JPS5825574B2 - How do you know what to do? - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing thermosetting resin molding materials, that is, thermosetting resins typified by phenolic resins, epoxy resins, diallyl phthalate resins, unsaturated polyester resins, etc. For example, in continuous automatic roll heating kneading, the gist is to control and adjust the amount of raw materials supplied onto the kneading rolls in accordance with the sheet temperature.

An object of the present invention is to establish a method for efficiently producing a thermosetting molding material that has stable fluidity and moldability and has no variation in these properties.

Generally, thermosetting resin molding materials include various resins, curing agents,
It is manufactured by heating and kneading a mixture of fillers, mold release agents, additives, etc. to give it fluidity, hardenability, and fillability suitable for molding.

Among these manufacturing and processing methods that involve heating and kneading, the heating and kneading method using rolls is generally used as a method for obtaining high-quality materials, and a batch method or a continuous method is adopted.

In particular, a continuous type heated cross-wire roll is excellent in terms of productivity.

Chemical reaction, drying, homogenization,
Densification progresses at the same time, and although the degree of these changes affects the quality and variation of the material's fluidity and moldability, it is difficult to reproduce exactly the same state, and the manufacturing method It was an issue at.

In addition, in the case of a continuous roll system, it is easy to set conditions, but it has not been established how to control the degree of heating and kneading.

Traditionally, as a method for managing heating cross-wire conditions, samples are collected after the drying and pulverizing processes after heating and measuring characteristics such as fluidity, and the measurement results are used to determine the roll cross-wire conditions, such as roll temperature, roll temperature, etc. It has been common practice to control the sheet take-out position or the amount of material charged onto the roll.

However, with this method, there is a delay in controlling the conditions due to the difference between the fluidity measurement position and the heating cross-wire position, as well as the fluidity measurement time, and it is impossible to control the material evenly down to minute units. Met.

The present invention is an attempt to solve this drawback, and as a result of considering a product with a fast response speed, we found that the material is custom-made after manufacturing and processing (the sheet temperature immediately before or immediately after being taken out from the roll corresponds to the material properties). By appropriately controlling the amount of raw materials fed onto the kneading rolls in accordance with the sheet temperature, we were able to improve the fluidity and moldability of the molding material obtained by heating and kneading, as well as their variations. I made sure to manage it uniformly.

A rotary feeder, screw feeder, or belt conveyor is generally used as a device for feeding the raw material onto the mixed roll.

In order to vary the amount of feed by type in these feeding devices, the feeding amount can be easily changed by changing the number of rotations of a rotary feeder or a screw feeder, and by changing the moving speed of a belt conveyor.

Hereinafter, a method for controlling heating crosstalk in a continuous automatic roll according to the present invention will be explained.

First, the temperature of each part of the sheet wound around the roll is measured, and the amount of raw material supplied is adjusted so that the sheet temperature at the sheet take-out position reaches a specified target temperature.

In the case of a continuous roll type, compared to a batch type, the heating and kneading on the roll changes steadily and continuously, and a continuous sheet can be taken out from one end of the wound sheet or any location, so the manufacturing method according to the present invention can be adopted.

On the other hand, in the case of a batch method, the temperature is discontinuous and differs depending on the portion of the sheet, so it cannot be used for material manufacturing control.

As described above, it is clear that the material manufactured by controlling the temperature of the sheet taken out continuously has less variation in fluidity as a molding material and has uniform and good molding processability compared to the material manufactured by the conventional method. This led to the establishment of a manufacturing method.

Thermosetting resin molding materials represented by phenol resin, epoxy resin, diallyl phthalate resin, unsaturated polyester resin, etc. are each manufactured by a roll method, and the present invention relates to the production of thermosetting resins that can be manufactured by a roll method. As a result of examining the effects of applying these methods, we found that a molding material with less variation (and uniformity and good moldability) could be obtained compared to when manufactured using a conventional method.

Thermosetting resins that can be manufactured by roll method, namely phenolic resins, epoxy resins, diallyl phthalate resins,
The technology of the present invention can be applied to unsaturated polyester resins in general, and will greatly contribute to technological progress that will enable the supply of high-quality products to the market.

Examples will be shown below.

Comparative example l Phenol resin (
15 parts of hexamethylenetetramine, 70 parts of wood flour, 15 parts of asbestos, 4 parts of stearic acid, and 4 parts of spirit black are premixed to 100 parts (usually novolac), and the continuous roll conditions, i.e., the roll temperature The settings were 90°C on the high temperature side and 60°C on the low temperature side, a raw material supply scale (corresponding to the supply speed) of 17, and a sheet take-out scale (corresponding to the length from the raw material input port to the sheet take-out position) of 10, and heated and kneaded using the usual method. and used as a molding material.

