RU2468054C1 - Method to produce compound - Google Patents

Abstract

FIELD: metallurgy.

SUBSTANCE: invention relates to the method for production of a heat resistant compound for sealing of electric radio engineering products. The compound contains an epoxide resin, a titanium-silicon-organic oligomer, a TMPT product, methyl tetrahydrophthalic or isomethyl tetrahydrophthalic anhydride, ground talc, ground dusty quartz and aluminium oxide. Epoxide resin and titanium-silicon-organic oligomer, the TMPT product, is heated. Talc, ground quartz and aluminium oxide are mixed in a ball mill for production of a homogeneous mass, then dried, introduced into a mixture of epoxide resin with titanium-silicon-organic oligomer, the TMPT product, and mixed. The mixture is cooled, and methyl tetrahydrophthalic or isomethyl tetrahydrophthalic anhydride melted at the same temperature is introduced into it. The compound is thoroughly mixed and vacuumised until active release of bubbles tops. After soaking in water, the compound is hardened in a thermal cabinet, then cooled with a thermal cabinet.

EFFECT: compound has increased mechanical tensile strength, increased specific impact viscosity, higher electric strength and specific volume resistance in an initial condition.

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Description

The present invention relates to the field of heat-resistant compounds used for sealing electrical and radio engineering products, such as transformer coils, chokes, etc.

The known compound [a.s. 535330, publ. 15.11.76], including epoxy diane resin, methyltetrahydrophthalic anhydride and a filler, characterized in that in order to increase the dielectric properties, specific impact strength and ensure thermal shock resistance from -60 to + 220 ° C, it additionally contains an organ titanium silicon oligomer of the general formula

where n = 2-5,

in the following ratio of components, parts by weight:

Epoxy Dianova Resin one hundred Organosilicon oligomer 10-40 Methyltetrahydrophthalic anhydride 25-40 Filler 200-220.

The production method consists in the fact that a filler (quartz, alumina, talc in a ratio of 2: 2: 1) is introduced into the mixture of ED-16 epoxy diane resin ED-16 and an organotitanium-silicon oligomer (TMFT product) heated at 30 ° C for 30 min. , cooled to 90 ° C and then methyltetrahydrophthalic anhydride is introduced, heated to 90 ° C. The compound was cured at 160 ° C for 8 hours with a stepwise rise in temperature and cooling.

However, this compound, prepared according to the above method, cannot be used for sealing large products due to large residual stresses (1.21 kgf / cm ² × deg), which can lead to cracking of products, especially after thermal shock from -60 to + 220 ° C.

A known method of obtaining a compound ETZ-16 [OST 4GO.054.213. Sealing of products of electronic equipment with polymeric materials] of the following composition, parts by weight:

Epoxy resin ED-16 one hundred TMFT Product 25 Methyltetrahydrophthalic or isomethyl tetrahydrophthalic anhydride 40 Talc ground 40 Powdered ground quartz 80 Alumina 80 Accelerator UP-606/2 0.3,

which consists in the fact that it is necessary to heat the epoxy resin ED-16 and the product TMPT to a temperature of (120 ± 10) ° C for 30 minutes Talc, ground quartz and alumina are mixed in a ball mill from 1.5 to 2 hours to obtain a homogeneous mass. The resulting mixture of fillers is dried at a temperature of 140 to 150 ° C for 2-3 hours. The mixture of fillers is introduced into the mixture of epoxy resin with the product TMPT at a temperature of (120 ± 10) ° C and mixed. The mixture is cooled to a temperature of (90 ± 10) ° С, methyltetrahydrophthalic or isomethyltetrahydrophthalic anhydride and the UP-606/2 accelerator are introduced at the same temperature. The compound is thoroughly mixed and vacuum at a temperature of from 90 to 100 ° C and a pressure of from 0.6 to 1.3 kPa until the active release of bubbles ceases, but not more than 30 minutes.

