JPS5850161B2 - 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 roll temperature conditions 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 is free from variations in these properties.

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

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

In particular, a continuous heating kneading roll is excellent in terms of productivity.

In heating and kneading with rolls, chemical reactions, drying, homogenization, and densification proceed simultaneously, and the extent of these changes all affect the quality and variation of the material's fluidity and moldability. It was difficult to reproduce exactly the same condition, which was a problem with the manufacturing method.

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

Traditionally, as a method to manage heating cross-wire conditions, samples are collected after the drying and pulverizing processes after heating cross-wire, and characteristics such as fluidity are measured.The measurement results are used to determine the roll cross-wire conditions, such as roll temperature, roll surface temperature, etc. It was common to control the sheet take-out position or the amount of material charged on 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 kneading position and the fluidity measurement time, and it is impossible to control the material evenly down to minute units. Met.

The present invention aims to solve this drawback, and as a result of studying a material with a fast mandrel speed, we found that the sheet temperature immediately before or immediately after taking it out from the roll corresponds to the material property, not the material property after manufacturing processing. We found that by appropriately controlling the roll temperature of the mixed wire roll in accordance with this sheet temperature, we confirmed that it is possible to make the fluidity and moldability of the material and their variations uniform.

In order to complete the technology of the present invention, it is necessary to quickly control the roll temperature in accordance with the sheet temperature. Therefore, the conventional bore trawl method was replaced with a drill trawl method to control the roll surface temperature. Temperature control made easy.

The bore roll method is a method in which the heating medium for roll heating is passed only through the center of the roll, and because the heat transfer area is small and the response is slow, it is extremely difficult to quickly and keep the roll surface temperature constant.

On the other hand, by adopting the drill trawl method, it is possible to provide a large number of heat medium conduction ports near the roll surface, thereby increasing the heat transfer effect and quickly controlling the roll temperature.

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

First, the temperature of each part of the sheet wrapped around the roll is measured, and the roll temperature is controlled so that the sheet temperature at the sheet removal position reaches the specified target temperature, and the conditions are set by moving the sheet removal scraper. do.

Once the roll conditions for heating and kneading are stable, the sheet take-out position is fixed and continuous production begins.

The temperature of the sheet on the roll varies depending on the amount of material to be fed.

In the case of a continuous roll type, compared to a batch type, the heating and kneading on the roll is steady and changes 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, it is discontinuous and the temperature varies depending on the portion of the sheet, and 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 usual 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 produced by a roll method. As a result of examining the effects of applying these manufacturing methods, it was found that a molding material with less variation, uniformity, and good moldability could be obtained compared to when manufactured using a conventional method.

The technology of the present invention can be applied to thermosetting resins that can be manufactured by roll method, such as phenol resins, epoxy resins, diallyl phthalate resins, unsaturated polyester resins, etc., and enables the supply of high-quality products to the market. This will greatly contribute to the advancement of technology.

Examples will be shown below.

Comparative Example 1 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 pre-mixed to 100 parts (normal novolak), and the continuous rolling conditions, i.e., roll temperature setting, are prepared. The mixture was heated and kneaded in the usual manner at a temperature of 90°C on the high temperature side and 60°C on the low temperature side, with a raw material supply scale (corresponding to the supply speed) of 17 and a sheet withdrawal scale (corresponding to the length from the raw material input port to the sheet withdrawal position) of 10. It was 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 Using raw materials with the same composition as in Comparative Example 1, raw material supply scale 17
, the sheet was heated and kneaded with a sheet take-out scale of 10, and the roll temperature was adjusted so that the take-out sheet temperature was in the range of 107 to 110°C.

The roll temperature at this time was 85 to 100°C on the high temperature side and 55 to 70°C on the low temperature side.

The variation in fluidity of this molding material was 6 degrees, 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 fluidity variation of this molding material was 27φ, and the molding processability in the molding test mold was at a good level.

Example 2 Using raw materials with the same composition as in Comparative Example 2, raw material supply scale 16,
The sea urchin and roll temperature were adjusted so that the sheet take-out scale 19 was heated and kneaded, and the take-out sheet temperature fell within the range of 79 to 82°C.

The roll temperature at this time was 80 to 100°C on the high temperature side and 65 to 75°C on the low temperature side.

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

Comparative Example 3 For 100 parts of diallyl phthalate resin (Daiso Tsubu A) as a raw material for diallyl phthalate resin material,
A premix of 4 parts of t-butyl perbenzoate, 100 parts of glass fiber, 30 parts of charcoal, 4 parts of calcium stearate, and 4 parts of carbon black was used as a raw material, and the roll temperature was set at 80°C on the high temperature side and on the low temperature side as continuous rolling conditions. 65℃
, a raw material supply scale 17, and a sheet take-out scale 35, the mixture was heated and kneaded in a conventional manner 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 degrees, 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, raw material supply scale 17
The roll temperature was adjusted so that the temperature of the sheet taken out after heating and kneading as the sheet take-out scale 35 was within the range of 97 to 100°C.

The roll temperature at this time is high temperature side 80~90℃ - low temperature side 6
The temperature was 0-70°C.

The fluidity of this molding material varied by more than 5, and the molding processability was extremely good.

Comparative Example 4 As raw materials for unsaturated polyester resin, for 100 parts of unsaturated polyester resin (ABP-240), 10 parts of diallyl slate monomer, 3 parts of -butyl perbenzoate, 100 parts of glass fiber, 200 parts of charcoal, 4 parts of zinc stearate and 4 parts of carbon black were premixed as raw materials, and continuous roll conditions, that is, roll temperature settings were 95°C on the high temperature side and 70°C on the low temperature side, raw material supply scale 17, and sheet take-out position scale 35. The mixture was heated and kneaded using a conventional method 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 factors, and the moldability in the molding test mold was moderate.

Example 4 Using raw materials with the same composition as in Comparative Example 4, raw material supply scale 17,
The sheet was heated and kneaded as the sheet take-out scale 35, and the roll temperature was adjusted so that the take-out sheet temperature fell within the range of 81 to 84°C.

The roll temperature at this time was 85 to 100°C on the high temperature side and 65 to 80°C on the low temperature side.

The variation in fluidity of this molding material was 6 factors, and the molding processability was extremely good.

Claims (1)

[Claims] 1. In heating kneading using a continuous automatic roll method using a drill trol, the temperature of the sheet wrapped around the roll is measured, and the roll temperature is controlled so that the sheet temperature at the sheet take-out position reaches the target specified temperature.
A method for producing a thermosetting resin molding material, the method comprising taking out a sheet using a scraper for taking out the sheet.