阅读说明：本技术 阻燃微米丝复合超细纤维及其制备方法 (Flame-retardant micron-silk composite superfine fiber and preparation method thereof ) 是由 余三川 雷太林 于 2020-12-31 设计创作，主要内容包括：本发明公开了一种阻燃微米丝复合超细纤维及其制备方法,包含以下重量份组成：阻燃剂1-4份、聚酯类高分子50-70份、聚酰胺类高分子20-50份,其特征是所述聚酯类高分子是聚对苯二甲酸乙二醇酯或聚对苯二甲酸丁二醇酯；所述聚酰胺类高分子是尼龙6、尼龙66、尼龙46、尼龙610、尼龙612和尼龙12中的一种。发明提供一种阻燃微米丝复合超细纤维,其纤维中的阻燃剂不含卤素成分阻燃剂,产品使用安全,强力损伤小适于后续的纤维加工,燃烧后不会影响使用者健康甚至生命安全,阻燃剂在纤维中分散效果好,工艺简单,操作方便,而且无污染,有利于保护环境。(The invention discloses a flame-retardant micrometer filament composite superfine fiber and a preparation method thereof, wherein the flame-retardant micrometer filament composite superfine fiber comprises the following components in parts by weight: 1-4 parts of flame retardant, 50-70 parts of polyester polymer and 20-50 parts of polyamide polymer, and is characterized in that the polyester polymer is polyethylene terephthalate or polybutylene terephthalate; the polyamide polymer is one of nylon 6, nylon 66, nylon 46, nylon 610, nylon 612 and nylon 12. The flame retardant in the fiber does not contain a halogen component flame retardant, the product is safe to use, the strong damage is small, the product is suitable for subsequent fiber processing, the health and even life safety of a user cannot be influenced after combustion, the flame retardant has a good dispersion effect in the fiber, the process is simple, the operation is convenient, no pollution is caused, and the environment is protected.)

1. The flame-retardant micrometer filament composite superfine fiber comprises the following components in parts by weight: 1-4 parts of flame retardant, 50-70 parts of polyester polymer and 20-50 parts of polyamide polymer, and is characterized in that the polyester polymer is polyethylene terephthalate or polybutylene terephthalate; the polyamide polymer is one of nylon 6, nylon 66, nylon 46, nylon 610, nylon 612 and nylon 12.

2. A preparation method of flame-retardant micrometer-filament composite superfine fiber is characterized by comprising the following steps:

step one, vacuum drying: drying polyester polymer and polyamide polymer at 60-160 deg.C for 8-24 hr;

step two, melt spinning: adopting a melt spinning method, melting and mixing polyester polymer and polyamide polymer melt, then extruding and drawing, cooling by circular blowing, bundling and oiling, drafting and winding to prepare micron-yarn composite pre-oriented yarn;

step three, false twist texturing: drawing, false twisting and deforming the micron silk composite pre-oriented yarn to prepare micron silk composite fiber, carrying out flame retardant treatment on the micron silk composite fiber by using a flame retardant to obtain flame-retardant micron silk composite fiber, and preparing flame-retardant micron silk composite superfine fiber by using an alkali treatment ultrasonic fiber opening method; the alkali treatment ultrasonic fiber opening method comprises the following steps: weighing a certain amount of the micrometer-grade composite fiber, preparing a sodium carbonate/acetone solution with the content of 1mol/L, performing alkali treatment and ultrasonic fiber opening in a normal-temperature environment, then performing water washing, acid washing and water washing to neutrality, drying, and enabling the diameter of the flame-retardant micrometer-grade composite superfine fiber to be 0.1-5 micrometers after fiber opening; the ultrasonic power of the alkali treatment ultrasonic fiber-opening method is 500w, the time is 20 minutes, the bath ratio is 1:100, and acetic acid solution is adopted for acid cleaning.

3. The method for preparing the flame-retardant micron-sized silk composite superfine fiber according to claim 2, wherein the flame-retardant treatment of the micron-sized silk composite superfine fiber by the flame retardant is as follows: adopting a flame retardant consisting of 40-50 parts of sodium tungstate, 30-60 parts of sodium molybdate, 20-30 parts of tartaric acid and 20-30 parts of citric acid; and (3) putting the micrometer silk composite fiber in an environment with the temperature of 70-100 ℃ and the pH value of 3-5, and soaking and boiling the micrometer silk composite fiber in a flame retardant water solution with the ratio of flame retardant to water of 1:30-1:25 for 10-15 minutes to obtain the flame-retardant micrometer silk composite fiber.

