JPS61145216A - Production of water-soluble phenolic resin for laminate - Google Patents

Abstract

PURPOSE:To produce in good yields a water-soluble phenolic resin for laminates having a high rate of curing, by using a tert. amine having a b.p. in a specified range as a catalyst. CONSTITUTION:The desired water-soluble phenolic resin is obtained by using a tert. amine having a b.p. which ranges from the reaction temperature at which the water-soluble phenolic resin is formed to the drying temperature used in the later production of laminates as a catalyst. As regards the boiling point range of the catalyst, the reaction temperature for producing the resin is usually 60-100 deg.C and the drying temperature is usually 140-160 deg.C where steam is used and, therefore, it can be selected from ranges therebetween, depending on the system used.

Description

DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for producing a water-soluble phenolic resin for laminates.

Conventional technology In recent years, with the development of electronic devices, laminates and copper-clad laminates used in electronic devices, etc. have become more sophisticated in order to reduce the insulation spacing and increase the density of punched holes due to the miniaturization of products. electrical properties and punchability are required.

In order to improve the electrical properties and punchability of a laminate, a two-step method for impregnating the base material with resin is usually most effective. That is, in the first step, the paper base material was impregnated with a water-soluble phenolic resin of relatively low molecular weight that has good affinity with the paper base material, and then dried, and then in the second step, it was modified with natural dry wax etc. This method involves impregnating a phenolic resin and drying it to obtain a laminated material for a laminated board.

A tertiary amine is usually used as a catalyst for obtaining the water-soluble phenolic resin for the first stage. In other words, catalysts containing metal ions cannot be used as insulating resins for laminated boards, and if ammonia, primary, or secondary amines are used as catalysts, they themselves will not participate in the reaction. , it is unsuitable because it produces a polymer and loses its water solubility.

Problems to be Solved by the Invention However, the disadvantages of using tertiary amines are that the reaction rate is slow and unreacted phenol tends to remain; Because it easily volatizes, the hardening rate in the drying process becomes slow after impregnating the base material with the water-soluble resin. This results in a decrease in yield and a decrease in production speed during actual mass production.

The object of the present invention is to improve the above-mentioned drawbacks, to produce a water-soluble phenolic resin suitable for laminates with good yield, and to produce one that has a fast curing speed.

Means for Solving the Problems In order to achieve the above objects, the present invention is directed to the production of a water-soluble phenolic resin for laminates, in which the boiling point of the catalyst is higher than the resin production reaction temperature and the drying process is carried out after the production of the laminate material. It is characterized by using a tertiary amine whose temperature is below.

Function In the present invention, during the resin reaction, the catalyst has a boiling point higher than the temperature of the reaction system, so the amount present in the system is larger than conventional low boiling point catalysts, and the effective amount for promoting the reaction is large. ,
In the process of impregnating the base material with this water-soluble phenolic resin and drying it, the time required for the catalyst to volatilize is longer than that of a low boiling point catalyst, which also promotes the curing reaction. have an effect. However, the catalyst ultimately
Since all of the amine evaporates, there is no adverse effect due to the amine remaining.

The boiling point range of the catalyst is generally within the range of resin reaction temperature from 60 to
100°C1 or when using steam, the drying temperature is 14
0 to 160''C, and can be selected within that range depending on the system.

Example Next, the present invention will be explained in detail.

Example 1 Phenol 610F in a Mitsuro flask equipped with a stirrer, thermometer, and condenser! -, 37% formali 71055', 8
6% paraform 407y-, triethylneamine (b,
p, 89.5°C) 19.2 S12 was added and reacted at 80'C for 4 hours.

When the gelation time on the 160°C heating plate reached 3 minutes, it was cooled, and when the temperature reached 50"C, methanol was added.
Adjust the resin content to 50 cm (referred to as varnish A).

Next, 720% tung oil, 580 p' of m-cresol, and 074 P of P"'f" S acid were added to the same flask, and after reacting at 80°C for 1 hour, 500% of phenol, 86
Chiparaform 45051-125 Thiammonia water 357
was added, reacted at 80"C, dehydrated when the gelation time reached 6 minutes on a 160°C heating plate, and then added methanol to adjust the resin content to 50%. Obtained a statement (referred to as varnish B).

Apply varnish A to 11 mils kraft paper so that the resin content is 20 yen. After drying at 140'C for 5 minutes, impregnate varnish B so that the total resin t (varnish A + varnish B) is 50%. Dry. After reaching a predetermined degree of hardening, the 8 sheets of the obtained laminate material are overlaid with 35 μm adhesive-coated copper foil on one side, heated and pressed, and a 1.6 m thick copper-clad laminate is formed. Obtained.

Comparative Example 1 In the same apparatus as in Example 1, phenol 61°7137% formalin 1051.86 tiparaform 407Li-,)
Limethylamine (b, p3, 2-3.8°Cat74
7w + Hg) 30% aqueous solution 647 was added and reacted at 80°C for 4 hours, then cooled when the gelation time on a 160°C heating plate reached 3 minutes, and when the temperature reached 50°C. Add methanol and adjust the resin content to 50 g (referred to as varnish C).

Varnish 0 and Varnish B were applied to kraft paper in the same manner as in the example.
were impregnated and dried in order to obtain a copper-clad laminate having a thickness of 1.6 fi.

Table 1 shows the characteristics of varnishes A and 0 obtained in Example 1 and Comparative Example 1 and the drying time during the laminate manufacturing process.

Table 1 Effects of the invention The water-soluble phenolic resin obtained from the invention (2) is
As can be seen in the table, its industrial value is extremely great in that it increases solid yield and curing rate, and is effective in improving material yield and productivity in the manufacture of laminates.

Claims (1)

[Claims] A water-soluble phenol resin for laminates, characterized in that a tertiary amine whose boiling point is higher than the resin production reaction temperature and lower than the drying temperature for subsequent production of laminate materials is used as a catalyst in the production of water-soluble phenolic resin for laminates. Method for producing phenolic resin.