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A kind of preparation method of Ni modified thermosetting phenolic 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 difficult control of pH value and low reaction efficiency, and achieve the effects of saving reaction time, sufficient reaction and stable pH value

Inactive Publication Date: 2016-06-22
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 65°C water bath. At 40°C, 1 / 4 of formaldehyde was added dropwise to phenol and basic catalyst NaOH, and an appropriate amount of methanol was added for pre-mixing for 15 minutes. In the process of slowly increasing the temperature to 80°C, continue to drop 1 / 4 of the formaldehyde until the timing starts at 80°C, and react for 1h. Then add the remaining formaldehyde, and react for 2.5h. After the time is up, cool to room temperature, add a mixed solution of oxalic acid and acetic acid to adjust the pH. At 48°C, carry out vacuum distillation until the water output reaches the estimated amount and the experiment ends. 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 content of residual phenol increased greatly and the solid content decreased. It shows that the reaction is not complete, and the reaction rate i...

Embodiment 2

[0022] Melt in a 65°C water bath. At 40°C, in phenol and basic catalysts NaOH and NiCl 2 Add 1 / 4 of formaldehyde to the mixed solution, and add an appropriate amount of methanol for pre-mixing for 15 minutes. In the process of slowly increasing the temperature to 80°C, continue to drop 1 / 4 of the formaldehyde until the timing starts at 80°C, and react for 1h. Then add the remaining formaldehyde, and react for 2.5h. After the time is up, cool to room temperature, add oxalic acid solution, and adjust the pH. At 48°C, carry out vacuum distillation until the water output reaches the estimated amount and the experiment ends. A viscous yellowish phenolic resin was obtained.

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

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Abstract

A method for preparing a Ni-modified thermosetting phenolic resin relates to a method for preparing a phenolic resin. In the present invention, the molar ratio of phenol to formaldehyde is 1:1.5, and the formaldehyde is sequentially added in batches to make the reaction more complete. An appropriate amount of methanol was added during the reaction. The basic catalyst is a mixed solution of NiCl2 and NaOH, and the weight is 3%-5% of the phenolic raw material. The acidic catalyst is a mixed acid buffer solution of oxalic acid and acetic acid, and the weight is 2%-4% of the phenolic raw material. The method uses oxalic acid, mixed acid buffer solution of acetic acid, and under the catalyst action of Ni compound, prepares phenolic resin with phenol raw material and formaldehyde raw material, and under the catalytic action of Ni compound, the chelating strength of cation is higher, and the activity of its ortho-position The stronger it is, the faster the reaction rate. The stability of the prepared phenolic resin was improved by warming the solution with mixed acid of oxalic acid and acetic acid.

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, and low porosity. It is used in 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 proce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/10
Inventor 高恩军赵富臣马驰
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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