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Preparation method of ultrahigh molecular weight phenolic resin

An ultra-high molecular weight, phenolic resin technology, applied in the field of preparation of ultra-high molecular weight phenolic resin, can solve the problems of high raw material ratio, easy gelation, difficult control of the production process, etc., and achieves mild conditions, reasonable molecular weight distribution, and process Simple to use effects

Active Publication Date: 2011-09-14
SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Ultra-high molecular weight phenolic resin is a thermoplastic phenolic resin with a weight average molecular weight of about 15,000 and above. In the production of existing ultra-high molecular weight phenolic resin, a relatively high ratio of raw materials is required, and it is difficult to control during the production process. It is easy to occur during the reaction process. Gel, no thermoplastic phenolic resin
[0004] Existing published patent CN1440990A discloses a preparation method of high molecular weight phenolic resin used for melt spinning. In this patent, transition metal oxide is used as catalyst, and the metal oxide remaining in the resin will affect the performance of phenolic resin. Electrical performance, and the production process uses a large amount of organic solvents, which increases the risk of operation and the difficulty of wastewater treatment to a certain extent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1 phenol / formaldehyde / hydrochloric acid

[0024] 500g of phenol, 350g of formaldehyde (37wt%), and 1.5g of hydrochloric acid (20wt%) were added to a stirring 1000ml four-necked flask with a condenser and mixed. Heat up to boiling reflux, react for 3 hours, heat up to 110°C for dehydration reaction, then cool down to 90°C, add 39g of formaldehyde (37wt%), 0.5g of hydrochloric acid (20wt%), and then reflux for reaction. When the melt viscosity of the resin reaches 3500MPa·s / 100°C, add 0.5g of sodium hydroxide, the pH of the resin reaches 6.4, and then continue to heat up and dehydrate until the temperature reaches 160°C to obtain ultra-high molecular weight phenolic resin. The resin has a number average molecular weight Mn of 1100 and a weight average molecular weight Mw of 14899. The softening point is 124°C, and the free phenol is 4.5%.

Embodiment 2

[0025] Embodiment 2 phenol / formaldehyde / sulfuric acid

[0026] Change hydrochloric acid into the sulfuric acid of 20wt%, other is the same as embodiment 1, still can obtain the phenolic resin of ultrahigh molecular weight. The number average molecular weight Mn of the resin is 1200, the weight average molecular weight Mw is 19980; the softening point is 130° C., and the free phenol is 4.3%.

Embodiment 3

[0027] Embodiment 3 cresol / formaldehyde / oxalic acid

[0028] 400g of cresol, 230g of formaldehyde (37wt%), 2.8g of oxalic acid (20wt%) were added to a 1000ml four-neck flask with a condenser and mixed. Heat up to boiling reflux, react for 3 hours, heat up to 110°C for dehydration reaction, then cool down to 95°C, add 25g of formaldehyde (37wt%), 0.5g of hydrochloric acid (20wt%), and then reflux for reaction. When the melt viscosity of the resin reaches 4500MPa·s / 100°C, add 0.9g of potassium hydroxide, the pH of the resin reaches 6, and then continue to heat up and dehydrate until the temperature reaches 160°C to obtain ultra-high molecular weight phenolic resin. The number average molecular weight Mn of the resin is 1350, and the weight average molecular weight Mw is 25400. Softening point 135°C, free cresol 4%.

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Abstract

The invention discloses a preparation method of ultrahigh molecular weight phenolic resin. The preparation method comprises the following steps of: (1) weighing phenol and aldehyde in a molar ratio of 1: (0.8-1.0) respectively, and weighing acid in a mass ratio of the acid to the phenol of (0.5-4): 100; (2) mixing the phenol, partial aldehyde and partial acid, heating till boiling, and refluxing for 2 to 4 hours, wherein the partial aldehyde or the partial acid accounts for 75 to 95 percent of the total adding amount of the aldehyde or the acid; (3) heating and dehydrating the reactants of the step (2), cooling the reactants to the temperature of between 80 and 100 DEG C, adding the rest aldehyde and the rest acid, heating till boiling, and refluxing for 1 to 3 hours; and (4) detecting the melting viscosity of the reactants in the refluxing process of the step (3), adding alkali when the viscosity reaches 2,000 to 4,500MPa.s / 100 DEG C, regulating the pH value to be between 4 and 7, heating and dehydrating to obtain the ultrahigh molecular weight phenolic resin. The weight-average molecular weight of the prepared phenolic resin can reach 14,000 to 30,000, the softening point is 120 to 140 DEG C, and the molecular weight distribution is 13 to 19.

Description

technical field [0001] The invention relates to the technical field of preparation of phenolic resin, in particular to a preparation method of ultra-high molecular weight phenolic resin. Background technique [0002] Phenolic resin is the earliest industrialized synthetic resin in the world. It has a history of nearly 100 years. Because of its advantages such as easy availability of raw materials, low price of raw materials, simple production process and equipment, and more importantly, the excellent properties of phenolic resin itself Performance, has been widely used in various fields of daily life. Among them, due to the high temperature resistance of ultra-high molecular weight phenolic resin itself, it is widely used in high-end molding compounds, friction materials, abrasive abrasives, etc. [0003] Ultra-high molecular weight phenolic resin is a thermoplastic phenolic resin with a weight average molecular weight of about 15,000 and above. In the production of existin...

Claims

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Application Information

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IPC IPC(8): C08G8/04C08G8/10C08G8/08
Inventor 唐一林江成真刘翠华刘卫
Owner SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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