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Preparation method of pentaerythritol triallyl ether

A technology of pentaerythritol triallyl ether and pentaerythritol, which is applied in the field of synthesis of pentaerythritol triallyl ether, can solve problems such as difficult operation and large investment in equipment, and achieve the effect of avoiding high-pressure operation

Active Publication Date: 2020-05-19
ZHUHAI SMOOTHWAY ELECTRONICS MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005]Nanjing Weier Chemical Co., Ltd. patent CN100410304C chooses water as the solvent to synthesize under the pressure of 0.2MPa to reduce the by-products and improve the selectivity. Due to the use of a pressurized device for reaction, there is equipment investment large, difficult to operate

Method used

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Examples

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preparation example Construction

[0021] A preparation method of pentaerythritol triallyl ether, comprising the following steps:

[0022] S1: Under normal pressure conditions, put the solid raw material pentaerythritol, the solvent pentaerythritol triallyl ether, the phase transfer catalyst tetrabutylammonium bromide, and the raw material sodium hydroxide 50% aqueous solution into the stirring reactor according to a certain proportion, and heat up to 90-100 °C to completely dissolve the pentaerythritol into a liquid.

[0023] S2: Add the raw material allyl chloride dropwise, maintain the reaction temperature at 95-105°C, and keep the allyl chloride and water continuously distilled out. After condensation, the allyl chloride and water are separated, and the allyl chloride is returned to the stirring reactor, and the feeding of the allyl chloride is controlled according to the water separation. speed, keep the reaction for 10-16 hours.

[0024] S3: Add a certain amount of water after the reaction, lower the tem...

Embodiment 1

[0036] Raw materials and dosage:

[0037] Pentaerythritol (>98%) 100g

[0038] Sodium hydroxide aqueous solution (50%) 190g

[0039] Pentaerythritol triallyl ether 10g

[0040] Allyl chloride 150g

[0041] Tetrabutylammonium bromide 3g

[0042] In a four-neck flask equipped with reflux condenser, stirrer, thermometer and dropping funnel, drop into pentaerythritol, aqueous sodium hydroxide solution (50%), pentaerythritol triallyl ether, tetrabutylammonium bromide respectively, Heat and stir to raise the temperature to 90°C until the pentaerythritol is completely dissolved into a liquid, start to add 150 g of allyl chloride dropwise, control the dropping speed slowly, and complete the dropwise addition in about 3 hours; layer of water; pay attention to observe the reaction temperature, the temperature rises to 110 ° C, continue to reflux for 1 hour to stop the reaction.

[0043] Add 50 g of collected water to the reacted mixture, stir evenly and then let stand to separate l...

Embodiment 2

[0045] Raw materials and dosage:

[0046] Pentaerythritol (>98%) 100g

[0047] Sodium hydroxide aqueous solution (50%) 220g

[0048] Pentaerythritol triallyl ether 12g

[0049] Allyl chloride 200g

[0050] Tetrabutylammonium bromide 5g

[0051] Process is the same as example 1, obtains product 167g; Wherein pentaerythritol diallyl ether content 3.28%, pentaerythritol triallyl ether content 84.76%, pentaerythritol tetraallyl ether content 11.04%, total ether content 99.08%; With pentaerythritol as The standard molar yield is 88.7%.

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Abstract

The invention provides a preparation method of pentaerythritol triallyl ether and particularly relates to the technical field of synthesis of pentaerythritol triallyl ether. The method is characterized by comprising the following steps: S1, under normal pressure, feeding pentaerythritol, pentaerythritol triallyl ether, tetrabutylammonium bromide and 50% sodium hydroxide aqueous solution into a stirring reaction kettle, and heating the mixture to dissolve pentaerythritol into liquid; S2, dropwise adding chloropropene, keeping chloropropene and water evaporated, and layering the chloropropene and water after condensation, and returning chloropropene to the stirring reaction kettle; and S3, after the reaction is finished, adding water, and cooling and standing the mixture for layering, and carrying out reduced pressure distillation on the upper organic phase to obtain the product pentaerythritol triallyl ether. According to the preparation method of pentaerythritol triallyl ether providedby the invention, pentaerythritol triallyl ether is adopted as a solvent during synthesis, the addition of an inert solvent in the existing process is optimized and removed, rectification recycling or environment-friendly treatment measures of the inert solvent are not needed, and high-pressure operation of taking water as the solvent is avoided, so that the reaction is beneficial to the generation of pentaerythritol triallyl ether.

Description

[technical field] [0001] The invention relates to a method for synthesizing polyol allyl ether compounds, in particular to the synthesis of pentaerythritol triallyl ether. [Background technique] [0002] Pentaerythritol triallyl ether has 3 allyl groups and 1 hydroxyl group, has the properties of isomerization, oxygen binding and polymerization, and is used as a polymer monomer or crosslinking agent to prepare acrylic polymers Type thickener and superabsorbent resin, improve the salt resistance of superabsorbent resin, its grafted improved unsaturated polyester, polyurethane resin, epoxy resin and UV curable resin can reduce and eliminate the effect of oxygen inhibition, to achieve air The application of photocuring in the field of chemical green low-carbon coatings is increasing year by year, and it is an important class of organic compounds. [0003] At present, the industrial preparation of pentaerythritol triallyl ether adopts the Williamson etherification reaction. Thi...

Claims

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Application Information

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IPC IPC(8): C07C43/178C07C41/01
CPCC07C41/01C07C43/1785
Inventor 徐辑亮韩晖毛冲陈宏佳
Owner ZHUHAI SMOOTHWAY ELECTRONICS MATERIALS
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