The compound is cured at a temperature of (100 ± 10) ° C - 1 h, then at a temperature of (120 ± 10) ° C - 1 h, then at a temperature of (140 ± 10) ° C - 1 h, then at a temperature of (160 ± 10) ) ° C - 3 hours

However, this method does not provide the necessary mechanical strength and specific impact strength, which is required to ensure thermal shock resistance of large-sized products. The insulating properties of the compound in wet conditions are insufficient for high-voltage products.

The technical result of the invention is:

- increase in mechanical tensile strength;

- increase in specific impact strength;

- increase in electric strength and specific volume resistance in the initial state and after exposure to water;

- increased resistance to surface partial discharges in difficult operating conditions (at 15% NaCl solution concentration, temperature (20 ± 5) ° C, ambient pressure 720 mmHg, humidity 100%, test voltage 5 kV eff . and an average electric field strength of 0.5 kV / cm).

The essence of the invention lies in the fact that the method of obtaining the compound, including, in parts by weight:

Epoxy resin ED-16 one hundred Organosilicon oligomer product TMFT 25 Methyltetrahydrophthalic or isomethyl tetrahydrophthalic anhydride 40 Talc ground 40 Powdered ground quartz 80 Alumina 80,

based on heating the epoxy resin ED-16 and the product TMPT to a temperature of (120 ± 10) ° C for 30 minutes, mixing talc, ground quartz and aluminum oxide in a ball mill from 1.5 to 2 hours to obtain a homogeneous mass, which then dried at a temperature of 140 to 150 ° C for 2-3 hours, then it is introduced into a mixture of epoxy resin ED-16 with an organotitanium oligomer TMFT product at a temperature of (120 ± 10) ° C and stirred, the mixture is cooled to a temperature of (90 ± 10) ° C and methyltetrahydrophthalic or isome melted at the same temperature is introduced into it ethyl tetrahydrophthalic anhydride, the compound is thoroughly mixed and vacuum at a temperature of 90 to 100 ° C and a pressure of 0.6 to 1.3 kPa until the active release of bubbles ceases, but no more than 30 minutes New in the proposed method is that the curing of the compound in a heating cabinet is carried out at a temperature of (100 ± 10) ° C for 2 hours, then at a temperature of (120 ± 10) ° C for 4 hours, then at a temperature of (140 ± 10) ° C - 4 hours, then at a temperature of (160 ± 10) ° С - 10 hours, then cooling - together with a heating cabinet.

To obtain the compound according to the claimed method, 100 g of ED-16 resin (GOST 10587-89) and 25 g of TMFT product (TU6-02-933-74) preheated to a temperature of (120 ± 10) ° C are introduced into the mixing tank and mixed at a temperature of (120 ± 10) ° C for 30 minutes The mixture is introduced pre-mixed in a ball mill for 1.5-2 hours and dried at 140-150 ° C for 2-3 hours; a mixture of fillers: 40 g of talc (TU21-25-159-79), 80 g of ground quartz pulverized (GOST 9077-82), 80 g of aluminum oxide (TU6-09-426-75). The mixture is cooled to a temperature of (90 ± 10) ° C and isomethyltetrahydrophthalic anhydride (TU6-10-124-91), preheated to (90 ± 10) ° C, is introduced into it. The mixture is evacuated at a temperature of (90-100) ° C and a pressure of from 0.6 to 1.3 kPa until the cessation of bubble formation, but not more than 30 minutes. Then the compound is cured at a temperature of (100 ± 10) ° C for 2 hours, then at a temperature of (120 ± 10) ° C for 4 hours, then at a temperature of (140 ± 10) ° C for 4 hours, then at a temperature of (160 ± 10) ° С - 10 hours, then cooled together with a heating cabinet.

Table 1 shows examples of the preparation of the compound of the claimed method.

