WO2017066975A1

WO2017066975A1 - Process for preparing coloured flame retardant polyester fibre

Info

Publication number: WO2017066975A1
Application number: PCT/CN2015/092610
Authority: WO
Inventors: 黄怀光; 沈亚林; 陈少双; 王树江; 施纯亮
Original assignee: 揭东巴黎万株纱华纺织有限公司
Priority date: 2015-10-23
Filing date: 2015-10-23
Publication date: 2017-04-27

Abstract

Provided is a process for preparing a coloured flame retardant polyester fibre. The preparation process comprises the following steps: respectively drying and grinding a polyester fibre, a flame retardant and a colour masterbatch, mixing same in the following ratios: 70-80 parts by weight of the polyester fibre, 5-15 parts by weight of the flame retardant, and 1-5 parts by weight of the colour masterbatch, melting and stirring same until uniform, extruding same by a twin screw, spinning same by a spinning nozzle, cooling and forming same to obtain the coloured flame retardant polyester fibre, then after-finishing same, comprising winding and bundling, crimping, and balancing same by a fully-automatic high-speed winder, and finally sizing and drying same, and enhancing elasticity to obtain the finished product.

Description

Preparation process of colored flame retardant polyester fiber

Technical field

The invention relates to the technical field of chemical fiber textile flame retardant materials, in particular to a preparation process of colored flame retardant polyester fibers.

Background technique

Among the garments, decorations and industrial products used in textile materials, most of them require textiles to have flame retardant properties, such as children's clothing, special industry clothing, textile decorations for public places such as hotels and entertainment, and transportation. Textiles, packaging textiles, etc. Therefore, flame retardant textile materials have broad market application prospects and requirements. Due to its high strength, chemical resistance, weather resistance and dimensional stability, polyester materials are currently the largest fiber variety in production and production of chemical fibers, and one of the most widely used fiber varieties. However, since polyester fiber is a combustible fiber, which limits the application of polyester fiber in many aspects, it is desired and has been exploring and developing flame retardant polyester fiber.

There are many patented methods and literature reports on the flame retardant modification of polyester fibers. From the perspective of flame retardant varieties, there are mainly phosphorus and non-phosphorus flame retardants; from the point of view of addition methods, there are mainly copolymerization methods and Blending method; from the perspective of fiber manufacturing methods, there are mainly single-component spinning and composite component spinning. The flame retardant polyester fiber is obtained by using the above various methods, or is not suitable for the flame retardant modification of the colored polyester fiber of the raw liquid, or the obtained colored polyester flame retardant fiber has low strength, and is not suitable for producing high strength. Flame retardant fabric varieties.

Polyester fiber is traded in polyester and is an important variety in synthetic fibers. As an important raw material in the textile industry, polyester fiber has greatly alleviated the shortage of natural fiber. It has become the most abundant synthetic fiber in chemical fiber, and is widely used in clothing, decoration, home textiles, industrial textiles and national defense. Industrial engineering and other aspects. Polyester fiber can be made of pure textile or blended with natural fibers such as cotton, wool, silk and hemp, and other chemical fibers. It can process all kinds of imitation wool and imitation with many colors, easy to wash and dry, and free from ironing. Cotton, imitation silk and imitation linen. Most of the colored polyester fiber fabrics in the prior art are dyed after the polyester fibers are formed, which is difficult to dye, high in cost and not environmentally friendly. For example, the Chinese patent discloses a method for preparing a polyester fiber textile thread. The patent is to form a polyester fiber and then dye it, which is difficult to dye, and the subsequent processing technology is cumbersome, high in cost and not environmentally friendly. Chinese patent "Preparation method of colored flame retardant extinction hollow polyester filament", application number 200910303607.6, application date 2009-06-24, The patent solves the problem of difficulty in dyeing polyester. However, the cost of preparing the polyester filament according to the method of the present invention is high, and the spinnability of the polyester filament is deteriorated after the addition of the masterbatch and the matting agent, resulting in deterioration of the product quality.

How to obtain colored flame-retardant polyester fiber with high coloring effect and high flame retardancy, and the added additive can not adversely affect the spinnability, has been a problem that people are very concerned about.

Summary of the invention

The object of the present invention is to overcome the defects in the prior art and provide a preparation process of a colored flame-retardant polyester fiber, which is not only simple in method, low in pollution, good in coloring efficiency, and low in production cost. Moreover, the colored flame-retardant polyester fiber prepared by the preparation process has good flame retardant effect, high fiber strength, good color fastness and no pollution to the environment.

