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Epoxy resin catalytic refining process

An epoxy resin, catalytic refining technology, applied in the production field of epoxy resin, can solve the problems of reducing the resin yield, many side reactions, increasing the consumption of sodium hydroxide, etc., to achieve the effect of reducing consumption and improving yield

Active Publication Date: 2008-05-14
NANTONG XINGCHEN SYNTHETIC MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to obtain products with lower organic chlorine, the common practice is to increase the amount and concentration of sodium hydroxide added for the second time, but after the concentration and amount of sodium hydroxide increase, there will be more side reactions. The epoxy resin that has completed the reaction further reacts to generate higher molecular weight resin, and this resin is insoluble in toluene, forms a kind of aging resin that is insoluble in water and toluene, reduces resin yield; dosage, the consumption of sodium hydroxide also increased

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] A catalytic refining process for epoxy resin, the preparation steps of which are: feeding bisphenol A and epichlorohydrin in a mass ratio of 1:1.0-1.2, adjusting the temperature to 55-65°C under the condition of 19-24Kpa, adding sodium hydroxide, The amount of addition is 166kg / ton of theoretical resin output. Distill excess epichlorohydrin after reacting for 3 to 5 hours to obtain semi-finished epoxy resin; add benzyl triethyl with a theoretical mass of 4.0 to 5.0‰ to the semi-finished epoxy resin. Ammonium chloride is used as a catalyst, and the amount of sodium hydroxide is calculated according to organic chlorine. The calculation formula is sodium hydroxide quality=semi-finished organic chlorine × 400 × resin theoretical yield × (1.1~3.5), and the above sodium hydroxide is made into 12~ Add the solution of 15% mass concentration to the semi-finished epoxy resin, then add solvent toluene to 90-110% of the mass obtained according to the resin theory, react at 79-83°C f...

Embodiment 2

[0008] Embodiment 2: (contrast with embodiment 3)

[0009] When producing WSR6101 (epoxy value is 0.41-0.47eq / 100g bisphenol A epoxy resin, the same below), the organic chlorine index of the material after recycling epichlorohydrin is 0.10-0.12eq / 100g, and the amount of sodium hydroxide added is according to 58kg (100%, calculation method of alkali amount: semi-finished organic chlorine × 400 × resin theoretical yield × coefficient, the same below; the coefficient is 1.32) / ton of resin output, the mass concentration is 12-13% solution, without solvent toluene React with a catalyst at 89-95°C for 2-3 hours, and the finished organic chlorine is 0.0064eq / 100g. Semi-finished organic chlorine refers to the equivalent number of organic chlorine atoms per 100 grams of semi-finished resin, unit: eq / 100g.

Embodiment 3

[0011] When producing WSR6101, bisphenol A and epichlorohydrin are fed in a mass ratio of 1:1.1, and the temperature is adjusted to 55-65°C under the condition of absolute pressure of 19-24Kpa, and the first part of sodium hydroxide is added: 166kg / t resin output, 3- After 5 hours of reaction, the excess epichlorohydrin was distilled, and the organic chlorine index of the material was 0.10-0.12eq / 100g, and the amount of sodium hydroxide added: by 48kg / ton of resin (the coefficient was 1.1), the mass concentration of the compound was 12-13%. Solution, add benzyltriethylammonium chloride according to 0.45% of the resin output, without adding solvent toluene, react at 89-95°C for 2-3 hours; add solvent to dissolve the resin according to the resin output ratio of 1:2, and wash with water Remove the sodium chloride and excess sodium hydroxide in the product; then evaporate the solvent to obtain the finished product, the finished product organic chlorine 0.0063eq / 100g.

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Abstract

The invention relates to a catalytic refining process of the epoxy resin, comprising following preparation steps: feeding according to mass ratio of the bisphenol A to the epichlorohydrin ranges from 1:1.0 to 1:1.2; adjusting the temperature to 55 DEG C to 65 DEG C under 19KPa to 14KPa and adding sodium hydroxide and resin of 166kg per ton theoretical yield; after 3 to 5 hours reaction, distilling the excessive epichlorohydrin to obtain semi-finished expoxy resin; adding benzyl triethyl ammonium chloride of 4.0 per mill to 5.0 per mill of the theoretical mass of the resin as catalyst. The quantity of sodium hydroxide added is calculated according to the organochlorine; the formula is: mass of sodium hydroxide is equal to semi finished organochlorine timing 400 timing the theoretical yield of resin timing 1.1 to 3.5; preparing the sodium hydroxide into the solution with concentration ranging from 12 per cent to 15 per cent and adding the semi-finished epoxy resin; adding solvent toluene of 90 per cent to 110 per cent of the resin theoretical mass; after 2 to 4 hours reaction, washing and removing the solvent to get epoxy resin.

Description

1. Technical field [0001] The invention belongs to the technical field of epoxy resin production, in particular to a catalytic refining process of epoxy resin. 2. Background technology [0002] Prior art: After recovering excessive epichlorohydrin, the low molecular weight epoxy resin will be refined by adding sodium hydroxide to reduce organic chlorine (hydrolyzed chlorine). In general practice, more sodium hydroxide must be added for lower organic chlorine, but adding more sodium hydroxide will increase the consumption of sodium hydroxide, increase the aging resin and reduce the yield. When producing WSR6101, after the excess epichlorohydrin and bisphenol A are slightly dissolved, adjust the temperature to 55-65°C, add the first part of sodium hydroxide (75-90% of the theoretical sodium hydroxide amount), and react for 3-5 hours At the end, epichlorohydrin is recovered by distillation, because the amount of sodium hydroxide added for the first time is only 75-90% of the t...

Claims

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Application Information

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IPC IPC(8): C08G59/06
Inventor 吴俊江秀明
Owner NANTONG XINGCHEN SYNTHETIC MATERIAL
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