Preparation method of phenolic resin

Abstract

The invention provides a preparation method of phenolic resin. The preparation method comprises the following steps of under the action of an alkaline catalyst, carrying out first reaction on phenolic compounds, aldehyde compounds, a reducing agent and boron-containing compounds to obtain reaction mixture, then carrying out second reaction on the reaction mixture and nitrogen-containing compound to obtain phenolic resin. The preparation method provided by the invention has the advantages that the chromaticity change of the prepared phenolic resin is small in different storage periods before curing and after finish of the curing process, the original performance of the resin is also not influenced and the usability of the resin is improved.

Description

technical field

[0001] The invention belongs to the technical field of polymer materials, in particular to a preparation method of phenolic resin. Background technique

[0002] Phenolic resin is a general term for resins produced by the reaction of phenols and aldehydes in the presence of catalysts. It is the earliest industrially produced polymer material. The cured phenolic resin has good physical and chemical properties and is widely used in industries, Agriculture, national defense and national economy and other aspects.

[0003] Phenolic resins are often used to make molding materials, friction materials, refractory materials, laminated materials, etc. Molding materials made of phenolic resins have excellent heat resistance, insulation and mechanical properties, especially good dimensional stability. It is widely used in aerospace, naval vessels and civil ships, firearms, electronic and electrical components, and power equipment components.

[0004] Phenolic resins ar...

Examples

preparation example Construction

[0026] The invention discloses a preparation method of phenolic resin, comprising the following steps:

[0027] A) under the action of a basic catalyst, the phenolic compound, the aldehyde compound, the reducing agent and the boron-containing compound are subjected to a first reaction to obtain a reaction mixture;

[0028] B) performing a second reaction on the reaction mixture obtained in the above step A) with a nitrogen-containing compound to obtain a phenolic resin.

[0029] In the present invention, under the action of the basic catalyst, the phenolic compound, the aldehyde compound, the reducing agent and the boron-containing compound are subjected to the first reaction to obtain a reaction mixture, and then the second reaction is carried out with the nitrogen-containing compound to obtain the phenolic resin. In the present invention, during the phenolic reaction process, specific proportions of boron-containing compounds, reducing compounds and nitrogen-containing compo...

Embodiment 1

[0048] First, put 1000kg of phenol, 450kg of formaldehyde solution with a mass concentration of 37%, and 9kg of sodium borohydride into the reaction kettle and mix them evenly, then add 30kg of sodium hydroxide, heat up to 60°C, and react at constant temperature for 2 hours, then add 18kg of four The sodium borate was then heated to 70° C., and the constant temperature reaction was continued for 2 hours to obtain a reaction mixture.

[0049] After mixing the above reaction mixture with 25kg of ethylenediamine, react at a temperature of 80°C. When the viscosity of the reaction product is 600cp / 25°C, stop the reaction, and then carry out vacuum distillation. When the reaction product of the above steps When the water content in the medium is 3%, stop the vacuum distillation and add 500kg of methanol. After the product obtained in the above steps is completely dissolved, the temperature is finally lowered to 35°C to obtain light-colored thermosetting phenolic resin 1#.

Embodiment 2

[0051] First, put 1000kg of phenol, 800kg of formaldehyde solution with a mass concentration of 37%, and 12kg of lithium aluminum hydride into the reactor and mix them evenly, then add 20kg of potassium hydroxide, heat up to 66°C, and react at constant temperature for 2 hours, then add 15kg of boric acid Then the temperature was raised to 75° C., and the constant temperature reaction was continued for 2 hours to obtain a reaction mixture.

[0052] After mixing the above reaction mixture with 25kg urea, react at a temperature of 80°C. When the viscosity value of the reaction product is 800cp / 25°C, stop the reaction, and then carry out vacuum distillation. When the reaction product of the above steps contains moisture When the content is 5%, stop the vacuum distillation and add 600kg of acetone. After the product obtained in the above steps is completely dissolved, the temperature is finally lowered to 35°C to obtain light-colored thermosetting phenolic resin 2#.

technical field

[0001] The invention belongs to the technical field of polymer materials, in particular to a preparation method of phenolic resin. Background technique

[0002] Phenolic resin is a general term for resins produced by the reaction of phenols and aldehydes in the presence of catalysts. It is the earliest industrially produced polymer material. The cured phenolic resin has good physical and chemical properties and is widely used in industries, Agriculture, national defense and national economy and other aspects.

[0003] Phenolic resins are often used to make molding materials, friction materials, refractory materials, laminated materials, etc. Molding materials made of phenolic resins have excellent heat resistance, insulation and mechanical properties, especially good dimensional stability. It is widely used in aerospace, naval vessels and civil ships, firearms, electronic and electrical components, and power equipment components.

[0004] Phenolic resins ar...

Examples

preparation example Construction

[0026] The invention discloses a preparation method of phenolic resin, comprising the following steps:

[0027] A) under the action of a basic catalyst, the phenolic compound, the aldehyde compound, the reducing agent and the boron-containing compound are subjected to a first reaction to obtain a reaction mixture;

[0028] B) performing a second reaction on the reaction mixture obtained in the above step A) with a nitrogen-containing compound to obtain a phenolic resin.

[0029] In the present invention, under the action of the basic catalyst, the phenolic compound, the aldehyde compound, the reducing agent and the boron-containing compound are subjected to the first reaction to obtain a reaction mixture, and then the second reaction is carried out with the nitrogen-containing compound to obtain the phenolic resin. In the present invention, during the phenolic reaction process, specific proportions of boron-containing compounds, reducing compounds and nitrogen-containing compo...

Embodiment 1

[0048] First, put 1000kg of phenol, 450kg of formaldehyde solution with a mass concentration of 37%, and 9kg of sodium borohydride into the reaction kettle and mix them evenly, then add 30kg of sodium hydroxide, heat up to 60°C, and react at constant temperature for 2 hours, then add 18kg of four The sodium borate was then heated to 70° C., and the constant temperature reaction was continued for 2 hours to obtain a reaction mixture.

[0049] After mixing the above reaction mixture with 25kg of ethylenediamine, react at a temperature of 80°C. When the viscosity of the reaction product is 600cp / 25°C, stop the reaction, and then carry out vacuum distillation. When the reaction product of the above steps When the water content in the medium is 3%, stop the vacuum distillation and add 500kg of methanol. After the product obtained in the above steps is completely dissolved, the temperature is finally lowered to 35°C to obtain light-colored thermosetting phenolic resin 1#.

Embodiment 2

[0051] First, put 1000kg of phenol, 800kg of formaldehyde solution with a mass concentration of 37%, and 12kg of lithium aluminum hydride into the reactor and mix them evenly, then add 20kg of potassium hydroxide, heat up to 66°C, and react at constant temperature for 2 hours, then add 15kg of boric acid Then the temperature was raised to 75° C., and the constant temperature reaction was continued for 2 hours to obtain a reaction mixture.

[0052] After mixing the above reaction mixture with 25kg urea, react at a temperature of 80°C. When the viscosity value of the reaction product is 800cp / 25°C, stop the reaction, and then carry out vacuum distillation. When the reaction product of the above steps contains moisture When the content is 5%, stop the vacuum distillation and add 600kg of acetone. After the product obtained in the above steps is completely dissolved, the temperature is finally lowered to 35°C to obtain light-colored thermosetting phenolic resin 2#.

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