CN102965750B - Method for preparing flame retardant viscose fiber - Google Patents

Abstract

The invention discloses a method for preparing flame retardant viscose fiber. The method comprising the following steps: A) mixing nano fiber having a flame retardant function, basic magnesium sulfate whisker, basic magnesium chloride whisker and magnesium salt whisker, then roasting the mixture in an oven of 400 DEG C, carrying out dispersion in absolute ethyl alcohol containing sodium hexametaphosphate, carrying out plasma treatment at normal pressure, carrying out ultrasonic dispersion and cleaning, filtering by a filter of 400 meshes and drying; B) uniformly mixing and drying the whisker and a titanate coupling reagent, adding and mixing antimonous oxide, hexabromocyclododecane, (HDPE+SEBS)-g-MAH and calcium stearate, and then adding cellulose spinning viscose to prepare flame retardant cellulose spinning viscose; and C) preparing the flame retardant viscose fiber by means of a wet or dry process spinning technology. The flame retardant viscose fiber is good in strength, stiffness, abrasive resistance and flame retardance.

Description

A kind of manufacture method of flame retardant viscose fiber

technical field

The present invention relates to a method for producing flame retardant viscose fiber. The flame retardant viscose fiber includes cellulose spinning viscose, basic magnesium sulfate whisker, magnesium salt whisker, basic magnesium chloride whisker, three Antimony oxide and hexabromocyclododecane belong to the technical field of textile fiber manufacturing.

Background technique

Viscose fiber is a regenerated cellulose fiber. It is made of natural cellulose as raw material, which is made into spinning viscose through alkalization, aging, yellowing and other processes, and is made by wet spinning. Viscose fiber has the structure and properties of cellulose. Good hygroscopicity, air permeability, softness, comfortable to wear; smooth and cool, antistatic and other characteristics, its fabrics are comfortable to wear, hygienic, chic and bright, and have properties that many fibers cannot match. With the improvement of people's living standards and the return to nature in clothing and home decoration, viscose fibers made of natural cellulose will surely develop into new fibers with high performance, differentiation, functionality and environmental protection to meet the needs of downstream products. Colorful requirements. But at present, the variety of viscose fiber is still very single, mainly conventional varieties, lacking in the development of non-consumable and high-end application fields.

Whiskers are grown in the form of single crystals with a very small diameter (0.1-10um), highly ordered atomic arrangements, and strength close to the theoretical value of a complete crystal. Adding a small amount of whiskers to polymer materials can endow high strength, heat resistance, flame retardancy, antibacterial and other functions. The basic magnesium sulfate whisker with flame retardant function can absorb a large amount of heat energy to reduce the temperature of the substrate due to the dehydration reaction of the crystal water in its molecules during combustion. In addition, the generated water vapor can not only dilute the concentration of the reaction gas in the flame zone, but also absorb smoke, and play the role of flame retardancy and smoke elimination. Both basic magnesium chloride whiskers and magnesium salt whiskers have good flame retardant effects. It is superior to commonly used flame retardant materials.

Contents of the invention

The object of the present invention is to overcome the shortcomings of the prior art and provide a method for producing flame-retardant viscose fibers with better strength, stiffness and abrasion resistance.

The object of the present invention is to be accomplished by following technical scheme, a kind of manufacture method of flame-retardant viscose fiber, and it adopts following steps:

A) According to the number of parts by mass, take 8-12 parts of basic magnesium sulfate whiskers whose characteristic parameters are 0.1-1.5um in diameter and 5-10um in length, and 6-10 parts whose characteristic parameters are 0.2-1um in diameter and 6-12um in length Basic magnesium chloride whiskers, 8-12 copies of magnesium salt whiskers with characteristic parameters of 0.2-0.8um in diameter and 6-10um in length, after mixing the above three kinds of whiskers evenly, bake them in a vacuum furnace at 350-450°C React for 4-6 hours, after cooling, stir and disperse in absolute ethanol containing sodium hexametaphosphate for 30-45 minutes, then treat with atmospheric pressure plasma for 10-20 minutes, and then disperse in 60-70°C deionized water containing calcium stearate dispersion Ultrasonic disperse and clean for 25-35 minutes, take the suspended whiskers in the upper layer of the solution and filter through 160 mesh, take the modified whisker mixed solution, and repeat the operation 3-5 times until it is filtered, and then dry it in a vacuum oven to obtain the modified Whiskers;