The temperature of the sheet taken out at this time was 98 to 112°C.

The variation in fluidity of this molding material was 34%, and the moldability (fillability, hardenability) in the molding test mold was moderate.

Example 1 Same as Comparative Example 1 - Using raw materials in a self-storage table, heating and kneading was carried out at a roll temperature of 90°C on the high temperature side and 60°C on the low temperature side, with a sheet take-out scale of 10, and the take-out sheet temperature was in the range of 108 to 111°C. The raw material supply scale was adjusted so that the

The raw material supply scale at this time was 15-24.

The variation in fluidity of this molding material was 5%, and the molding processability in the molding test mold was extremely good.

Comparative Example 2 Epoxy resin (
Epicoat EP-1001) 10 parts diaminodiphenylmethane, 100 parts clay, 40 parts glass fiber, 4 parts zinc stearate, 4 parts carbon black
The molding material is prepared by heating and kneading the raw material by pre-mixing the following parts and heating and kneading it in a conventional manner under the conditions of continuous rolls, that is, the roll temperature setting is 95°C on the high temperature side and 60°C on the low temperature side, raw material supply scale 16, sheet take-out scale 19. And so.

The temperature of the sheet taken out at this time was 77 to 86°C.

The variation in fluidity of this molding material was 27%, and the molding processability in the molding test mold was good.

Example 2 Using raw materials with the same composition as in Comparative Example 2, the roll temperature was set to 95°C on the high temperature side and 60°C on the low temperature side, and sheet take-out scale 19.
The raw material supply scale was adjusted so that the sheet temperature after heating and kneading was within the range of 79 to 82°C.

The raw material supply scale at this time was 17-23.

The variation in fluidity of this molding material was 5%, and the molding processability in the molding test mold was extremely good.

Comparative Example 3 As a raw material for diallyl phthalate resin material, 4 parts of t-butyl perbenzoate and 100 parts of glass fiber were used for 100 parts of diallyl phthalate resin (Daiso Tsubu A).
30 parts of charcoal, 4 parts of calcium stearate, and 4 parts of carbon black were premixed as a raw material, and as continuous rolling conditions, the roll temperature was set at 80°C on the high temperature side and 65°C on the low temperature side.
℃, a raw material supply scale of 17, and a sheet take-out scale of 35, the mixture was heated and kneaded by a conventional method to obtain a molding material.

The temperature of the sheet taken out at this time was 92 to 103°C.

The variation in fluidity of this molding material was 36%, and the molding processability in the molding test mold was at a good level.

Example 3 Using raw materials with the same composition as in Comparative Example 3, the roll temperature was set to 80°C on the high temperature side and 65°C on the low temperature side, and sheet take-out scale 35.
After heating and kneading, the raw material supply scale was adjusted so that the take-out sheet temperature was within the range of 97 to 100°C.

The raw material supply scale at this time was 13-20.

The variation in fluidity of this molding material was 5%, and the molding processability in the molding test mold was extremely good.

Comparative Example 4 As raw materials for unsaturated polyester resin, 10 parts of diallyl phthalate monomer, 3 parts of t-butyl perbenzoate, 100 parts of glass fiber, and 200 parts of charcoal were added to 1.00 parts of unsaturated polyester resin (ARP-240). Department,
4 parts of zinc stearate and 4 parts of carbon black are premixed as a raw material, and the continuous roll conditions are set, that is, the roll temperature is set at 95°C on the high temperature side and 70°C on the low temperature side, and the raw material supply scale is 1.
7. At the scale 35 at the sheet take-out position, the mixture was heated and kneaded in a conventional manner to obtain a molding material.

Note that the temperature of the sheet taken out at this time was 78 to 90°C.

The variation in fluidity of this molding material was 44%, and the moldability in the molding test mold was moderate.

Example 4 Using raw materials with the same composition as in Comparative Example 4, the roll temperature was set at 95°C on the high temperature side to 70°C on the low temperature side, and the sheet take-out scale was 35.
After heating and kneading, the raw material supply scale was adjusted so that the take-out sheet temperature was in the range of 83 to 86°C.

The raw material supply scale at this time was 14-25.

The variation in fluidity of this molding material was 5%, and the molding processability in the molding test mold was extremely good.

Claims (1)

[Claims] 1. A method for producing a thermosetting resin molding material, which comprises adjusting the amount of raw material supplied onto the kneading rolls in accordance with the sheet temperature in heating kneading using a continuous automatic roll system.