KR20020048783A - Process of preparing a polyamide 6 fibre endurable against heat and light - Google Patents

Abstract

PURPOSE: A process of preparing polyamide 6 by adding a specified amount of a hindered amine light stabilizer(HALS) composition having a chain similar to a main chain to polyamide 6 is provided. The product obtained by this process exhibits excellent light resistance and heat resistance and colored goods thereof have excellent light fastness. CONSTITUTION: A hindered amine light stabilizer compound represented by formula(I) is added in an amount of 0.1 to 3.0% by weight, based on the weight of polyamide 6. In formula, R is C1-7 alkyl or C1-7 alkoxy. For example, 100% by weight of polyamide 6 chips having a moisture content of 80ppm or less are mixed with 1.0 to 30.0% by weight of the compound of the formula(I) to produce a master batch, which is mixed with polyamide 6 in a ratio of 1:9 and then melt-spun.

Description

Process for preparing a polyamide 6 fiber endurable against heat and light

The present invention relates to a process for producing polyamide 6 fibers having excellent heat resistance and light resistance while increasing productivity.

The reason why the polyamide fibers are discolored by heat or light or change in physical properties can be interpreted as the radicals formed by the heat or light of the polymer chain of the polyamide are decomposed by a chain reaction.

During this process, the production of hydroperoxides is of great importance, as a result of which the main chain of polyamide is decomposed.

In order to alleviate this process, there are two main compounds commonly used as stabilizers.

The first is inorganic stabilizers such as metal copper compounds and manganese compounds, and the second is organic stabilizers with steric hindrance.

However, after dyeing the nylon and testing the light resistance, an experimental result showed that the organic-based stabilizer is superior in terms of the strong residual rate and the light fastness than the inorganic type.

In addition, as a conventionally developed technique, a method for producing polyamide using an organic Halz system of EP 97/43335 is known.

However, when the Benzegori alone was used, the chip remained noticeably yellowed.

The present invention significantly improves the disadvantages of the prior art as described above, and by adding a certain equivalent of Hals having a chain similar to the main chain to polyamide 6, polyamide 6 fibers having excellent heat resistance and light resistance can be produced. The technical task is to provide a method for manufacturing with excellent workability.

According to the present invention, a polyamide 6 chip having a moisture content of 80 ppm or less and a compound having structural formula (I) having a moisture content of 80 ppm or less dried for 10 hours after setting at a relative viscosity of 2.7 to 3.0 and a temperature of 110 DEG C are 1.0 to 100 weight of polyamide 6. ~ 30.0% by weight to prepare a masterbatch.

After compounding using a compounding machine, hindered amine Hals is added as a light and heat stabilizer.

The masterbatches thus prepared are mixed to melt spinning so that the ratio of polyamide 6 to masterbatch is 9: 1 to adjust the content of 0.1 to 3.0% by weight for polyamide 6 fibers.

R is C 1-7 alkyl or C 1-7 alkoxy.

The additive of Structural Formula (I) is added in an amount of 0.1 to 3.0% by weight based on the total amount of polyamide 6.

At this time, the method of adding compound of Structural Formula (I), which is a light and heat stabilizer, can be divided into three types. First, the method is added during polymerization, and the second is the method used when drying chips after polymerization. Or a method of injecting during spinning.

In the case of the present invention, a method of mixing the polyamide in the molten state with the additive of formula (I) in an extruder before spinning was used.

When the content of the additive is less than 0.1% by weight, it does not show any effect as a stabilizer. When the content of the additive exceeds 3.0% by weight, the yellowing of the polyamide becomes severe, resulting in problems in workability and quality.

Polyamide 6 blended in an extruder fixed with two static mixers and one dynamic mixer at the edge of a 30 mm screw is melt spun at 270 to 300 ° C. and then passed through a spinneret. Stretching is carried out between the roller and the stretching roller.

The filament yarn passed through the drawing roller is wound up through two gourd rollers at a speed of 4000 m / min in the final winder.

<Property test method>

(1) viscosity

Viscosity measurement was performed with a Uberod viscometer, and the viscosity value was given as a relative viscosity.

(2) light stability

The strength loss is measured after the yarns are fixed in the metal frame using QUV, a weather resistance promoting tester, exposed to ultraviolet rays at 60 ° C. for 200 hours.

(3) strength

The filament yarn was tested according to the test method for strength and elongation. The test conditions were 20cm in sample length and 200m / min in tensile speed.

(4) daylight fastness

Daylight fastness tests were carried out on Xenotest, where the drawn thread was fixed to a metal frame.

Exposure to 50, 100, and 200 hours of light, respectively.

The strength loss was measured after this time interval.

(5) thermal stability

To determine the thermal stability, the fibers were subjected to an oven test under conditions such as in air at 180 ° C., 190 ° C., and 200 ° C. for one hour.

Physical properties such as color change and intensity were measured.

Example 1

1. Prepare a polyamide 6 masterbatch containing 5% by weight of a hindered amine Hals compound of formula (I), wherein R is a methoxy group.

② Melt spinning is carried out by mixing the masterbatch made in ① in 1 ratio with respect to polyamide 6 9.

At this time, the winder speed is 4000m / min.

Example 2

A masterbatch was prepared as in Example 1 but containing 10 wt% of a hindered amine Hals compound.

Comparative Example 1

As in Example 1, but without using the masterbatch of the hindered amine Hals compound was melt-spun using only polyamide 6.

The results were as in Tables 1 to 4.

TABLE 1

division RV before UV treatment RV after UV treatment Comparative Example 1 2.74 2.45 Example 1 2.70 2.62 Example 2 2.66 2.63

TABLE 2

division Intensity decrease by light (cN / tex) 0 hours 50 hours 100 hours 200 hours Comparative Example 1 50.6 47.8 44.9 37.8 Example 1 53.4 53.0 52.2 48.9 Example 2 53.8 53.7 54.5 52.4

Note) The fibers used here are all 45 deniers of 6 polyamides.

TABLE 3

division Color fastness after UV treatment Sandalwood Dye Comparative Example 1 Level 3 2nd class Example 1 Grade 5 Grade 4 Example 2 Grade 5 Grade 5

Dyeing condition: dye Tectiron (3combi), liquid ratio 16.689: 1

owf (yellow 0.032, blue 0.0178, red 0.015)

TABLE 4

division Strength drop by heat (cN / tex) Room temperature 180 ℃ 190 ℃ 200 ℃ Comparative Example 1 50.6 40.1 34.5 23.2 Example 1 53.4 47.7 42.2 35.3 Example 2 53.8 48.1 42.9 34.4

Note) The fibers used here are all 45 denier of polyamide 6 yarn.

The polyamide 6 fiber produced according to the present invention exhibits excellent light resistance and heat resistance, and also has excellent daylight fastness of the dye.

Claims (1)

A method for producing a polyamide 6 fiber having excellent heat and light resistance, characterized by adding 0.1 to 3.0% by weight of a hindered amine-based Hals compound represented by the following structural formula (I) based on the weight of polyamide 6. -Below- R is C 1-7 alkyl or C 1-7 alkoxy.