B) Take 0.8-1.2 parts of titanate coupling agent in parts by mass, dilute the titanate coupling agent 1:3 with isopropanol, mix well, and then add 10-15 parts of the modification obtained in step A) Whiskers, closed mixing and stirring reaction at 70-80°C for 30-45min, drying, then adding 1-1.5 parts of antimony trioxide, 2-3 parts of hexabromocyclododecane, (HDPE+SEBS)-g -MAH compatibilizer 1.5-2 parts, dispersant calcium stearate 0.3 parts, closed mixing and stirring reaction at 65-75 ℃ for 30-45 minutes, then add 90-110 parts of cellulose spinning viscose, closed stirring reaction 45-60min, obtain flame-retardant cellulose spinning viscose;

C) The flame-retardant cellulose spinning viscose obtained in step B) is stirred, mixed, filtered, defoamed, and matured on special viscose equipment; a flame-retardant viscose is made by wet or dry spinning technology. glue fiber.

The preferred technical scheme of the present invention is:

Step A) Take 10 parts by mass of basic magnesium sulfate whiskers whose characteristic parameters are 0.1-1.5um in diameter and 5-10um in length, and 8 parts of basic magnesium sulfate whiskers whose characteristic parameters are 0.2-1um in diameter and 6-12um in length. Magnesium chloride whiskers, 10 parts of magnesium salt whiskers whose characteristic parameters are 0.2-0.8um in diameter and 6-10um in length, after mixing the three kinds of whiskers evenly, roasting and reacting in a vacuum furnace at 400°C for 5 hours, and after cooling, add Stir and disperse sodium hexametaphosphate in absolute ethanol for 38 minutes, then treat with plasma at normal pressure for 15 minutes, then ultrasonically disperse and wash in deionized water at 65°C containing calcium stearate dispersion for 30 minutes, take the suspended whiskers in the upper layer of the solution and pass through a 160-mesh Filtrate, take the modified whisker mixed solution, and repeat the operation 4 times until it is filtered, and then dry it in a vacuum oven to obtain the modified whisker;

Step B) Take 1.0 parts of titanate coupling agent in parts by mass, dilute and mix the titanate coupling agent 1:3 with isopropanol, and then add 12 parts of the modified whiskers obtained in step A), Closed mixing and stirring reaction at 75°C for 38 minutes, drying, then adding 1.2 parts of antimony trioxide, 2.5 parts of hexabromocyclododecane, 1.8 parts of (HDPE+SEBS)-g-MAH compatibilizer, dispersant hard 0.3 part of calcium fatty acid was mixed and stirred for reaction at 70°C for 38 minutes, then 100 parts of cellulose spinning viscose was added, and stirred for 52 minutes to obtain a flame-retardant cellulose spinning viscose.

The present invention adds nano-scale basic magnesium sulfate whiskers, magnesium salt whiskers, basic magnesium chloride whiskers, antimony trioxide, hexabromocyclodeca whiskers, etc. Dioxane, etc.; through viscose mixing, viscose filtration, viscose degassing, viscose aging, and then wet spinning technology to make flame-retardant viscose fiber; this kind of cellulose flame-retardant viscose fiber has better It can be widely used in fire protection, thermal engineering, carpets, curtains, bedding, car cushions and room decoration, etc., especially suitable for public places with fire safety requirements.

