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Method for controlling lignin-phenolic resin adhesive reaction end point

A technology of phenolic resin glue and control method, applied in the directions of adhesives, aldehyde/ketone condensation polymer adhesives, adhesive types, etc., can solve the problems of unsuitable tracking and monitoring production needs, cumbersome, different, etc., to achieve economical convenience Detection method, the effect of avoiding errors

Active Publication Date: 2011-04-13
ANHUI GEYI CYCLIC ECONOMY IND PARK
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, practice shows that the viscosity value measured by the viscometer often cannot correctly reflect the end point of the reaction, which affects product quality; the molecular weight detection method is expensive and cumbersome to operate, and is not suitable for the production needs of tracking monitoring
Although the atomization observation method is simple, because the lignin solution is black, it affects the visual inspection effect. The same sample often varies from person to person, and different results are obtained.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 365kg of highly active alkali lignin solution with a solid content of 22% and pH 13.5, 120kg of phenol (lignin replaces 40% phenol), and 220kg of formaldehyde (80% of the total amount) into the reactor, and fully After mixing, add 55kg of 30% liquid caustic soda (80% of the total amount), heat up to 85-100°C within 30 minutes, keep warm for 30 minutes, add the remaining liquid caustic soda and 20% of the total amount of water, 80-85°C After keeping warm for 10 minutes, add the remaining formaldehyde and stir evenly. After raising the temperature to 85-100°C and keeping warm for 10 minutes, perform the following detection: use a measuring cylinder to take 20ml of sample from the reaction kettle and pour it into a small beaker, slowly add 4mol / L hydrochloric acid, and stir while adding acid Until the precipitate appears, observe the color of the precipitate and test the toughness, and check it every 10 minutes. When the flexibility of the brown precipitate gradually de...

Embodiment 2

[0024] Add 365kg of high-activity alkali lignin solution with solid content of 20% and pH 13.5, 80kg of phenol (lignin replaces 50% phenol), and 204kg of formaldehyde (80% of the total amount) into the reactor, and fully After mixing, add 52kg of 30% liquid caustic soda (80% of the total amount), heat up to 85-100°C within 30 minutes, keep warm for 30 minutes, add the remaining liquid caustic soda and 20% of the total amount of water, 80-85°C After keeping warm for 10 minutes, add the remaining formaldehyde and stir evenly, raise the temperature to 85-100°C and keep warm for 10 minutes, then carry out the following test: take 20ml of sample from the reaction kettle with a measuring cylinder and pour it into a small beaker, slowly add 2mol / L phosphoric acid, and stir while adding acid Until the precipitate appears, observe the color of the precipitate and test the toughness, and check it every 10 minutes. When the flexibility of the brown precipitate gradually decreases, and the...

Embodiment 3

[0026] Add 300kg of high-activity alkali lignin solution with solid content of 20% and pH 13.5, 140kg of phenol (lignin replaces 30% phenol), and 260kg of formaldehyde into the reaction kettle. After fully mixing at 40-60°C, add 30% of Liquid caustic soda 60kg, heat up to 85-100°C within 30min, keep warm for 40min, then carry out the following test: use a measuring cylinder to sample 20ml from the reaction kettle and pour it into a small beaker, slowly add 5mol / L p-toluenesulfonic acid, and stir while adding acid until A precipitate appeared. Observe the color of the precipitate and test the toughness, and check it every 10 minutes. When the flexibility of the brown precipitate gradually decreases, and the brittleness gradually increases to the point where the drawn wire is easy to break and the broken surface has a brown luster, immediately lower the temperature, terminate the polymerization reaction, and cool down. Glue will come out at 40-45°C, the bonding strength of the c...

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PUM

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Abstract

The invention relates to a method for controlling a lignin-phenolic resin adhesive reaction end point. The method comprises the following steps of: sampling and performing acidification and detection, wherein the acidification is to add 2 to 5mol / L acid solution into the taken sample in a stirring state until cakes are generated; the detection is to detect the cakes; and when the cakes are brown,can be lengthened by stretching after being taken out but are easy to break, and a fracture surface has brown gloss, the end point is achieved. The control method is not limited by the proportion that phenol is substituted by the lignin, is not influenced by the polymerization reaction process of the lignin, the phenol and formaldehyde, and simply, fast, conveniently, visually, accurately and reliably reflects the end point of the lignin-phenolic resin adhesive reaction, so that a reliable, economical and convenient detection method is provided for the industrialized production of a lignin-based phenolic resin adhesive.

Description

1. Technical field [0001] The invention relates to a method for controlling the end point of a chemical reaction, in particular to a method for controlling the end point of the reaction of an alkali lignin-phenolic resin composite adhesive. 2. Background technology [0002] The traditional phenolic resin adhesive is formed by the polymerization reaction of phenol and formaldehyde under alkaline conditions, and its bonding strength depends on the degree of polymerization between molecules and the size of its molecular weight; When the polymerization is excessive, the molecular weight of the resin is too large, and the bonding strength is also reduced. Therefore, in actual production, it is the key to determine the quality of phenolic resin adhesives to grasp the degree of polymerization of the resin in time, terminate its polymerization reaction, and optimize the bonding strength of the resin. The traditional methods for detecting the degree of polymerization of phenolic res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J161/14G01N21/82
Inventor 陈存武陈乃富陈宇管淑清宗武郭万宏刘天霁
Owner ANHUI GEYI CYCLIC ECONOMY IND PARK
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