4. The method for preparing the flame-retardant micron-sized composite superfine fiber according to claim 3, wherein the melt spinning process comprises the following process parameters: the melt spinning temperature is 270-280 ℃, the annular blowing air speed is 0.45 +/-0.05 m/min, the annular blowing temperature is 23-25 ℃, the annular blowing humidity is 35-45RH percent, the drafting multiple of POY is 1.5-2.0 times, the spinning speed of POY is 2800-3500m/min, the drafting multiple of FDY is 3.0-4.5 times, and the spinning speed is 4000-4800 m/min.

Technical Field

The invention relates to the technical field of chemical fibers, in particular to a flame-retardant micron-silk composite superfine fiber and a preparation method thereof.

Background

The flame-retardant fiber is a fiber which is only smoldered in flame, does not generate flame per se, is separated from the flame, and is self-extinguished by smoldering, and is widely applied to clothes, home furnishings, decorations, non-woven fabrics, fillers and the like. Compared with common fibers, the flame-retardant fibers have obviously reduced flammability, obviously slowed combustion rate in the combustion process, quick self-extinguishment after leaving a fire source and less release of toxic smoke. The traditional halogen flame retardant can generate suffocating toxic gas during combustion, and influences the health and life safety of users.

Disclosure of Invention

The invention aims to solve the technical defects and provide the flame retardant micrometer filament composite superfine fiber which does not contain halogen components, is safe, has small strength damage, is suitable for subsequent fiber processing, has simple process, small flame retardant addition amount and no environmental pollution and the preparation method thereof.

In order to achieve the purpose, the flame-retardant micrometer filament composite superfine fiber provided by the invention comprises the following components in parts by weight: 1-4 parts of flame retardant, 50-70 parts of polyester polymer and 20-50 parts of polyamide polymer, and is characterized in that the polyester polymer is polyethylene terephthalate or polybutylene terephthalate; the polyamide polymer is one of nylon 6, nylon 66, nylon 46, nylon 610, nylon 612 and nylon 12.

The invention provides a preparation method of flame-retardant micrometer filament composite superfine fiber, which comprises the following steps:

step one, vacuum drying: drying polyester polymer and polyamide polymer at 60-160 deg.C for 8-24 hr;

step two, melt spinning: adopting a melt spinning method, melting and mixing polyester polymer and polyamide polymer melt, then extruding and drawing, cooling by circular blowing, bundling and oiling, drafting and winding to prepare micron-yarn composite pre-oriented yarn;

step three, false twist texturing: drawing, false twisting and deforming the micron silk composite pre-oriented yarn to prepare micron silk composite fiber, carrying out flame retardant treatment on the micron silk composite fiber by using a flame retardant to obtain flame-retardant micron silk composite fiber, and preparing flame-retardant micron silk composite superfine fiber by using an alkali treatment ultrasonic fiber opening method; the alkali treatment ultrasonic fiber opening method comprises the following steps: weighing a certain amount of the micrometer-grade composite fiber, preparing a sodium carbonate/acetone solution with the content of 1mol/L, performing alkali treatment and ultrasonic fiber opening in a normal-temperature environment, then performing water washing, acid washing and water washing to neutrality, drying, and enabling the diameter of the flame-retardant micrometer-grade composite superfine fiber to be 0.1-5 micrometers after fiber opening; the ultrasonic power of the alkali treatment ultrasonic fiber-opening method is 500w, the time is 20 minutes, the bath ratio is 1:100, and acetic acid solution is adopted for acid cleaning.

The flame retardant treatment of the micron silk composite fiber by the flame retardant comprises the following steps: adopting a flame retardant consisting of 40-50 parts of sodium tungstate, 30-60 parts of sodium molybdate, 20-30 parts of tartaric acid and 20-30 parts of citric acid; and (3) putting the micrometer silk composite fiber in an environment with the temperature of 70-100 ℃ and the pH value of 3-5, and soaking and boiling the micrometer silk composite fiber in a flame retardant water solution with the ratio of flame retardant to water of 1:30-1:25 for 10-15 minutes to obtain the flame-retardant micrometer silk composite fiber.

The melt spinning process comprises the following process parameters: the melt spinning temperature is 270-280 ℃, the annular blowing air speed is 0.45 +/-0.05 m/min, the annular blowing temperature is 23-25 ℃, the annular blowing humidity is 35-45RH percent, the drafting multiple of POY is 1.5-2.0 times, the spinning speed of POY is 2800-3500m/min, the drafting multiple of FDY is 3.0-4.5 times, and the spinning speed is 4000-4800 m/min.

The flame-retardant micrometer-yarn composite superfine fiber and the preparation method thereof have the advantages that the flame retardant in the fiber does not contain a halogen component flame retardant, the product is safe to use, the strong damage is small, the subsequent fiber processing is suitable, the health and even life safety of a user cannot be influenced after the flame is burnt, the dispersing effect of the flame retardant in the fiber is good, the process is simple, the operation is convenient, no pollution is caused, and the environment is protected.