In order to achieve the above object, the present invention provides a process for preparing a colored flame-retardant polyester fiber, and the preparation steps thereof are as follows:

S1, drying: drying the polyester fiber, the flame retardant, and the masterbatch separately;

S2, grinding: the polyester fiber, the flame retardant, and the masterbatch dried by the step S1 are respectively ground into a powder in a vacuum drying environment, and used;

S3, mixing: the polyester fiber after the step S2 is used in a weight ratio of 70 to 80 parts, the flame retardant is 5 to 15 parts by weight, the masterbatch is divided into 1 to 5 parts by weight, and the mixture is stirred for 30 minutes. Evenly

S4, melting: the mixture after the step S3 is melted, and stirred well;

S5, spinning: the melt melted and stirred in step S4 is extruded from a double rotating screw, and spun by a spinneret and cooled to form a colored flame-retardant polyester fiber;

S6, finishing: the colored flame-retardant polyester fiber obtained in step S5 is wound by a fully automatic high-speed winder, bundled, crimped, and placed in a balance room for balance;

S7. Stereotype: The colored flame-retardant polyester fiber balanced in step S6 is shaped and dried, and subjected to bombing to obtain a finished product.

Further, the flame retardant in the step S1 is a polylactic acid flame retardant, which has a good biodegradation function and is beneficial to environmental protection.

Further, the polylactic acid flame retardant is prepared by melt copolymerization of melamine or a primary amine or o-phenylenediamine containing a benzimidazole structure with lactic acid.

Further, in the step S1, the masterbatch is in parts by weight, 60 parts by the carrier, and the toner 15 parts, 15 parts of dispersant, 4 parts of heat stabilizer, 4 parts of antibacterial agent, 4 parts of antioxidant, and 3 parts of additive. The antibacterial agent, the antioxidant and the additive are added to the masterbatch used in the invention, which can further strengthen the anti-aging property of the masterbatch, improve the antibacterial property of the masterbatch, and achieve the antibacterial and antibacterial effects.

Further, the carrier is a mixture carrier prepared from the following raw materials in parts by weight: 20 parts of polyolefin, 15 parts of polyterephthalate, and 10 parts of polyamide resin. Compared with the existing masterbatch, the mixed carrier enables synergistic effect between the mixed carrier and the dispersant and heat stabilizer, ensuring the stability of the material during processing and long-term outdoor use, and the mechanical properties of the material are more Preferably, the color masterbatch is used to achieve a uniform dispersion effect.

Preferably, the dispersing agent is any one of polyethylene wax, ethylene-vinyl acetate wax, ethylene bis-stearyl amide, and pentaerythritol stearate. The combination of various dispersing agents enables various dispersing agents and mixed carriers to be used in combination, which produces a synergistic effect, improves the dispersibility, coloring power, hiding power of the masterbatch, and has weather resistance, acid resistance and heat resistance. And cold resistance properties and maintain the chemical stability of the pigment.

Preferably, the heat stabilizer is epoxy glyceride, epoxy fatty ester, calcium stearate or zinc stearate; the antibacterial agent is chitosan, carboxymethyl chitosan or nano silver; The antioxidant is one or more of tea polyphenols, phytic acid, tocopherols, and flavonoids. Using natural antibacterial agents and natural antioxidants, the masterbatch is more environmentally friendly and healthier during use.

Further, in the step S1, the drying temperature is 110 to 120 ° C, and the drying time is 1 to 2 h. It is ensured that each raw material is dry and anhydrous before being mixed and melted, preventing the spinning process from interrupting the filament phenomenon.

Further, the ambient temperature of the vacuum drying in the step S2 is 110 to 120 ° C, and the polishing time is 1 to 2 h. Ensure that the raw materials are again absorbed and wet during the grinding process, causing the polyester fibers to break during the spinning process.

Further, the melting temperature in the step S4 and the temperature in the step S5 are constant at 280 ° C during the extrusion of the twin rotary screw. The temperature during the entire melting, stirring process and twin-screw extrusion process is strictly controlled at 280 ° C, which is beneficial to the preparation of the colored flame-retardant polyester fiber to maintain better spinnability and higher product quality.

The beneficial effects of the invention:

(1) In the preparation process of the colored flame-retardant polyester fiber of the present invention, the raw materials are sufficiently dried at the same time, and then all the raw materials are ground and pulverized in a dry environment, and uniformly mixed and then melted, so that the melted and spun before spinning The melt coloring is better and uniform, and the dispersion effect of the masterbatch is better. Prepared fiber spinning The performance is improved, the flame retardant effect is good, the decomposition temperature is high, the thermal stability is good, the dyeing performance is better, the color is better and brighter than the ordinary dyed fiber, and the color fastness is high.

