JPS5825573B2 - 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, the gist of this invention is to adjust the sheet take-out position in accordance with the sheet temperature in a continuous automatic roll type heating cross-wire system.

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.

In general, thermosetting resin molding materials are made by heating and kneading a mixture of various resins, curing agents, fillers, mold release agents, additives, etc. to have fluidity, curability, and fillability suitable for molding. It is processed and manufactured.

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 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.

Conventionally, as a method of controlling heating cross-wire conditions, samples are taken after the drying and pulverizing steps after heating and kneading, and characteristics such as fluidity are measured.The measurement results are used to determine the roll cross-wire conditions, such as roll temperature and roll surface. It was 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 kneading 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 method with a fast response speed, we found that the sheet temperature immediately before or immediately after being taken out from the roll corresponds to the material properties, not the material properties after manufacturing processing. We found that by adjusting the take-out position according to the sheet temperature, we were able to achieve rapid control and manufacture of uniform material.

A method for controlling heating crosstalk in a continuous automatic roll according to the present invention will be described in detail below.

First, measure the temperature of each part of the sheet wrapped around the roll, and at the position where the target specified temperature is reached, take out the sheet with a scraper to obtain the specified material, or at the position where the sheet temperature is constant. The second method is to take out the sheet while moving the take-out position and obtain a constant amount of material.

The scraper for taking out the sheet is structured to move in conjunction with the sheet temperature.

In the case of the continuous roll type, compared to the batch type, the heating and kneading on the roll is steady and changes continuously, and the continuous sheet can be taken out from the lower end of the wrapped sheet or from any location. The manufacturing method 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.

Compared to materials manufactured by conventional methods, materials manufactured by controlling the temperature of sheets that are continuously taken out have less variation in fluidity as a molding material (and have uniform and good molding processability). This has 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, we 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 a roll method, such as phenolic resins, epoxy resins, diallyl phthalate resins, and unsaturated polyester resins.
This will greatly contribute to technological advances that will enable the supply of high-quality products to the market.

Examples will be shown below.

Comparative Example 1 Phenol resin (
To 100 parts (usually novolak), 15 parts hexamethylenetetramine, 70 parts wood flour, 15 parts asbestos, 4 parts stearic acid, and 4 parts spirit black are premixed as raw materials, and the continuous roll conditions, i.e., roll temperature setting high temperature. 90°C - Low temperature 60°C 1 Raw material supply scale (corresponds to the supply speed) 17, sheet take-out scale (corresponds to the length from the raw material input port to the sheet take-out position) 10, heat and knead by the usual method to form a molding material. did.

The temperature of the sheet taken out during material production was 98 to 112°C, the variation in fluidity of this molding material was 34%, and the molding processability (fillability, hardenability) in the molding test mold was moderate. .

Example 1 Raw materials having the same composition as in Comparative Example 1 were heated and kneaded under continuous roll conditions, ie, roll temperature setting high temperature 90°C - low temperature 60°C, raw material supply scale (supply speed) 17.

As a result of adjusting the sheet take-out position so that the take-out sheet temperature during material production was within the range of 107 to 110°C, the scale of the sheet take-out position was 8 to 11.

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 As a raw material for an epoxy resin material, 10 parts of diaminodiphenylmethane, 100 parts of clay, and 4 parts of glass fiber were added to 100 parts of epoxy resin (Epicote EP~1001).
0 parts, 4 parts of zinc stearate, and 4 parts of carbon black were premixed as raw materials, and the conditions for continuous rolls were as follows: roll temperature setting high temperature 95°C - low temperature 60°C, raw material supply scale 16
, at sheet take-out scale 19, and heated and kneaded by a normal method to obtain a molding material.

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

Note that the temperature of the sheet taken out during material production was 77 to 86°C.

Example 2 Using raw materials with the same composition as in Comparative Example 2, heating and kneading were carried out under the same continuous roll conditions as in Comparative Example 2, including roll temperature settings and raw material supply scale, and the take-out sheet temperature during material production was 80 to 83. The sheet take-out position was adjusted so that it was within the range of ℃.

The scale of the sheet take-out position was 16 to 21.

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

3 As raw materials for diallyl phthalate resin material, 4 parts of 4-butyl perbenzoate and 100 parts of glass fiber are added to 100 parts of diallyl phthalate resin (Dyne-Dap A).
1 part, 30 parts of charcoal, 4 parts of calcium stearate, and 4 parts of carbon black were premixed as raw materials, and the roll temperature was set as continuous roll conditions: high temperature 80°C - low temperature 65°C1.
A molding material was prepared by heating and kneading in a conventional manner using a raw material supply scale 17 and a sheet take-out scale 35.

The variation in fluidity of this molding material was 36%, and the moldability (fillability, hardenability) in the molding test mold was moderate.

Note that the sheet temperature during material production was 92 to 103°C.

Example 3 Using the same raw materials as in Comparative Example 3, the continuous roll conditions were as follows: both the roll temperature setting and raw material supply scale were the same as Comparative Example 3.
Heat and knead under the same conditions as above until the sheet temperature is 97-10.
The sheet take-out position was adjusted so that the temperature was within the 0°C range.

At this time, the scale of the sheet take-out position was 30-36.

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

Example 4 As a raw material 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 calcium carbonate are used for 100 parts of unsaturated polyester resin (ABP-240).
1 part, 4 parts of zinc stearate, and 4 parts of carbon black were premixed as a raw material, and the continuous roll conditions were set at a high temperature of 95°C to a low temperature of 70°C, a raw material supply speed scale of 17, and a sheet take-out position of a scale of 35. The mixture was heated and kneaded using a conventional method to obtain a molding material.

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

Note that the sheet temperature during material production was 78 to 90'C.

Example 4 Using raw materials with the same pressure blend as in Comparative Example 4, heating and kneading was carried out under the same conditions as in Comparative Example 4, including the roll temperature setting and raw material supply scale, as continuous roll conditions, and the take-out sheet temperature was in the range of 81 to 84 ° C. I adjusted the sheet ejection position so that it would fit.

At this time, the scale of the sheet take-out position was 31 to 36.

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

Claims (1)

[Claims] 1. A method for producing a thermosetting resin molding material, which comprises adjusting the sheet take-out position in accordance with the sheet temperature in heating cross-tracking using a continuous automatic roll method.