RU1819269C - Method of polyamide plasticized composition preparing - Google Patents

Abstract

Usage: manufacturing products for structural purposes. SUMMARY OF THE INVENTION: after heating a reaction mixture of the following composition, parts by weight: dodecalactam 100; o-phthalatoethylenediamine copper 0.01-0.03; stabilizer 0,032-0,04; adipic acid 0.05-0.4; water 2.0-4.0; o-phosphoric acid 0.1-0.35, at 265-290 ° C under a pressure of 14 atm for 3 hours and then reducing the pressure to atmospheric, M-butylbenzenesulfonamide in an amount of 8-16 wt. .h. per 100 parts by weight dodecalactam. 1 s.p., 2 tab. with IS The aim of the invention is to increase the impact resistance of products during operation at low temperatures. The goal is achieved by heating the reaction mixture, including lactam. a copper complex of o-phthalic acid with ethylene diamine, a stabilizer is potassium iodide or magnesium chloride, a molecular weight regulator, and water, with dodeca00 ce os Os o co

Description

lactam, as a copper complex of ophthalic acid - o-phthalatoethylenediamine-copper, adipic acid as a molecular weight regulator and additionally introduce o-phosphoric acid in the following ratio of the components of the reaction mixture, wt.h .: Dodecalactam 100 o- Phthalatoethylenediamine-copper 0.01-0.03 Stabilizer 0.032-0.07 Adipic acid 0.05-0.4 Water 2.0-4.0 o-Phosphoric acid 0.1-0.35 and after heating the reaction mixture at N-butylbenzenesulfone is introduced at 265-290 ° C under a pressure of 14 atm for 3 hours and a subsequent decrease in pressure to atmospheric amide in an amount of 8-16 wt.h. 100 ma.ch. dodecalactam.

In addition, target additives are additionally added to the reaction mixture in an amount of 0.2-1.2 parts by weight of 100 May. dodecalactam.

The process is carried out as follows: the polymerization is carried out in a heated reactor with stirring at 265-290 ° C and a pressure of up to 14 atm, in the presence of water, a catalyst, a molecular weight regulator, o-phthalatoethylenediamine and additives. After reducing the pressure to atmospheric pressure when the polymer reaches a molecular weight of more than 5000, N-butylbenzenesulfonamide is introduced with stirring at a temperature of 265-275 ° C. The synthesis is carried out in an inert gas stream. The finished polymer is discharged through a die, cooled with water and granulated.

Standard samples were prepared from the polymer thus obtained for testing according to the following indicators:

- impact resistance according to Charlie on samples with a notch in accordance with GOST 4647-80;

- tensile strength according to GOST 11262-80.

- elongation at break according to GOST 11262-80.

The tubes were made using the operating method in the following processing mode:

- temperature of the material cylinder, ° C:

I zone - 180 ° C

II zone - 195 ° С ill zone - 200 ° С

- nozzle temperature - 180 ° C.

At the exit of the extruder nozzle, the tube was cooled by running water with a temperature of 18-22 ° C.

The tubes were tested for impact on 5 samples in accordance with TU 6-49-0203534-7-88 at temperatures of -40 ° C, -50 ° C, -60 ° C by acting on the sample

5 free-falling cargo. A tube sample was considered to pass the test if no cracks were found on it after impact. Table 1 shows the test results of the tubes depending on the formulation of the compositions.

Obtained according to this invention, the materials may contain various target additives, for example: antioxidants, heat stabilizers, flame retardants,

5 flame retardants, dyes, substances that enable the products to be removed from the mold, as well as fillers, such as fiberglass, talc, graphite, and others, introduced during or after synthesis.

