4-bis [(2,2,6,6,-tetramethyl-piperidinyl)imino]-1,6-hexanediamine[(2,2,6,6-tetramethyl-4-piperidinyl) A compound of imino]} and polysuccinic acid (4-hydroxy-2,2,6,6-tetramethyl-1-piperidine ethanol) ester, the mass ratio of the two is 1:3, and the entrainer for cyclohexane.

[0053] In the reactor, 2451 g of methyl acrylate and 1444 g of ethylene glycol-methyl ether were added according to the weight ratio of substances of 1.5:1, 78 g of catalyst and 7.8 g of polymerization inhibitor were added.

[0054] The reaction kettle is heated up, and when the bottom temperature of the rectification column on the reaction kettle rises to 50°C, the top reflux pump of the rectification tower is turned on, and the entrainer is refl...

Embodiment 3

[0058] 5 liters of reactor, the rectification tower on the reactor is Φ50×2.5mm, and the height of the tower is 1000mm.

[0059] The catalyst is a compound of dibutyl tin oxide and tetrabutyl titanate, the mass ratio of the two is 3:1, and the polymerization inhibitor is poly{[6-[(1,1,3,3-tetramethylbutyl Base)amino]]-1,3,5-triazine-2,4-bis[(2,2,6,6,-tetramethyl-piperidinyl)imino]-1,6-hexanediamine [(2,2,6,6-tetramethyl-4-piperidinyl)imino]} and polysuccinic acid (4-hydroxy-2,2,6,6-tetramethyl-1-piperidine ethanol) ester compound, the mass ratio of the two is 1:3, and the entrainer is methylcyclohexane.

[0060] In the reactor, 2451 g of methyl acrylate and 1444 g of ethylene glycol-methyl ether were added according to the weight ratio of substances of 1.5:1, 78 g of catalyst and 7.8 g of polymerization inhibitor were added.

[0061] The reaction kettle is heated up, and when the bottom temperature of the rectification column on the reaction kettle rises to 50°C, the top ref...

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Abstract

Disclosed is a method for preparing (methyl) methoxyethyl acrylate. The method includes that an integrated device with a reacting kettle on the lower portion and a rectifying tower on the upper portion is utilized, (methyl) methyl acrylate and glycol-methyl ether are used as raw materials, the raw materials are heated and reacted in the reacting kettle under the action of catalysts and polymerization inhibitors to generate the (methyl) methoxyethyl acrylate, and then the separation and purification are performed to obtain the product. According to the method, a reactive distillation and azeotropic distillation coupling technology is utilized, the reactive distillation and the azeotropic distillation are performed in the same tower, the equipment investment is reduced, the energy consumption is reduced, the material ratio is lowered, the reaction time is shortened, and the efficiency of a reactor is improved; an ester exchange process is utilized, so that the waste water can not be generated, and the highly purified (methyl) methoxyethyl acrylate can be obtained after separation; composite catalysts are utilized, so that the reacting efficiency is increased, the reaction time is shortened, and the quantity of generated polymers is lowered; and the novel polymerization inhibitors are utilized, so that the chromaticity of the product is improved.

Description

technical field [0001] The invention relates to a preparation method of chemical products, in particular to a preparation method of methoxyethyl acrylate and methoxyethyl methacrylate. Background technique [0002] Methoxyethyl acrylate or methoxyethyl methacrylate has high temperature resistance and oil resistance, so that it can be used as a comonomer of polyacrylic acid elastomer, an important monomer for the manufacture of low temperature and ultra low temperature resistant acrylate rubber, It is a comonomer for the manufacture of coating resins, and can also be used as barrier coatings and adhesives, PVC impact modifiers, and contact lenses. Its copolymer provides good adhesion, chemical resistance, elasticity, high impact resistance, weather resistance and low shrinkage, and is a good reactive diluent for light curing. [0003] Chinese patent 200810053582.4 describes the preparation process of methoxyethyl (meth)acrylate, which uses acrylic acid and ethylene glycol-me...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/03C07C67/54
CPCY02P20/10
Inventor 安丰发李虹
Owner 苏州和创化学有限公司
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