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Preparation method of phenolic resin having narrow molecular weight distribution

A narrow molecular weight distribution, phenolic resin technology, applied in the direction of aldehyde/ketone condensation polymer adhesives, adhesive types, adhesives, etc., can solve the problems of increased cost, waste water pollution, complicated process, and inability to obtain molecular weight distribution, etc.

Active Publication Date: 2014-04-30
SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

U.S. Patent US6045966 adopts the method of precipitating phenol-formaldehyde polymer in batches with organic solvent\water mixture to classify phenolic resin to achieve the purpose of controlling the molecular weight distribution of phenolic resin. This type of method consumes a large amount of organic solvent, which increases the cost and waste water Pollution
Japanese patent 00135829.4 synthesizes a narrow molecular weight distribution resin synthesis method based on the process of alkali first and then acid. This method is complex and the molecular weight distribution of the prepared phenolic resin is above 1.2. It is impossible to obtain a narrower molecular weight distribution and more uniform properties of the phenolic resin.

Method used

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  • Preparation method of phenolic resin having narrow molecular weight distribution

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preparation example Construction

[0044] The preparation method provided by the present invention specifically includes: adding phenol, aldehyde accounting for 50% of the total aldehyde, to the equipment with a reflux device, adjusting the temperature to 40-45°C, adding an alkali catalyst, adjusting the temperature to 55-85°C, and constant temperature After 1-3 hours, add the remaining 50% aldehyde, measure the content of free aldehyde accounting for 3-5wt% of aldehyde compounds at a constant temperature of 55-85°C, quickly cool down to 48-50°C, add a low-molecular polymerization initiator, and rapidly cool down Below 25°C, settle for 24 hours, filter and dry.

[0045] The resin synthesized by the invention has a narrow molecular weight distribution, and the production process is simple and environment-friendly. The filtrate after filtration can be adjusted for wood bonding. Due to excessive aldehyde, the utilization rate of the phenolic compound is 100%, which protects the environment.

Embodiment 1

[0047] Put 500g of phenol and 500g of formaldehyde into a reaction flask equipped with stirring, thermometer and reflux device, adjust the temperature to 40°C, add 25g of sodium hydroxide, raise the temperature to 60°C and react at constant temperature for 2 hours, add 500g of formaldehyde, adjust the temperature to 50°C ℃, constant temperature until the content of free aldehyde accounts for 3.8wt% of aldehyde compounds, add urea, keep the temperature constant for 10 minutes, quickly lower the vacuum and reflux temperature to 12 ℃ while stirring, settle for 24 hours, filter and dry.

[0048] Detect the molecular weight distribution of the phenolic resin prepared by the present embodiment by gel solution chromatography GPC, the result is as follows figure 1 As shown, it can be seen that the molecular weight distribution Mw / Mn of the phenolic resin prepared in this embodiment is 1.05, which is smaller than the molecular weight distribution of the prior art. The phenolic resin wi...

Embodiment 2

[0050] Put 500g of phenol and 500g of formaldehyde into a reaction flask equipped with a stirring, thermometer and reflux device, adjust the temperature to 45°C, add 25g of sodium hydroxide, raise the temperature to 50°C and react at a constant temperature for 3 hours, add 500g of formaldehyde, and adjust the temperature to 45°C ℃, constant temperature until the content of free aldehyde accounts for 4.5wt% of aldehyde compounds, add urea, keep the temperature constant for 10 minutes, quickly lower the vacuum and reflux temperature to 12 ℃ while stirring, settle for 24 hours, filter and dry.

[0051] The molecular weight distribution of the phenolic resin prepared in this example was detected by gel solution chromatography (GPC). The molecular weight distribution Mw / Mn of the phenolic resin prepared in this example was 1.03, which was smaller than the molecular weight distribution of the prior art. The phenolic resin with narrow molecular weight distribution prepared by the pres...

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Abstract

The invention provides a preparation method of a phenolic resin having narrow molecular weight distribution. The preparation method comprises the following steps: a) mixing a phenol compound, a first aldehyde compound and an alkaline catalyst for polycondensation reaction to obtain a prepolymer; b) mixing a second aldehyde compound with the precpolymer for further polycondensation reaction; and c) when the content of free aldehyde in a reaction system is 3-5wt%, adding a low-molecule polymer initiator in the reaction system for further reaction to obtain the phenolic resin. The phenolic resin prepared by using the method is narrow in molecular weight distribution; production process is environment-friendly; and filtrate obtained after filtration can be used for wood adhesion through regulation, thereby ensuring the utilization rate of phenol and protecting environment.

Description

technical field [0001] The invention relates to the field of polymer preparation, in particular to a preparation method of a narrow molecular weight distribution phenolic resin. Background technique [0002] Phenolic resin is a polymer obtained by polycondensation of phenol and aldehyde. Because phenolic resin has a phenolic unit and a regular molecular chain structure, phenolic resin has comprehensive properties such as heat resistance and flame retardancy, and has become one of the important industrial resin varieties in the past century. Phenolic resins are generally prepared using phenol and formaldehyde. It is obtained by polycondensation under the action of a catalyst. Since the polymerization is polycondensation and gradual polymerization, the resin system is determined to be a phenolic mixture with various molecular weight distributions. It has the defects of asynchronous curing and large internal stress during curing. [0003] Now more and more research work is don...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/10C08G8/24C08G8/04C09J161/10C09J161/12
Inventor 邢介名姜广锋焦锋董岳
Owner SHANDONG SHENGQUAN NEW MATERIALS CO LTD