(2) The invention adopts polylactic acid flame retardant, has good biodegradation function, is beneficial to environmental protection, non-toxic, non-corrosive, and has good flame retardant performance and long flame retardant effect period.

(3) The masterbatch used in the invention produces a synergistic effect between the mixed carrier and the mixed dispersant and the heat stabilizer, ensuring the stability of the material during processing and long-term outdoor use, and the mechanical properties of the material are better. The coloring of the color masterbatch is used to achieve uniform dispersion, and the prepared colored flame-retardant polyester fiber has improved spinning performance and good thermal stability.

(4) Since the antibacterial agent, antioxidant and additives are added to the masterbatch, the anti-aging property of the masterbatch can be further enhanced, the antibacterial property of the masterbatch is improved, and the antibacterial and antibacterial effects are achieved. The use of a plurality of dispersing agents allows a combination of various dispersing agents and a mixed carrier to produce a synergistic effect, improve the properties of the masterbatch, and improve the properties of the prepared fibers.

detailed description

Embodiments of the invention are described in detail below. It is to be understood that the following description is only illustrative, and is not intended to limit the scope of the invention.

Example 1

A preparation process of colored flame-retardant polyester fiber, the preparation steps are as follows:

S1, drying: drying polyester fiber, polylactic acid flame retardant and masterbatch, respectively, drying temperature is 110-120 ° C, drying time is 1 h, standby;

The polylactic acid flame retardant is prepared by melt copolymerization of melamine or a primary amine or o-phenylenediamine containing a benzimidazole structure with lactic acid;

The color masterbatch is composed of 60 parts by weight, 15 parts of toner, 15 parts of dispersing agent, 4 parts of heat stabilizer, 4 parts of antibacterial agent, 4 parts of antioxidant, and 3 parts of additive;

The carrier in the masterbatch is prepared from the following raw materials in parts by weight: 20 parts of polyolefin, 15 parts of polyterephthalate, and 10 parts of polyamide resin;

The dispersing agent in the masterbatch is any one of polyethylene wax, ethylene-vinyl acetate wax, ethylene bis-stearyl amide, and pentaerythritol stearate;

The heat stabilizer in the masterbatch is epoxy glyceride, epoxy fatty ester, calcium stearate or zinc stearate;

The antibacterial agent in the masterbatch is chitosan, carboxymethyl chitosan or nano silver;

The antioxidant in the masterbatch is one or more of tea polyphenols, phytic acid, tocopherol, and flavonoids;

S2: Grinding: The polyester fiber, the polylactic acid flame retardant and the masterbatch dried in the step S1 are respectively ground into a powder in a vacuum drying environment, and the vacuum drying environment temperature is 110 to 120 ° C, and the grinding time is 1h, spare;

S3, mixing: the weight fraction of the polyester fiber after the step S2 is 70 parts, the weight fraction of the flame retardant is 5 parts, the weight fraction of the masterbatch is 1 part, and the mixture is stirred for 30 minutes until uniform;

S4, melting: the mixture after the step S3 is melted, the melting temperature is constant at 280 ° C, and the mixture is sufficiently stirred at a constant temperature;

S5. Spinning: the melt after melt-stirring in step S4 is extruded by a double-rotating screw, and the temperature in the double-rotating screw extrusion process is constant at 280 ° C, and is sprayed by a spinneret and cooled to form a colored flame-retardant polyester. fiber;

Example 2

S1, drying: drying polyester fiber, polylactic acid flame retardant and masterbatch, respectively, drying temperature is 110-120 ° C, drying time is 1.5 h, standby;

S2: Grinding: The polyester fiber, the polylactic acid flame retardant and the masterbatch dried in the step S1 are respectively ground into a powder in a vacuum drying environment, and the vacuum drying environment temperature is 110 to 120 ° C, and the grinding time is 1.5h, spare;

S3, mixing: the weight fraction of the polyester fiber after the step S2 is 75 parts, the weight fraction of the flame retardant is 10 parts, the weight of the masterbatch is 3 parts, and the mixture is stirred for 30 minutes until uniform;

Example 3

S1, drying: drying polyester fiber, polylactic acid flame retardant and masterbatch, respectively, drying temperature is 110-120 ° C, drying time is 2 h, standby;

S2: Grinding: The polyester fiber, the polylactic acid flame retardant and the masterbatch dried in the step S1 are respectively ground into a powder in a vacuum drying environment, and the vacuum drying environment temperature is 110 to 120 ° C, and the grinding time is 2h, spare;