Table 1 No. p / p the name of the operation Prototype Example 1 Example 2 Example 3 one Drying components, ° C / h 140-150 / 2-3 140/3 145/2 150/2 2 Warming up the components, ° С / h 120 ± 10/30 110/30 120/30 130/30 3 The temperature of mixing the components, ° C / h 90 ± 10 90 80 one hundred four Vacuum mode: - temperature, ° С / h 90-100 90 one hundred 95 - pressure, kPa 0.6-1.3 0.6 1,0 1.3 - time, min No more than 30 thirty twenty 2.5 5 Curing Mode, ° C / h 100 ± 10/1 h 100 ± 10/2 h 90 ± 10/2 h 110 ± 10/2 h 120 ± 10/1 h 120 ± 10/4 h 110 ± 10/4 h 130 ± 10/4 h 140 ± 10/1 h 160 ± 10/10 h 150 ± 10/10 h 170 ± 10/10 h 160 ± 10/3 h 6 Cooling - together with a heating cabinet

Table 2 shows the properties of the compound obtained by the claimed method and by the known OST 4GO.054.213.

table 2 No. p / p The properties Prototype Example 1 Example 2 Example 3 one The ultimate tensile stress (GOST 11262), kgf / cm ² 400 520 530 525 2 Specific impact strength (GOST 4647), kJ / m ² 10-15 twenty 21 23 3 Electric strength (GOST 6433.3), kV / mm: - in the initial state at 15-35 ° C 23 27 27 27.5 - after exposure to water for 48 hours at 15-35 ° C 22 25 25 26 four Volume resistivity (GOST 6433.2), Ohm × cm: - in the initial state at 15-35 ° C 1 × 10 ¹⁴ 8.7 × 10 ¹⁵ 8.8 × 10 ¹⁵ 8.5 × 10 ¹⁵ - after exposure to water for 48 hours at 15-35 ° C 1 × 10 ¹² 2.0 × 10 ¹⁵ 1.9 × 10 ¹⁵ 1.5 × 10 ¹⁵ 5 Resistance to surface partial discharges in difficult operating conditions, min 64.1 209.30 209.23 209.35

As can be seen from the tables, the claimed method provides:

- increase in mechanical tensile strength ("520 kgf / cm ² " versus "400 kgf / cm ² ");

- increase in specific impact strength ("20-23" kJ / m ² against "10-15" kJ / m ² );

- higher values of electric strength and specific volume resistance in the initial state and after exposure to water for 48 hours at (15-35) ° C;

- increased resistance to surface partial discharges in difficult operating conditions ("209.23 min" versus "64.1 min").

Claims (1)

A method of obtaining a compound, including, parts by weight:
Epoxy resin ED-16 one hundred Organosilicon oligomer product TMFT 25 Methyltetrahydrophthalic or isomethyl tetrahydrophthalic anhydride 40 Talc ground 40 Powdered ground quartz 80 Alumina 80,
based on heating the ED-16 epoxy and the TMFT product to a temperature of (120 ± 10) ° C for 30 minutes, stirring talc, ground quartz and aluminum oxide in a ball mill from 1.5 to 2 hours to obtain a homogeneous mass, which then dried at a temperature of 140 to 150 ° C for 2-3 hours, then it is introduced into a mixture of epoxy resin ED-16 with an organotitanium oligomer TMFT product at a temperature of (120 ± 10) ° C and stirred, the mixture is cooled to a temperature of (90 ± 10) ° C and methyltetrahydrophthalic molten at the same temperature is introduced into it or zometyl tetrahydrophthalic anhydride, the compound is thoroughly mixed and vacuum at a temperature of 90 to 100 ° C and a pressure of 0.6 to 1.3 kPa until the active release of bubbles ceases, but no more than 30 minutes, characterized in that the compound is cured in a heating cabinet at a temperature (100 ± 10) ° С - 2 hours, then at a temperature of (120 ± 10) ° С - 4 hours, then at a temperature of (140 ± 10) ° С - 4 hours, then at a temperature of (160 ± 10) ° С - 10 hours, then cooling - together with a heating cabinet.