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Preparation method of Ni-modified thermosetting phenol resin

A phenolic resin and thermosetting technology, which is applied in the field of Ni-modified thermosetting phenolic resin preparation, can solve the problems of low reaction efficiency and difficult pH control, achieve full reaction, save reaction time, and increase substitution speed.

Inactive Publication Date: 2015-02-04
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation of thermosetting phenolic resin mostly adopts the buffer system formed by strong acid and strong alkali, which causes many shortcomings and deficiencies such as difficult control of pH value and low reaction efficiency during the reaction process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Melt in a water bath at 65°C. At 40°C, 1 / 4 formaldehyde was added dropwise to phenol and basic catalyst NaOH, and an appropriate amount of methanol was added for premixing for 15 min. In the process of slowly ramping up to 80°C, continue to add 1 / 4 formaldehyde dropwise until the timer starts at 80°C, and react for 1 hour. Then add the remaining formaldehyde and react for 2.5 hours. After the time is up, it is cooled to room temperature, and a mixed solution of oxalic acid and acetic acid is added to adjust the pH. At 48°C, vacuum distillation was performed, and the experiment ended when the effluent amount reached the expected amount. A viscous yellowish phenolic resin was obtained.

[0020] In this example, only NaOH was used as the basic catalyst, and NiCl was not added. 2 . It was found that in the final product phenolic resin, the residual phenol content was greatly increased and the solid content decreased. It shows that the reaction is not complete, and ...

Embodiment 2

[0022] Melt in a water bath at 65°C. NaOH and NiCl in phenol and alkaline catalyst at 40°C 2 Add 1 / 4 formaldehyde to the mixed solution, and add an appropriate amount of methanol for premixing for 15min. In the process of slowly ramping up to 80°C, continue to add 1 / 4 formaldehyde dropwise until the timer starts at 80°C, and react for 1 hour. Then add the remaining formaldehyde and react for 2.5 hours. After the time is up, it is cooled to room temperature, and oxalic acid solution is added to adjust the pH. At 48°C, vacuum distillation was performed, and the experiment ended when the effluent amount reached the expected amount. A viscous yellowish phenolic resin was obtained.

[0023] In this embodiment, only the oxalic acid solution is added, and the mixed acid solution of oxalic acid and acetic acid is not added. After the obtained phenolic resin is heated, the degradation degree is obviously higher than that of the phenolic resin prepared with the mixed acid buffer sol...

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PUM

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Abstract

The invention discloses a preparation method of Ni-modified thermosetting phenol resin, and relates to a preparation method of phenolic resin. The molar ratio of phenol to formaldehyde is 1:1.5, and the formaldehyde is sequentially added in batches, so that reaction is more sufficient. In a reacting process, a proper amount of methanol is added. A mixed solution of NiCl2 and NaOH serves as a basic catalyst, and the weight of the mixed solution accounts for 3-5% of phenol raw materials. A mixed acid buffer solution of oxalic acid and acetic acid is taken as an acid catalyst, and the weight of the buffer solution accounts for 2-4% of the phenol raw materials. According to the method disclosed by the invention, the phenolic resin is prepared from phenol and formaldehyde raw materials under the effects of the mixed acid buffer solution mixed with acetic acid and a catalyst of a Ni compound; under the catalysis effect of the Ni compound, as the chelating strength of cation is higher, the activity on the ortho-position is stronger and the reaction rate is rapider. By virtue of the mixed acid buffer solution of oxalic acid and acetic acid, the stability of the prepared phenolic resin is improved.

Description

technical field [0001] The invention relates to a method for preparing a phenolic resin, in particular to a method for preparing a Ni-modified thermosetting phenolic resin. Background technique [0002] Thermosetting phenolic resin has very strong wetting ability, good molding performance, high bulk density, low porosity, used for refractory products, and can be kept for three months at 15°C-20°C. The advantages of phenolic resin products are mainly dimensional stability, Heat-resistant, flame-retardant, good electrical insulation, strong acid resistance, it is mainly used in various industries such as transportation, construction, military, mining, etc., and has a wide range of applications. [0003] At present, the preparation of thermosetting phenolic resin mostly adopts the buffer system formed by strong acid and strong base, which causes many shortcomings and deficiencies such as difficult control of pH value and low reaction efficiency during the reaction process. ...

Claims

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Application Information

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IPC IPC(8): C08G8/10
Inventor 高恩军赵富臣马驰
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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