Detailed Description

In order to more clearly understand the technical solution of the present invention, the present invention is further illustrated by the following examples.

Example 1:

the flame-retardant micrometer fiber composite superfine fiber described in the embodiment comprises the following components in parts by weight: 1 part of flame retardant, 50 parts of polyethylene terephthalate and 20 parts of nylon 6, wherein the flame-retardant micrometer composite superfine fiber is obtained by alkali treatment and ultrasonic fiber opening with acetone as a medium.

The flame retardant comprises 40 parts of sodium tungstate, 30 parts of sodium molybdate, 20 parts of tartaric acid and 20 parts of citric acid.

The preparation method of the flame-retardant micron-silk composite superfine fiber comprises the following steps:

step one, vacuum drying. Polyethylene terephthalate and nylon 6 were dried at 60 ℃ for 8 h.

And step two, melt spinning. The method comprises the steps of adopting a melt spinning method, carrying out melt mixing on polyethylene terephthalate and nylon 6, then carrying out extrusion drawing, cooling by circular blowing, bundling and oiling, and carrying out drafting winding to prepare the micron-yarn composite pre-oriented yarn.

And step three, false twist texturing. Drawing, false twisting and deforming the micron silk composite pre-oriented yarn to prepare micron silk composite fiber, carrying out flame retardant treatment on the micron silk composite fiber by using a flame retardant to obtain flame-retardant micron silk composite fiber, and preparing flame-retardant micron silk composite superfine fiber by using an alkali treatment ultrasonic fiber opening method; the melt spinning process comprises the following process parameters: the composite melt spinning temperature is 270 ℃, the air speed of the circular blowing air is 0.4m/min, the temperature of the circular blowing air is 23 ℃, the humidity of the circular blowing air is 35RH percent, the drafting multiple of POY is 1.5 times, the spinning speed of the POY is 2800m/min, the drafting multiple of FDY is 3.0 times, and the spinning speed is 4000 m/min.

The flame retardant treatment process comprises the following specific steps: and (3) placing the micrometer silk composite fiber in an environment with the temperature of 70 ℃ and the PH of 3, and soaking and boiling the micrometer silk composite fiber in a flame retardant water solution with the ratio of the flame retardant to the water of 1:30 for 10 minutes to obtain the flame-retardant micrometer silk composite fiber.

The alkali treatment ultrasonic fiber opening method comprises the following steps: weighing 1 part of flame-retardant micro-yarn composite fiber, preparing 100 parts of sodium carbonate/acetone solution with the content of 1mol/L at the same time, carrying out alkali treatment and ultrasonic fiber opening at the bath ratio of 1:100 under the normal temperature environment, carrying out ultrasonic treatment for 20 minutes and ultrasonic power of 500w, then carrying out cleaning and acid washing, cleaning with water to be neutral, drying and carrying out fiber characteristic test.

The resulting fiber properties are shown in table 1.

Example 2:

the flame-retardant micrometer fiber composite superfine fiber described in the embodiment comprises the following components in parts by weight: 4 parts of flame retardant, 70 parts of polybutylene terephthalate and 50 parts of nylon 612, wherein the flame-retardant micrometer composite superfine fiber is obtained by performing alkali treatment and ultrasonic fiber opening on acetone as a medium.

The flame retardant comprises 50 parts of sodium tungstate, 60 parts of sodium molybdate, 30 parts of tartaric acid and 30 parts of citric acid.

The preparation method of the flame-retardant micron-silk composite superfine fiber comprises the following steps:

step one, vacuum drying. Polybutylene terephthalate and nylon 612 were dried at 180 ℃ for 24 h.

And step two, melt spinning. The method comprises the steps of adopting a melt spinning method, carrying out melt mixing on polybutylene terephthalate and nylon 612 melt, then carrying out extrusion drawing, cooling by circular blowing, bundling and oiling, and carrying out drafting winding to prepare the micron-yarn composite pre-oriented yarn.

And step three, false twist texturing. Drawing, false twisting and deforming the micron silk composite pre-oriented yarn to prepare micron silk composite fiber, carrying out flame retardant treatment on the micron silk composite fiber by using a flame retardant to obtain flame-retardant micron silk composite fiber, and preparing flame-retardant micron silk composite superfine fiber by using an alkali treatment ultrasonic fiber opening method; the melt spinning process comprises the following process parameters: the composite melt spinning temperature is 290 ℃, the air speed of the circular blowing is 0.45m/min, the temperature of the circular blowing is 25 ℃, the humidity of the circular blowing is 45RH percent, the drafting multiple of the POY is 2.0 times, the spinning speed of the POY is 3500m/min, the drafting multiple of the FDY is 4.5 times, and the spinning speed is 4800 m/min.