Detailed ways

The present invention will be described in detail below in conjunction with specific embodiments: a kind of manufacture method of flame-retardant viscose fiber of the present invention, this manufacture method adopts following steps:

A) According to the number of parts by mass, take 8-12 parts of basic magnesium sulfate whiskers whose characteristic parameters are 0.1-1.5um in diameter and 5-10um in length, and 6-10 parts whose characteristic parameters are 0.2-1um in diameter and 6-12um in length Basic magnesium chloride whiskers, 8-12 copies of magnesium salt whiskers with characteristic parameters of 0.2-0.8um in diameter and 6-10um in length; after mixing the above three kinds of whiskers evenly, roast them in a vacuum furnace at 350-450°C React for 4-6 hours, after cooling, stir and disperse in absolute ethanol containing sodium hexametaphosphate for 30-45 minutes, then treat with atmospheric pressure plasma for 10-20 minutes, and then disperse in 60-70°C deionized water containing calcium stearate dispersion Ultrasonic disperse and clean for 25-35 minutes, take the suspended whiskers in the upper layer of the solution and filter through 160 mesh, take the modified whisker mixed solution, and repeat the operation 3-5 times until it is filtered, and then dry it in a vacuum oven to obtain the modified Whiskers;

B) Take 0.8-1.2 parts of titanate coupling agent in parts by mass, dilute the titanate coupling agent 1:3 with isopropanol, mix well, and then add 10-15 parts of the modification obtained in step A) Whiskers, closed mixing and stirring reaction at 70-80°C for 30-45min, drying, then adding 1-1.5 parts of antimony trioxide, 2-3 parts of hexabromocyclododecane, (HDPE+SEBS)-g -MAH compatibilizer 1.5-2 parts, dispersant calcium stearate 0.3 parts, closed mixing and stirring reaction at 65-75 ℃ for 30-45 minutes, then add 90-110 parts of cellulose spinning viscose, closed stirring reaction 45-60min, obtain flame-retardant cellulose spinning viscose;

C) The flame-retardant cellulose spinning viscose obtained in step B) is stirred, mixed, filtered, defoamed, and matured on special viscose equipment; a flame-retardant viscose is made by wet or dry spinning technology. glue fiber.

Embodiment 1: the manufacture method of flame-retardant viscose fiber of the present invention, it adopts following steps:

Step A) Take 10 parts by mass of basic magnesium sulfate whiskers whose characteristic parameters are 0.1-1.5um in diameter and 5-10um in length, and 8 parts of basic magnesium sulfate whiskers whose characteristic parameters are 0.2-1um in diameter and 6-12um in length. Magnesium chloride whiskers, 10 parts of magnesium salt whiskers whose characteristic parameters are 0.2-0.8um in diameter and 6-10um in length; after mixing the three kinds of whiskers evenly, roasting and reacting in a vacuum furnace at 400°C for 5 hours, and after cooling, add Stir and disperse sodium hexametaphosphate in absolute ethanol for 38 minutes, then treat with plasma at normal pressure for 15 minutes, then ultrasonically disperse and wash in deionized water at 65°C containing calcium stearate dispersion for 30 minutes, take the suspended whiskers in the upper layer of the solution and pass through a 160-mesh Filtrate, take the modified whisker mixed solution, and repeat the operation 4 times until it is filtered, and then dry it in a vacuum oven to obtain the modified whisker;

Step B) Take 1.0 parts of titanate coupling agent in parts by mass, dilute and mix the titanate coupling agent 1:3 with isopropanol, and then add 12 parts of the modified whiskers obtained in step A), Airtightly mixed and stirred at 75°C for 38 minutes, dried, and then added 1.2 parts of antimony trioxide, 2.5 parts of hexabromocyclododecane, 1.8 parts of (HDPE+SEBS)-g-MAH compatibilizer, dispersant hard 0.3 parts of calcium fatty acid, mixed and stirred under the condition of 70°C for 38 minutes, then added 100 parts of cellulose spinning viscose, and reacted for 52 minutes with closed stirring to obtain flame-retardant cellulose spinning viscose;

C) The flame-retardant cellulose spinning viscose obtained in step B) is stirred, mixed, filtered, defoamed, and matured on special viscose equipment; a flame-retardant viscose is made by wet or dry spinning technology. glue fiber.