0 Example 1.8 a reactor with a volume of 8 l, equipped with electric heating, a jacket with a coolant and a mixing device, is loaded with 3000 g (100 parts by weight) of dodecalactam, 90 g (3 parts by weight) of water, 6 g (0.2

5 parts by weight of orthophosphoric acid GOST 10678-76 as a catalyst, 12 g (0.4 parts by weight) of adipic acid GOST 10558-80 as a molecular weight regulator, 0.45 g (0.01 parts by weight) o-phthalatoethylenediamine

0 GOST 6-22-282-89 and as a target additive potassium iodide GOST 4232-74 in an amount of 1.2 g (0.04 parts by weight).

The temperature in the reactor was adjusted to 280-285 ° C. Vi kept under pressure

5 14 atm for 3 hours. Then the pressure is reduced to atmospheric for 1.5 hours. 3a due to heat removal due to evaporation of water, the melt temperature decreases to 265-270 ° C. At this temperature, with constant stirring, 240 g (8 parts by weight) of N-butylbenzenesulfonamide are introduced and the synthesis is continued for 3 hours in an inert gas stream. Then the polymer melt is discharged through a die in the form of a vein, cooled in water

5 bath and granulate.

The properties of the obtained material and products from it are presented in table. 1.

Examples 1-9 are carried out analogously to example 1.

Examples 1-5. In table 1 are made in accordance with the invention.

Examples 6–9 are given for comparison. The properties of materials and products made of them, made in accordance with the above examples, are given in Table 1.

In all these examples, 3 parts by weight were used. water, 0.2 wt.h. phosphoric acid and 0.4 wt.h. adipic acid.

Going beyond the declared ratios of less than 0.1: 8-16 leads to the production of material with lower impact resistance, not satisfying the requirements for this type of product, 0-phthalate diethylene copper in the amount of 0.04 wt.h. does not dissolve in the dodecalactam melt, and therefore it is not practical to make articles with such an amount of o-phthalatoethylenediamine.

Table 2 shows the test results of tubes for automobile brake systems made from the polymer composition obtained according to the invention. Tests were conducted according to TU 6-49-02003 534-7-88 according to paragraph 8.8. Tubes with a diameter of 12x1.5 and a length of 600 ± 10 mm were used as the test object. According to TU, impact tests were carried out at temperatures of min 40 ° C, minus 50 ° C, minus 60 ° C. Samples with a testing device were placed in a freezer with a holding temperature of 4 hours. The tubes were tested for impact by a free-flowing load with a spherical base with a radius of 16 mm and a mass of 450 g from a height of 300 mm. Preliminarily, the samples were tested for impact at room temperature. The following results were obtained, which supplement Table 1.

Claims (2)

1. Method for the preparation of a polyamide plasticized heating composition 5 0 5 0 we eat a reaction mixture including lactam, a complex of o-phthalic acid, ethylenediamine, a stabilizer - potassium iodide and magnesium chloride, a molecular weight regulator and water, characterized in that, in order to increase the impact resistance of products during operation during at low temperatures, dodecalactam is used as lactam, o-phthalatoethylenediamine copper is used as a copper complex of o-phthalic acid, adipic acid is used as a molecular weight regulator, and o-phosphoric acid is additionally introduced in the following ratio of the components of the reaction mixture, in parts by weight: Dodecalactam 100 o-Phthalatoethylenediamine-copper 0.01-0.03 Stabilizer 0.032-0.07 Adipic acid 0.05-0.4 Water 2.0-4.0 o-Phosphoric acid 0.1-0.35 after heating the reaction mixtures at 265-290 ° C under a pressure of 14 atm for 3 hours and then reducing the pressure to atmospheric, N-butylbenzenesulfonamide was introduced in an amount of 8-16 parts by weight. per 100 parts by weight dodecalactam. 2. The method according to claim 1, characterized in that target additives are additionally introduced into the reaction mixture in an amount of 0.2-1.2 parts by weight. per 100 parts by weight dodecalactam. I. Examples of the invention 0,07 P. Examples for comparison in Priide 9, in the synthesis “were used O.O. of copper acetate (GOST 5852-79) Magnesium chloride - GOST 7759-73 Carbon black - GOST 7885-79 Calcium carbonate - GOST 91 19-78 0.2 0 51 bj b5 i.9 and 350 360 380 360 360 b.r. b.r. b. R. 6.R. b.r. Note. Example 9 a plasticizer is released on the surface of articles. Table 2