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Preparation method of neopentyl glycol dimethacrylate

A technology of neopentyl glycol dimethacrylate and methyl methacrylate is applied in the preparation of carboxylate, the preparation of organic compounds, the preparation of ester groups and hydroxyl groups, etc., which can solve the problem of low product conversion rate and catalyst price. Expensive, high production costs, to achieve the effect of shortening the reaction time, reducing the reaction cost and improving the efficiency

Active Publication Date: 2014-04-30
抚顺东联安信化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] Most of the above documents and patents are related to the esterification or transesterification of methacrylates and alcohols to prepare higher alcohol esters of methacrylates. Specifically, the transesterification of MMA and neopentyl glycol produces neopentyl dimethacrylate There is only one article on glycol esters, and the solid acid, alkali metal, and organotin catalysts mentioned in the article also have the problems of low product conversion rate, expensive catalyst price, and high production cost.

Method used

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  • Preparation method of neopentyl glycol dimethacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1200g of methyl methacrylate and 250g of neopentyl glycol were added into the reactor 1, 14.5g of sodium thiocyanate was added as a catalyst, and 2g of tetramethylpiperidinyl nitroxide radical phosphite was added as a polymerization inhibitor.

[0037] Start stirring, heat up, and when the temperature in the reactor 1 rises to 90-98°C, the top of the tower starts to discharge, full reflux, and when the temperature of the top of the tower is stable at 62-64°C, start the top reflux ratio system, and the reflux ratio is 6 : 1~6:2, by adjusting the reflux ratio, the temperature at the top of the tower is stabilized at 62~70°C. When the temperature of the kettle rises to 110~130°C, and the temperature at the top of the tower rises significantly, stop heating, cool down, and take samples for analysis .

[0038] The product in the still is 884.5g in total, and its composition is (measured by gas chromatography):

[0039] Methanol 0.05%

[0040] Methyl methacrylate 83.05%

...

Embodiment 2

[0045] 1200g of methyl methacrylate and 250g of neopentyl glycol were added into reactor 1, 14.5g of potassium carbonate was added as a catalyst, and 2g of tetramethylpiperidinyl nitroxide radical phosphite was added as a polymerization inhibitor.

[0046] Start stirring, heat up, and when the temperature in the reactor 1 rises to 90-98°C, the top of the tower starts to discharge, full reflux, and when the temperature of the top of the tower is stable at 62-64°C, start the top reflux ratio system, and the reflux ratio is 6 : 1~6:2, by adjusting the reflux ratio, the temperature at the top of the tower is stabilized at 62~70°C. When the temperature of the kettle rises to 110~130°C, and the temperature at the top of the tower rises significantly, stop heating, cool down, and take samples for analysis .

[0047] The product in the still is 1262g in total, and its composition is (measured by gas chromatography):

[0048] Methanol 0.04%

[0049] Methyl methacrylate 56.9%

[0050...

Embodiment 3

[0055] Add 1200kg methyl methacrylate and 250kg neopentyl glycol to reaction kettle 1, add 14.5kg sodium thiocyanate and potassium carbonate (mixing ratio 1:3) as catalyst, add 2kg tetramethylpiperidine nitrogen oxygen free Triphosphite as a polymerization inhibitor.

[0056] Start stirring, heat up, and when the temperature in the reactor 1 rises to 90-98°C, the top of the tower starts to discharge, full reflux, and when the temperature of the top of the tower is stable at 62-64°C, start the top reflux ratio system, and the reflux ratio is 6 : 1~6:2, by adjusting the reflux ratio, the temperature at the top of the tower is stabilized at 62~70°C. When the temperature of the kettle rises to 110~130°C, and the temperature at the top of the tower rises significantly, stop heating, cool down, and take samples for analysis .

[0057] The total product in the kettle is 1263kg, and its composition is (measured by gas chromatography):

[0058] Methanol 0.05%

[0059] Methyl methacr...

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Abstract

The invention discloses a preparation method of neopentyl glycol dimethacrylate. The preparation method comprises the following steps: reacting methyl methacrylate and neopentyl glycol used as raw materials by adopting a reaction rectification ester exchange technology in the presence of a catalyst and a polymerization inhibitor so as to obtain a reaction product containing neopentyl glycol dimethacrylate; distilling the reaction product under the condition of reduced pressure to remove excess methyl methacrylate, and then remove the catalyst and the polymerization inhibitor, thus obtaining the neopentyl glycol dimethacrylate product. The preparation method has the advantages that the carbonate and thiocyanate compound catalyst is adopted, can be recycled and has a good catalytic effect, the reaction time is shortened, the reaction efficiency is improved, and the production amount of polymers is reduced; the nitroxide free radical polymerization inhibitor is adopted, the using amount of the polymerization inhibitor is reduced, and the polymerization inhibition effect is improved.

Description

technical field [0001] The invention relates to a preparation method of chemical products, in particular to a preparation method of neopentyl glycol dimethacrylate. Background technique [0002] Neopentyl glycol dimethacrylate is a functional methacrylate, which can be used as a co-crosslinking agent for peroxidative crosslinking, and is suitable for the vulcanization system of synthetic rubber that is difficult to vulcanize with sulfur. It has the characteristics of shortening the crosslinking time and improving vulcanized rubber. It can also be used as a modifier, suitable for radiation crosslinking of PVC wires and photosensitive resins, adhesives, coatings, foam plastics, etc. [0003] The preparation methods of neopentyl glycol dimethacrylate in the prior art mainly include esterification and transesterification. [0004] TQ225.24 introduces a method for efficiently synthesizing neopentyl glycol dimethacrylate with methacrylic acid and neopentyl glycol as raw material...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/03C07C67/54
CPCC07C67/03C07C69/54
Inventor 里光
Owner 抚顺东联安信化学有限公司
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