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 alkynyl-containing cardanol-type phenolic resin and its composite material, can solve the problems of low shrinkage rate, high residual rate of pyrolysis, single element, etc., and achieves sufficient curing. , the effect of reducing the existence of bubbles and the simple preparation process

Inactive Publication Date: 2013-11-20
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

Examples

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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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
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