S3, mixing: the polyester fiber after the step S2 is 80 parts by weight, the flame retardant is 15 parts by weight, the masterbatch is 5 parts by weight, and the mixture is stirred for 30 minutes until uniform;

In order to verify whether the colored flame-retardant polyester fiber prepared by the present invention achieves the intended effect of the invention, the performance test of the colored flame-retardant polyester fiber prepared by the present invention is carried out, and the results are as follows:

It can be seen from the above table that the colored flame retardant polymer prepared by the present invention has a tensile strength of 4.3 cN/dtex, a tensile strength variation coefficient of 4.45%, and a tensile elongation of 24.6%. Ester fiber has good spinning performance, good stability, excellent flame retardant performance, long flame retardant effect, high color fastness, and better dyeing performance. The colored flame retardant polyester fiber is more colored than ordinary dyed fiber. Bright. At the same time, it also has antibacterial properties, achieving antibacterial and antibacterial effects.

It should be noted that the above-described embodiments are merely illustrative of the invention and are not intended to limit the embodiments. For those of ordinary skill in the art, the basis of the above description Other different forms of changes or changes can also be made. There is no need and no way to exhaust all of the implementations. Obvious changes or variations resulting therefrom are still within the scope of the invention.

Claims

A process for preparing a colored flame-retardant polyester fiber, characterized in that the preparation steps are as follows:

S1, drying: drying the polyester fiber, the flame retardant, and the masterbatch separately;

S2, grinding: the polyester fiber, the flame retardant, and the masterbatch dried by the step S1 are respectively ground into a powder in a vacuum drying environment, and used;

S3, mixing: the polyester fiber after the step S2 is used in a weight ratio of 70 to 80 parts, the flame retardant is 5 to 15 parts by weight, the masterbatch is divided into 1 to 5 parts by weight, and the mixture is stirred for 30 minutes. Evenly

S4, melting: the mixture after the step S3 is melted, and stirred well;

S5, spinning: the melt melted and stirred in step S4 is extruded from a double rotating screw, and spun by a spinneret and cooled to form a colored flame-retardant polyester fiber;

S6, finishing: the colored flame-retardant polyester fiber obtained in step S5 is wound by a fully automatic high-speed winder, bundled, crimped, and placed in a balance room for balance;

S7. Stereotype: The colored flame-retardant polyester fiber balanced in step S6 is shaped and dried, and subjected to bombing to obtain a finished product.
The process for preparing a colored flame-retardant polyester fiber according to claim 1, wherein the flame retardant in the step S1 is a polylactic acid flame retardant.
The process for preparing a colored flame-retardant polyester fiber according to claim 2, wherein the polylactic acid flame retardant is made of melamine or a primary amine or o-phenylenediamine containing a benzimidazole structure and lactic acid. Prepared by melt copolymerization.
The process for preparing a colored flame-retardant polyester fiber according to claim 1, wherein the color master batch in the step S1 is 60 parts by weight, 15 parts of a toner, and 15 parts by weight of the masterbatch. 4 parts of heat stabilizer, 4 parts of antibacterial agent, 4 parts of antioxidant, and 3 parts of additive.
The process for preparing a colored flame-retardant polyester fiber according to claim 4, wherein the carrier is a mixture carrier, and the mixture carrier is prepared from the following raw materials by weight: 20 parts of polyolefin 15 parts of polyterephthalate and 10 parts of polyamide resin.
The process for preparing a colored flame-retardant polyester fiber according to claim 4, wherein the dispersing agent is polyethylene wax, ethylene-vinyl acetate wax, ethylene bis-stearate, pentaerythritol stearate Any two of them.
A process for preparing a colored flame-retardant polyester fiber according to claim 4, wherein The heat stabilizer is epoxy glyceride, epoxy fatty ester, calcium stearate or zinc stearate; the antibacterial agent is chitosan, carboxymethyl chitosan or nano silver; The antioxidant is one or more of tea polyphenols, phytic acid, tocopherols, and flavonoids.
The process for preparing a colored flame-retardant polyester fiber according to claim 1, wherein the drying temperature in the step S1 is 110 to 120 ° C, and the drying time is 1 to 2 h.
The process for preparing a colored flame-retardant polyester fiber according to claim 1, wherein the ambient temperature of the vacuum drying in the step S2 is 110 to 120 ° C, and the grinding time is 1 to 2 h.
A process for preparing a colored flame-retardant polyester fiber according to claim 1, wherein the melting temperature in the step S4 and the temperature in the step S5 are constant at 280 ° C during the extrusion of the twin rotary screw.