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Silane-modified phenolic resin and preparation method thereof

The technology of novolac resin and phenolic resin is applied in the field of silane-modified phenolic resin and its preparation. efficiency, overcoming the effect of uneven blending and dispersion

Active Publication Date: 2016-08-24
GUANGZHOU BAIYUN CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The blending of two substances with large polarity differences will inevitably lead to uneven dispersion due to the difference in compatibility, which will eventually lead to insignificant improvement in polymer performance.

Method used

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  • Silane-modified phenolic resin and preparation method thereof
  • Silane-modified phenolic resin and preparation method thereof
  • Silane-modified phenolic resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The preparation method of the silane-modified phenolic resin of the present embodiment may further comprise the steps:

[0033] (1), preparation novolac resin

[0034] Add 188.015g (2mol) of phenol, 137.062g of 37wt% formaldehyde solution (1.7mol), 100g of distilled water, and 1.88g of oxalic acid (as a catalyst) to a 1000ml three-necked flask. React at 125°C for half an hour. After completion of the reaction, the product was poured into distilled water and washed repeatedly to remove unreacted free phenol and formaldehyde, and the catalyst, and further remove small molecules in vacuum to obtain a translucent viscous fluid with a viscosity of 2100cp, which is novolac resin (203.179g ), hydroxyl equivalent 107, molecular weight Mn=1560, molecular weight distribution d=1.67;

[0035] (2), prepare Schiff base trialkoxysilane

[0036] 44.231g γ-aminopropyltriethoxysilane (0.2mol), 12.017g paraformaldehyde (0.4mol), 150ml chloroform, and 10g CaH 2 , reacted under vigorou...

Embodiment 2

[0050] The preparation method of the silane-modified phenolic resin of the present embodiment may further comprise the steps:

[0051] (1), preparation novolac resin

[0052] Add 94.067g (1mol) of phenol, 64.916g of 37wt% formaldehyde solution (0.8mol), 50g of distilled water, and 0.9516g of oxalic acid into a 500m three-necked flask. half an hour. After completion of the reaction, the product was poured into distilled water and washed repeatedly to remove unreacted free phenol and formaldehyde, and the catalyst, and further remove small molecules in vacuum to obtain a translucent viscous fluid with a viscosity of 700 cp, which is novolac resin (102.601g ), hydroxyl equivalent 109, molecular weight Mn=950, molecular weight distribution d=1.27;

[0053] (2), prepare Schiff base trialkoxysilane

[0054] 35.858g γ-aminopropyltrimethoxysilane (0.2mol), 12.017g paraformaldehyde (0.4mol), 150ml toluene, and 10g CaH 2 , reacted under vigorous stirring in a 500ml three-necked flas...

Embodiment 3

[0068] The preparation method of the silane-modified phenolic resin of the present embodiment may further comprise the steps:

[0069] (1), preparation novolak resin

[0070] Add 376.268g (4mol) of phenol, 292.013g of 37wt% formaldehyde solution (3.598mol), 50g of distilled water, and 3.636g of oxalic acid to a 2000m three-necked flask. half an hour. After completion of the reaction, the product was poured into distilled water and washed repeatedly to remove unreacted free phenol and formaldehyde, and the catalyst, and further remove small molecules in vacuum to obtain a translucent viscous fluid with a viscosity of 5100 cp, which is novolac resin (418.528g ), hydroxyl equivalent 108, molecular weight Mn=3700, molecular weight distribution d=1.57;

[0071] (2), prepare Schiff base trialkoxysilane

[0072] 44.206g γ-aminopropyltriethoxysilane (0.2mol), 12.099g paraformaldehyde (0.2mol), 150ml dichloromethane, and 15g CaH 2 , reacted under vigorous stirring in a 1000ml three...

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Abstract

The invention discloses silane modified phenolic resin and a preparation method thereof. The silane modified phenolic resin has the chemical structural formula (I) as shown in the specification. In the formula, n ranges from 10 to 2000, and R is methyl or ethyl. The preparation method comprises the following three steps: I, preparing linear phenolic resin, wherein the hydroxyl equivalent is 104-109; II, enabling gamma-amino-hydrocarbon siloxane and paraformaldehyde to react so as to obtain Schiff alkali trialkoxysilane; III, enabling Schiff alkali trialkoxysilane and the linear phenolic resin to be subjected to Mannich reaction so as to form a loop, so as to obtain the silane modified linear phenolic resin. The silane modified phenolic resin has remarkable effects in improving the temperature and wet resistance of phenolic resin and improving the mechanical strength, the wearing resistance and the acid-alkali resistance of a silicone sealant.

Description

technical field [0001] The invention belongs to the field of phenolic resins, in particular, the invention relates to a silane-modified phenolic resin and a preparation method thereof. Background technique [0002] Phenolic resin is the earliest industrialized synthetic resin in the world. After more than 100 years of history, phenolic resin is characterized by low price, heat resistance, ablation resistance, flame retardancy, and less combustion smoke. It is widely used as molding compound, Crosslinking agent, coating, etc. However, the phenolic hydroxyl group and methylene group on the phenolic resin structure are easily oxidized, and the heat resistance is affected. In addition, because a large number of phenolic hydroxyl groups in the phenolic resin do not form a saturated hydrogen bond network, the phenolic resin shows high hygroscopicity in many applications. The biggest disadvantage of the phenolic resin when used as an electronic material is its large Water absorpt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/28C08G8/10
Inventor 付子恩陈建军陈何国刘光华黄恒超
Owner GUANGZHOU BAIYUN CHEM IND
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