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Preparation method of modified phenolic resin adhesive

A technology for phenolic resins and adhesives, applied in adhesives, aldehyde/ketone condensation polymer adhesives, adhesive types, etc., can solve problems such as high curing temperature, reduction of free phenol content, reduction of hot pressing temperature of phenolic resin adhesives, etc. , to achieve the effect of improving heat resistance and bonding strength, increasing bonding strength, and improving reactivity

Inactive Publication Date: 2013-05-01
JIANGSU HUAYUAN MINING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Phenolic resin (PF) adhesives are widely used in the wood industry. Phenolic resin adhesives have the advantages of high bonding strength, water resistance, heat resistance, wear resistance and good chemical stability. But the phenolic resin adhesive itself also has shortcomings, such as the nature and structure of the phenolic resin adhesive determines that its curing temperature is higher, the curing speed is slower, especially the cost of phenolic resin is relatively high, and the existence of free formaldehyde and free phenol leads to its environmental pollution. The hazards are greater, which limits the application fields of phenolic resin adhesives
Nanoclay is widely used in phenolic resins. The chlorosilane-modified nanofibrous silicate clay containing halogenated hydrocarbon groups is used in phenolic resin adhesives to reduce the content of free phenol in phenolic resin adhesives. This technology has not been reported in the literature so far

Method used

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  • Preparation method of modified phenolic resin adhesive
  • Preparation method of modified phenolic resin adhesive
  • Preparation method of modified phenolic resin adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: Prepare modified phenolic resin adhesive according to the following steps

[0023] (1) Add 300 g of 1 mol / L sulfuric acid solution to 30 g of attapulgite, stir and react at 100°C for 2 hours, filter and wash until the filtrate pH=6, dry and crush the filter cake to obtain acid treatment attapulgite;

[0024] (2) Take 20 grams of acid-treated attapulgite, and add 200 grams of n-butanol, 2 grams of 3-bromopropyltrichlorosilane and 0.2 grams of distilled water to it in turn, and ultrasonically react for 40 minutes at room temperature, and then in 110 ° C Stir and reflux for 3 hours, filter, dry at room temperature, and pulverize to obtain 3-bromopropyltrichlorosilane-modified nano attapulgite;

[0025] (3) At a temperature of 45°C, add 100 grams of phenol, 10 grams of a 40% mass fraction of sodium hydroxide aqueous solution, keep warm and stir for 20 minutes; then add 90 grams of a 39% mass fraction of formaldehyde solution, heat up to 60°C and stir for 30 m...

Embodiment 2

[0026] Embodiment 2: Prepare modified phenolic resin adhesive according to the following steps

[0027] (1) Add 750 grams of 0.8 mol / L hydrochloric acid solution to 40 grams of attapulgite, stir and react at 90°C for 6 hours, filter and wash until the filtrate pH=5, dry and crush the filter cake to obtain acid treatment attapulgite;

[0028] (2) Take 30% acid-treated attapulgite, and add 480 g of methanol, 12 g of chloromethyldimethylsilyl chloride and 3 g of distilled water to it in sequence, conduct ultrasonic reaction at room temperature for 90 minutes, and then stir and reflux at 60°C. React for 8 hours, filter, dry at room temperature, and pulverize to obtain chloromethyldimethylchlorosilane-modified nano attapulgite;

[0029] (3) At 48°C, add 100 grams of phenol, 15 grams of 35% aqueous sodium hydroxide solution, and keep stirring for 30 minutes; then add 85 grams of 38% formaldehyde solution, heat up to 65°C, and stir to react For 45 minutes, continue to add 35 grams ...

Embodiment 3

[0030] Embodiment 3: Prepare modified phenolic resin adhesive according to the following steps

[0031] (1) Add 1000 g of 0.5 mol / L hydrochloric acid solution to 50 g of sepiolite, stir and react at 20°C for 24 hours, filter and wash until the filtrate pH=7, dry and crush the filter cake to obtain acid-treated sea pumice;

[0032] (2) Take 40 grams of acid-treated sepiolite, and add 200 grams of n-propanol, 0.4 grams of dichloromethyldimethylsilyl chloride and 0.08 grams of distilled water to it in turn, and ultrasonically react for 120 minutes at room temperature, and then in 90 ° C Stir under reflux, react for 2 hours, filter, dry at room temperature, and pulverize to obtain dichloromethyldimethylsilane-modified sepiolite;

[0033] (3) At a temperature of 50°C, add 100 grams of phenol, 30 grams of a 20% aqueous sodium hydroxide solution, and keep stirring for 40 minutes; then add 120 grams of a 36% aqueous formaldehyde solution, and heat up to 80°C and stir for 60 minutes. ...

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Abstract

The invention discloses a preparation method of a modified phenolic resin adhesive. The method includes the steps of adding a mineral acid solution into nanofiber-shaped silicate clay, stirring for reaction, filtering and washing, drying a filter cake, and grinding to prepare acid-treated nanofiber-shaped silicate clay; adding an organic solvent, an organic surface modifier and water sequentially into the acid-treated nanofiber-shaped silicate clay, performing ultrasound reaction at the room temperature, filtering, drying, and grinding to prepare nanofiber-shaped silicate clay after organic surface modification; adding phenol and a sodium hydroxide solution into the container, then adding an aldehyde water solution, finally adding the nanofiber-shaped silicate clay after organic surface modification, stirring for backflow, cooling and discharging to prepare the modified phenolic resin adhesive. The preparation method is simple and easy, rich in source of raw materials, and low in cost; the prepared modified phenolic resin adhesive is low in cost, high in a bonding strength, and good in heat resistance; and the content of free phenol in the phenolic resin adhesive is reduced, so that harm of the phenolic resin adhesive to the environment is avoided.

Description

technical field [0001] The invention relates to a preparation method of a modified phenolic resin adhesive, which belongs to the technical field of composite materials, and the product is used in the wood industry. Background technique [0002] Phenolic resin (PF) adhesives are widely used in the wood industry. Phenolic resin adhesives have the advantages of high bonding strength, water resistance, heat resistance, wear resistance and good chemical stability; but phenolic resin adhesives themselves also have disadvantages, such as phenolic resin adhesives. The nature and structure determine its high curing temperature and slow curing speed, especially the high cost of phenolic resin, and the existence of free formaldehyde and free phenol lead to its greater harm to the environment, which limits the application field of phenolic resin adhesives . The technology of modifying phenolic resin adhesives through inorganic fillers and organic fillers is widely used. Chinese patent ...

Claims

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Application Information

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IPC IPC(8): C09J161/10C09J11/04C08G8/10
Inventor 姚超夏建文罗士平于海洋夏青左士祥刘文杰
Owner JIANGSU HUAYUAN MINING