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Modified phenolic resin capable of producing in-situ graphene and preparing method thereof

A technology of in-situ generation of phenolic resin, applied in the field of phenolic resin, can solve the problems of low yield and low yield of graphene, and achieve the effect of simple and easy control of process conditions, simple preparation method, and difficult curing

Inactive Publication Date: 2017-01-11
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the yield is low, and the yield of graphene in the pyrolytic carbon of the prepared phenolic resin is not high

Method used

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  • Modified phenolic resin capable of producing in-situ graphene and preparing method thereof
  • Modified phenolic resin capable of producing in-situ graphene and preparing method thereof
  • Modified phenolic resin capable of producing in-situ graphene and preparing method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] This embodiment discloses a preparation method of a modified phenolic resin capable of generating graphene in situ, the preparation method comprising the following preparation steps:

[0028] 1) Preparation of phenolic resin intermediate product: Mix 0.1mol of phenol, 0.07mol of formaldehyde and 0.66g of hydrochloric acid, stir evenly, keep warm at 60°C for 60min, then raise the temperature to 80°C, keep warm for 120min to obtain phenolic resin Resin intermediates;

[0029] 2) Preparation of water-containing modified phenolic resin: adjust the acidity and alkalinity of the phenolic resin intermediate product prepared in the step 1) with ammonia water to ensure that the pH is between 6.0 and 6.4, then add 0.01mol of glycine, and heat the mixture at 80°C The temperature was kept at a temperature of 30 minutes, then the temperature was lowered to 50 ° C, and 0.001 mol of copper inorganic salt was added, and the temperature was kept for 30 minutes, and then the temperature ...

Embodiment 2

[0032] This embodiment discloses a preparation method of a modified phenolic resin capable of generating graphene in situ, the preparation method comprising the following preparation steps:

[0033] 1) Preparation of phenolic resin intermediate product: Take 0.1mol of p-cresol, 0.07mol of acetaldehyde and 0.11g of oxalic acid, mix them well, stir them evenly, keep them under the condition of 70°C for 30 minutes, then raise the temperature to 100°C, and keep them for reaction 180min, obtain phenolic resin intermediate product;

[0034] 2) Preparation of water-containing modified phenolic resin: adjust the acidity and alkalinity of the phenolic resin intermediate product prepared in the step 1) with ammonia water to ensure that the pH is between 6.4 and 6.8, then add 0.001mol of iminodiacetic acid, in Insulate and react at 100°C for 60 minutes, then lower the temperature to 70°C, continue to add 0.002 mol of nickel inorganic salt, heat for 60 minutes, and then cool the temperatu...

Embodiment 3

[0037] This embodiment discloses a preparation method of a modified phenolic resin capable of generating graphene in situ, the preparation method comprising the following preparation steps:

[0038] 1) Preparation of phenolic resin intermediate product: take 0.1 mol of hydroquinone, 0.07 mol of paraformaldehyde (average relative molecular weight is 600) and 0.77 g of sulfuric acid, mix them, stir them evenly, and keep them warm for 60 minutes at 65°C. Then the temperature was raised to 90° C., and the heat preservation reaction was carried out for 120 minutes to obtain the intermediate product of phenolic resin;

[0039]2) Preparation of water-containing modified phenolic resin: adjust the acidity and alkalinity of the phenolic resin intermediate product prepared in the step 1) with ammonia water to ensure that the pH is between 6.8 and 7.2, and then add 0.01mol of nitrilotriacetic acid at 90 ℃ for 30 minutes, then lower the temperature to 50 ℃, continue to add 0.001 mol of ir...

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Abstract

Belonging to the field of phenolic resin technplogy, the invention discloses modified phenolic resin capable of producing in-situ graphene and a preparing method thereof. This preparing method produces phenolic resin intermediate by mixing phenolic compounds, aldehyde compounds and acidic catalysts, and then adjusts PH between 6. 0-8. 0 to get modified water-holding phenolic resin by adding glycine or aminopolycanboxylic acid plus transition metal ions; after vacuum heating, adding ethanol or ethylene glycol to adjust viscosity, and then finally to obtain the modified phenolic resin which can produce in-situ graphene. This preparing method is easy and with mild operation condition allowing transition metal ions to be modified onto resins without the introduction of impurities, on the promise of a high generation rate which can be 0.1wt%-10wt% of in-situ graphene produced by the modified phenolic resin in low temperature.

Description

technical field [0001] The invention belongs to the technical field of phenolic resins, in particular to a modified phenolic resin capable of generating graphene in situ and a preparation method thereof. Background technique [0002] Phenolic resin is a general term for resins produced by the reaction of phenols and aldehydes in the presence of catalysts. It is the earliest industrially produced polymer material. The cured phenolic resin has good physical and chemical properties and is widely used in industries, Agriculture, national defense and national economy and other aspects. Phenolic resin is often used to make adhesive materials, friction materials, refractory materials, laminated materials, etc. Due to the easy availability of phenolic resin raw materials, low price, simple production process and equipment requirements, it has become an indispensable tool for in-situ graphene generation. One of the raw materials. [0003] Graphene is a material in which carbon atom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28C01B32/184
CPCC08G8/28
Inventor 伍林丁建强程坚童坤程少辉陈亚桥李泽亚张琪刘盈饶文昊严柳李亚伟
Owner WUHAN UNIV OF SCI & TECH
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