Embodiment 2: the manufacture method of a kind of flame-retardant viscose fiber of the present invention, it adopts following steps:

A) According to the number of parts by mass, take 8 parts of basic magnesium sulfate whiskers whose characteristic parameters are 0.1-1.5um in diameter and 5-10um in length, and 6 parts of basic magnesium chloride whose characteristic parameters are 0.2-1um in diameter and 6-12um in length Whiskers, 8 parts of magnesium salt whiskers whose characteristic parameters are 0.2-0.8um in diameter and 6-10um in length; after mixing the above three kinds of whiskers evenly, roasting reaction in a vacuum furnace at 350°C for 4h, and after cooling, add six Stir and disperse in absolute ethanol of sodium metaphosphate for 30 minutes, then treat with normal pressure plasma for 10 minutes, then ultrasonically disperse and wash in 60°C deionized water containing calcium stearate dispersion for 25 minutes, take the suspended whiskers in the upper layer of the solution and filter through 160 mesh , take the modified whisker mixed solution, and repeat the operation 3 times until it is filtered, and then dry it in a vacuum oven to obtain the modified whisker;

B) Take 0.8 parts by mass of titanate coupling agent, dilute and mix the titanate coupling agent 1:3 with isopropanol, then add 10 parts of the modified whisker obtained in step A), and Closed mixing and stirring reaction at 70°C for 30 minutes, drying, then adding 1 part of antimony trioxide, 2 parts of hexabromocyclododecane, 1.5 parts of (HDPE+SEBS)-g-MAH compatibilizer, dispersant stearin Calcium acid 0.3 part, airtight mixing and stirring reaction at 65°C for 30 minutes, then add 90 parts of cellulose spinning viscose, and airtight stirring reaction for 45 minutes to obtain flame-retardant cellulose spinning viscose;

C) The flame-retardant cellulose spinning viscose obtained in step B) is stirred, mixed, filtered, defoamed, and matured on special viscose equipment; a flame-retardant viscose is made by wet or dry spinning technology. glue fiber.

Embodiment 3: the manufacture method of a kind of flame-retardant viscose fiber of the present invention, it adopts following steps:

A) According to the number of parts by mass, take 12 parts of basic magnesium sulfate whiskers whose characteristic parameters are 0.1-1.5um in diameter and 5-10um in length, and 10 parts of basic magnesium chloride whose characteristic parameters are 0.2-1um in diameter and 6-12um in length Whiskers, 12 parts of magnesium salt whiskers whose characteristic parameters are 0.2-0.8um in diameter and 6-10um in length; after mixing the above-mentioned three kinds of whiskers evenly, roasting reaction in a vacuum furnace at 450°C for 6h, and after cooling, add six Stir and disperse in absolute ethanol of sodium metaphosphate for 45 minutes, then treat with normal pressure plasma for 20 minutes, then ultrasonically disperse and wash in 70°C deionized water containing calcium stearate dispersion for 35 minutes, take the suspended whiskers in the upper layer of the solution and filter through 160 mesh , take the modified whisker mixed solution, and repeat the operation 5 times until it is filtered, and then dry it in a vacuum oven after filtering to obtain the modified whisker;

B) Take 1.2 parts by mass of titanate coupling agent, dilute and mix the titanate coupling agent 1:3 with isopropanol, and then add 15 parts of the modified whisker obtained in step A). Closed mixing and stirring reaction at 80°C for 45 minutes, drying, then adding 1.5 parts of antimony trioxide, 3 parts of hexabromocyclododecane, 2 parts of (HDPE+SEBS)-g-MAH compatibilizer, dispersant stearin Calcium acid 0.3 part, airtight mixing and stirring reaction at 75°C for 45 minutes, then add 110 parts of cellulose spinning viscose, and airtight stirring reaction for 60 minutes to obtain flame-retardant cellulose spinning viscose;

C) The flame-retardant cellulose spinning viscose obtained in step B) is stirred, mixed, filtered, defoamed, and matured on special viscose equipment; a flame-retardant viscose is made by wet or dry spinning technology. glue fiber.

The embodiments of the present invention are not limited to the above-mentioned three embodiments, and any number of embodiments can be obtained by any replacement in the specific embodiments through the numerical ranges disclosed above, which are not listed one by one.