The flame retardant treatment process comprises the following specific steps: and (3) placing the micrometer silk composite fiber in an environment with the temperature of 100 ℃ and the pH value of 5, and soaking and boiling the micrometer silk composite fiber in a flame retardant water solution with the ratio of the flame retardant to the water of 1:25 for 15 minutes to obtain the flame-retardant micrometer silk composite fiber.

The alkali treatment ultrasonic fiber opening method comprises the following steps: weighing 1 part of flame-retardant micro-yarn composite fiber, preparing 100 parts of sodium carbonate/acetone solution with the content of 1mol/L at the same time, carrying out alkali treatment and ultrasonic fiber opening at the bath ratio of 1:100 under the normal temperature environment, carrying out ultrasonic treatment for 20 minutes and ultrasonic power of 500w, then carrying out cleaning and acid washing, cleaning with water to be neutral, drying and carrying out fiber characteristic test.

The resulting fiber properties are shown in table 1.

Example 3:

the flame-retardant micrometer fiber composite superfine fiber described in the embodiment comprises the following components in parts by weight: 3 parts of flame retardant, 60 parts of polyethylene terephthalate and 35 parts of nylon 12, wherein the flame-retardant micrometer filament composite superfine fiber is obtained by performing alkali treatment and ultrasonic fiber opening on acetone as a medium.

The flame retardant comprises 45 parts sodium tungstate, 45 parts sodium molybdate, 25 parts tartaric acid and 25 parts citric acid.

The preparation method of the flame-retardant micron-silk composite superfine fiber comprises the following steps:

step one, vacuum drying. The polyethylene terephthalate and nylon 12 were dried at 120 ℃ for 16 h.

And step two, melt spinning. The method comprises the steps of adopting a melt spinning method, carrying out melt mixing on polyethylene terephthalate and nylon 12, then carrying out extrusion drawing, cooling by circular blowing, bundling and oiling, and carrying out drafting winding to prepare the micron-yarn composite pre-oriented yarn.

And step three, false twist texturing. Drawing, false twisting and deforming the micron silk composite pre-oriented yarn to prepare micron silk composite fiber, carrying out flame retardant treatment on the micron silk composite fiber by using a flame retardant to obtain flame-retardant micron silk composite fiber, and preparing flame-retardant micron silk composite superfine fiber by using an alkali treatment ultrasonic fiber opening method; the melt spinning process comprises the following process parameters: the composite melt spinning temperature is 280 ℃, the air speed of the circular blowing is 0.45m/min, the temperature of the circular blowing is 24 ℃, the humidity of the circular blowing is 40RH percent, the drafting multiple of POY is 1.75 times, the spinning speed of the POY is 3150m/min, the drafting multiple of FDY is 3.75 times, and the spinning speed is 4400 m/min.

The flame retardant treatment process comprises the following specific steps: and (3) putting the micrometer silk composite fiber in an environment with 85 ℃ and pH of 4, and soaking and boiling the micrometer silk composite fiber in a flame retardant aqueous solution with the ratio of the flame retardant to the water of 1:25 for 12 minutes to obtain the flame-retardant micrometer silk composite fiber.

The alkali treatment ultrasonic fiber opening method comprises the following steps: weighing 1 part of flame-retardant micro-yarn composite fiber, preparing 100 parts of sodium carbonate/acetone solution with the content of 1mol/L at the same time, carrying out alkali treatment and ultrasonic fiber opening at the bath ratio of 1:100 under the normal temperature environment, carrying out ultrasonic treatment for 20 minutes and ultrasonic power of 500w, then carrying out cleaning and acid washing, cleaning with water to be neutral, drying and carrying out fiber characteristic test.

The resulting fiber properties are shown in table 1.

And (3) judging the flame retardant property: according to the American Standard for safety of automobiles (FMVSS-302), the burning rate of the horizontally supported test piece was measured, and if the flame did not reach the mark line, it was judged as "flame retardant".

The fiber characteristics of the flame-retardant micro-filament composite ultrafine fibers prepared in examples 1 to 3 are shown in the following table.

TABLE 1 fiber Property Table

As shown in the results in Table 1, the flame-retardant micrometer filament composite superfine fiber is prepared by adopting a flame retardant aqueous solution for immersion and boiling and an alkali treatment ultrasonic fiber opening mode, the diameter of the obtained superfine fiber is less than 0.5 micrometer, the fiber strength is about 3cN/dtex, the elastic recovery rate is more than 90 percent, and the flame-retardant micrometer filament composite superfine fiber has flame retardant performance.