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Preparation method of alkynylated cardanol phenolic resin/titanium dioxide composite material

A technology of phenolic resin and composite material, which is applied in the field of preparation of alkynylated cardanol-type phenolic resin and its composite material, can solve the problems of low shrinkage, single element, high residual rate of pyrolysis, etc., and achieve sufficient curing, The effect of reducing the existence of air bubbles and simple preparation process

Inactive Publication Date: 2014-12-03
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 4. The elements contained in the molecular structure are relatively single, the residual rate of pyrolysis is high, and the shrinkage rate is low

Method used

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  • Preparation method of alkynylated cardanol phenolic resin/titanium dioxide composite material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1. Preparation of Cardanol Phenolic Resin

[0037] The temperature of the water bath is controlled at 50°C, add 0.1mol (30g) cardanol, 0.085mol (2.53g) formaldehyde, and 0.002mol (0.60g) oxalic acid into a 250mL three-necked flask, stir, heat the water bath to 85°C, and react for 3.5 hours Neutralize with 0.1mol / L KOH aqueous solution to pH 7, then wash off unreacted cardanol, formaldehyde and catalyst with 1L of 50°C distilled water for 5 times, and remove the residual distilled water by rotary evaporation to obtain brown-red cardanol phenolic phenolic novolac resin.

[0038] 2. Preparation of alkynylated cardanol-type phenolic resin

[0039] The temperature of the water bath is controlled at 50°C, and 28g of cardanol-type phenolic resin prepared in step 1, 52.29g of n-butanol, and 0.08mol (4.48g) of potassium hydroxide are added to a 250mL three-necked flask, and then 0.12mol of (14.28g) 3-bromopropyne, the dropping time is controlled at half an hour, stirred, heate...

Embodiment 2

[0045] 1. Preparation of Cardanol Phenolic Resin

[0046]The temperature of the water bath is controlled at 50°C, add 0.1mol (30g) cardanol, 0.085mol (2.53g) formaldehyde, and 0.002mol (0.60g) oxalic acid into a 250mL three-necked flask, stir, heat the water bath to 85°C, and react for 3.5 hours Neutralize with 0.1mol / L KOH aqueous solution to pH 7, then wash off unreacted cardanol, formaldehyde and catalyst with 1L of 50°C distilled water for 5 times, and remove the residual distilled water by rotary evaporation to obtain brown-red cardanol phenolic phenolic novolac resin.

[0047] 2. Preparation of alkynylated cardanol-type phenolic resin

[0048] The temperature of the water bath is controlled at 50°C, and 28g of cardanol-type phenolic resin prepared in step 1, 52.29g of n-butanol, and 0.08mol (4.48g) of potassium hydroxide are added to a 250mL three-necked flask, and then 0.12mol of (14.28g) 3-bromopropyne, the dropping time is controlled at half an hour, stirred, heated...

Embodiment 3

[0054] 1. Preparation of Cardanol Phenolic Resin

[0055] The temperature of the water bath is controlled at 50°C, add 0.1mol (30g) cardanol, 0.085mol (2.53g) formaldehyde, and 0.002mol (0.60g) oxalic acid into a 250mL three-necked flask, stir, heat the water bath to 85°C, and react for 3.5 hours Neutralize with 0.1mol / L KOH aqueous solution to pH 7, then wash off unreacted cardanol, formaldehyde and catalyst with 1L of 50°C distilled water for 5 times, and remove the residual distilled water by rotary evaporation to obtain brown-red cardanol phenolic phenolic novolac resin.

[0056] 2. Preparation of alkynylated cardanol-type phenolic resin

[0057] The temperature of the water bath is controlled at 50°C, and 28g of cardanol-type phenolic resin prepared in step 1, 52.29g of n-butanol, and 0.08mol (4.48g) of potassium hydroxide are added to a 250mL three-necked flask, and then 0.12mol of (14.28g) 3-bromopropyne, the dropping time is controlled at half an hour, stirred, heate...

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Abstract

The invention discloses a preparation method of an alkynylated cardanol phenolic resin / titanium dioxide composite material. The preparation method is characterized by firstly reacting cardanol with formaldehyde to prepare a cardanol phenolic resin, secondly reacting the cardanol phenolic resin with 3-propargyl bromide to alkynylate the cardanol phenolic resin, and finally mixing the alkynylated cardanol phenolic resin as a prepolymer with tetrabutyl titanate and curing the mixture, thus obtaining the alkynylated cardanol phenolic resin / titanium dioxide composite material. The composite material has higher thermal decomposition temperature and mass residual rate.

Description

1. Technical field [0001] The invention relates to a preparation method of alkynylated resin and its composite material, in particular to the preparation of alkynylated cardanol-type phenolic resin and its composite material. 2. Background technology [0002] Since the 1950s, the development of high-tech such as aerospace has promoted the research on heat-resistant polymer materials, and many heat-resistant polymers have therefore been applied one after another. Alkyne-based resin (ATR) is a new type of high temperature resistant thermosetting resin. Alkyne-based resin refers to terminal alkyne oligomers or terminal alkyne compounds. Under certain conditions (such as heat, radiation, etc.), a new type of cross-linked network structure is formed by addition polymerization using the high reactivity of the alkyne group. Thermosetting resin material. Due to the excellent heat resistance and process performance of alkyne-based resin, it is expected to replace conventional pheno...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L61/14C08K3/22C08G8/30
Inventor 史铁钧吴竞郭立颖张方王启东
Owner HEFEI UNIV OF TECH