Claims (2)

1. a manufacture method for fire resistant viscose acetal fibre, is characterized in that this manufacture method adopts following steps:

A) getting 8-12 part characterization parameter diameter by mass fraction is that 0.1-1.5 μ m, length are the alkali magnesium sulfate crystal whisker of 5-10 μ m, 6-10 part characterization parameter diameter is that 0.2-1 μ m, length are the basic magnesium chloride whisker of 6-12 μ m, and 8-12 part characterization parameter diameter is that 0.2-0.8 μ m, length are the magnesium salt whisker of 6-10 μ m; After above-mentioned three kinds of whiskers are mixed, calcination 4-6h in 350-450 DEG C of vacuum drying oven, after cooling containing dispersed with stirring 30-45min in the absolute ethyl alcohol of calgon, then atmospheric plasma is processed 10-20min,, cleaning 25-35min loose in the 60-70 DEG C of deionized water for ultrasonic wavelength-division containing calcium stearate dispersion again, getting solution upper strata suspension whisker filters through 160 orders, get modified crystal whiskers mixed liquor, and repeat 3-5 time until filtering, after filtering, dry at vacuum drying oven, obtain modified crystal whiskers;

B) get 0.8-1.2 part titanate coupling agent by mass fraction, titanate coupling agent 1 ﹕ 3 is diluted, mixed with isopropyl alcohol; Then add 10-15 part steps A) modified crystal whiskers that obtains, airtight mix and blend reaction 30-45min, oven dry under 70-80 DEG C of condition, then add 0.3 part of antimonous oxide 1-1.5 part, hexabromo-Cyclododecane 2-3 part, (HDPE+SEBS)-g-MAH bulking agent 1.5-2 part, dispersant calcium stearate, airtight mix and blend reaction 30-45min under 65-75 DEG C of condition, add again cellulose spinning viscose 90-110 part, airtight stirring reaction 45-60min, obtains fire-retardant cellulose spinning viscose;

C) by step B) stirring on special viscose equipment of fire-retardant cellulose spinning viscose, mixing, filtration, deaeration, the maturation that obtain; Adopt wet spinning technology to make a kind of fire resistant viscose acetal fibre.

2. according to the manufacture method of the fire resistant viscose acetal fibre described in claim 1, it is characterized in that in described step:

Steps A) to get 10 parts of characterization parameter diameters by mass fraction be 0.1-1.5 μ m, length is the alkali magnesium sulfate crystal whisker of 5-10 μ m, 8 parts of characterization parameter diameters are 0.2-1 μ m, length is the basic magnesium chloride whisker of 6-12 μ m, 10 parts of characterization parameter diameters are 0.2-0.8 μ m, length is the magnesium salt whisker of 6-10 μ m, after these three kinds of whiskers are mixed, calcination 5h in 400 DEG C of vacuum drying ovens, after cooling containing dispersed with stirring 38min in the absolute ethyl alcohol of calgon, then atmospheric plasma is processed 15min, loose in 65 DEG C of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion again, clean 30min, getting solution upper strata suspension whisker filters through 160 orders, get modified crystal whiskers mixed liquor, and repeat 4 times until filtering, after filtering, dry at vacuum drying oven, obtain modified crystal whiskers,

Step B) get 1.0 parts of titanate coupling agents by mass fraction, titanate coupling agent 1 ﹕ 3 is diluted with isopropyl alcohol, mix, then add 12 parts of A) modified crystal whiskers that obtains, airtight mix and blend reaction 38min under 75 DEG C of conditions, dry, then add 1.2 parts of antimonous oxides, 2.5 parts of hexabromo-Cyclododecane, (HDPE+SEBS)-1.8 parts of g-MAH bulking agents, 0.3 part of dispersant calcium stearate, airtight mix and blend reaction 38min under 70 DEG C of conditions, add again 100 parts of cellulose spinning viscoses, airtight stirring reaction 52min, obtain fire-retardant cellulose spinning viscose.