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Lignin modified phenolic resin, foam thereof, preparation method of resin, and preparation method of foam

A phenolic resin foam and phenolic resin technology are applied in the fields of lignin-modified phenolic resin, foam and its preparation, which can solve the problems of long gel time, increased production cost, reduced thermal insulation performance, and reduced foam strength, and achieves good thermal insulation performance. , The effect of high curing activity and low slag removal rate

Active Publication Date: 2014-12-31
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, phenolic foam also has disadvantages such as easy pulverization and poor toughness.
In addition, due to the reduction of oil reserves and the continuous rise of oil prices in recent years, the production cost of phenolic resin and phenolic foam using petroleum as raw material continues to increase; at the same time, toxic free phenol and formaldehyde are produced during the production of phenolic resin and phenolic foam. It is difficult to be removed, so the environmental protection issues of phenolic resin and phenolic foam have always attracted the attention of users
Moreover, compared with pure phenolic resin, the lignin-modified phenolic resin synthesized by the above-mentioned phenolized lignin has lower curing reactivity, longer gel time and higher free aldehyde content.
Compared with pure phenolic foam, the thermal insulation performance and foam strength of the phenolic foam prepared with the above-mentioned phenolized lignin modified phenolic resin will be reduced to varying degrees.

Method used

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  • Lignin modified phenolic resin, foam thereof, preparation method of resin, and preparation method of foam
  • Lignin modified phenolic resin, foam thereof, preparation method of resin, and preparation method of foam

Examples

Experimental program
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Effect test

Embodiment 1

[0059] 1. Preparation of phenolized lignin

[0060] Take 100g of lignin, add it into a high-temperature and high-pressure reactor, then add 100g of phenol, stir, then add 3g of phosphoric acid, stir, close the reactor, and replace the air in the reactor with nitrogen. Raise the temperature to 250°C for 2 hours (reaction pressure about 4MPa). After the reaction is completed, pass condensed water to cool down the reactor, then open the exhaust valve to release the pressure, and open the reactor to obtain a phenol solution of phenolized lignin (Mn=617).

[0061] 2. Preparation of Lignin Modified Phenolic Resin

[0062] Add 15.0 g (0.1594 mol) of phenol to 10.0 g of lignin phenolization products (containing 0.0531 mol of phenol), mix well, heat up to 50 ° C, adjust its pH value to 9 with 50 wt % NaOH aqueous solution; then add 34.50 g (that is, 0.4251mol formaldehyde) formaldehyde aqueous solution with a concentration of 37wt%; react the reaction system at a constant temperature...

Embodiment 2

[0067] One, the preparation of phenolized lignin: same as embodiment 1.

[0068] 2. Preparation of Lignin Modified Phenolic Resin

[0069] Take 10.0g of lignin phenolization product (containing 0.0531mol of phenol) in a three-necked flask without adding phenol, raise the temperature to 50°C, adjust its pH value to 8 with 50wt% NaOH aqueous solution, and mix 8.62g (0.1062mol of formaldehyde ) formaldehyde solution with a concentration of 37wt% was added dropwise; the reaction system was reacted at a constant temperature of 50°C for 3h (including the time consumed by dropping formaldehyde), then raised to 80°C for a constant temperature of 3h, and then heated to 90°C for 1h; the reaction The temperature of the system dropped rapidly to below 60°C, and the reaction was terminated. Add p-toluenesulfonic acid to adjust the pH value to neutral; then dehydrate the product to obtain lignin-modified phenolic resin. Resin indicators such as resin solid content and gel time are shown i...

Embodiment 3

[0073] One, the preparation of phenolized lignin: same as embodiment 1.

[0074] 2. Preparation of Lignin Modified Phenolic Resin

[0075] Take 10.0g of lignin phenolization products (containing 0.0531mol of phenol) into a three-necked flask, add 15.0g (0.1594mol) of phenol, raise the temperature to 60°C, adjust its pH value to 9 with 50wt% KOH aqueous solution, drop by drop Add 34.50g (0.4251mol formaldehyde) formaldehyde aqueous solution with a concentration of 37wt%; react the reaction system at a constant temperature of 60°C for 2h (including the time consumed by dropping formaldehyde), then raise the temperature to 70°C for 5h, then raise the temperature to 90°C for reaction 0.2h. The temperature of the reaction system was rapidly lowered to below 60°C, and the reaction was terminated. Add p-toluenesulfonic acid to adjust the pH value to neutral; then dehydrate the product to obtain lignin-modified phenolic resin. Resin indicators such as resin solid content and gel ti...

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Abstract

The invention belongs to the technical field of organic composite materials, and especially relates to a lignin modified phenolic resin, a foam thereof, a preparation method of the resin, and a preparation method of the foam. The preparation method of the lignin modified phenolic resin comprises the following steps: 1, mixing an acid catalyst with phenol and lignin, and reacting at 230-300DEG C under 2-5MPa to obtain a lignin phenolation product solution; and 2, adding formaldehyde, and reacting to obtain the lignin modified phenolic resin, wherein phenol can be added or not added to the lignin phenolation product solution obtained in step 1 before the addition of formaldehyde. The lignin modified phenolic resin synthesized through the method has a high curing activity, and has a shorter gelling time and a lower content of free formaldehyde than low temperature phenolated lignin modified phenolic resin. The phenolic foam prepared by using the lignin modified phenolic resin has the advantages of good toughness, high percentage of close area, and good thermal insulation performance.

Description

technical field [0001] The invention belongs to the technical field of organic composite materials, and in particular relates to a lignin-modified phenolic resin, foam and a preparation method thereof. Background technique [0002] Phenolic foam is a new type of thermal insulation material, which has very broad application prospects due to its advantages of light weight, heat insulation, and flame retardancy. It was used in the insulation of missiles and rocket heads in the early days. In recent years, due to the strict requirements on the thermal stability and heat resistance stability of synthetic foams in high-rise buildings, transportation, and space technology, phenolic foams have developed more rapidly. . As a new type of multi-purpose foam material, phenolic foam has been widely valued for its advantages of heat resistance, flame retardant and self-extinguishing, resistance to flame penetration, and no dripping in case of fire. However, phenolic foam also has disadv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/34C08L61/14C08J9/14
Inventor 赵彤姜晓文李昊王娟刘哲高建伟田昶斌
Owner INST OF CHEM CHINESE ACAD OF SCI
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