CN103255488B - Preparation method of high-strength viscose fiber - Google Patents

Abstract

The invention relates to a preparation method of high-strength viscose fiber, which belongs to the technical field of textile fiber processing. The present invention mainly disperses the inorganic nano-whiskers or organic nano-whiskers through the dispersion liquid, then blends them with the viscose collagen solution, and prepares high-strength viscose fibers through processes such as stirring, standing for defoaming, filtering, and spinning. Filament or staple. The strength of the obtained viscose fiber is 20-50% higher than that spun by traditional techniques. The preparation method of the invention has simple process, no need of special equipment, convenient operation and control, and is easy to realize industrialized production. The viscose fiber prepared by the method has higher strength than the viscose fiber prepared by the traditional method and is widely used.

Description

A kind of preparation method of high-strength viscose fiber

technical field

The invention relates to a preparation method of high-strength viscose fiber, which belongs to the technical field of textile fiber processing.

Background technique

Viscose fiber has a long history. As early as the end of the 19th century, British scientists Cross, Bevan, and Beadle invented the method for preparing cellulose sulfonate. For more than 100 years, due to the wide source of natural cellulose as raw material of viscose fiber, which belongs to renewable resources; the product has good wearing performance, has a series of advantages such as moisture absorption, breathability, softness, easy dyeing, and antistatic, making it very comfortable to wear; and viscose The fiber can be degraded naturally and will not cause environmental pollution. Although viscose fiber has the above-mentioned series of advantages, its disadvantages are obvious: its strength is low, especially its wet strength is poor;

China Publication Patent No. CN101775671A, published on July 14, 2010, the name of the invention is a high-strength viscose fiber and its production method. The application discloses a high-strength viscose fiber and its production method. Its features The method is to mix bacterial cellulose with viscose spinning solution and make viscose fiber. The production method comprises the steps of: pretreating the flake bacterial cellulose, and then pulverizing it by a ball milling method to obtain micronano-scale bacterial cellulose powder; adding the bacterial cellulose powder to the viscose spinning solution to disperse evenly and defoaming to obtain a spinning stock solution; the above spinning stock solution is made into high-strength viscose fiber. The viscose fiber prepared by the method of the invention has high strength, low shrinkage and good elasticity, can be blended and interwoven with cotton, wool and other synthetic fibers, and can be used in the fields of high-grade clothing fabrics and industrial textiles. However, in this method, the flake bacterial cellulose needs to be made into bacterial cellulose powder first, and then the bacterial cellulose powder is directly added to the viscose spinning solution. The non-uniform mixing of plain powder particles and viscose fiber spinning solution will easily affect the performance of the fiber.

Therefore, how to effectively prepare high-strength viscose fibers, and the process is simple and easy to control, has significant social and economic benefits, and is conducive to promoting the industrial upgrading of my country's chemical fiber industry.

Contents of the invention

For above-mentioned existence problem, the purpose of the present invention is to overcome above-mentioned defect, a kind of preparation method of high-strength viscose fiber is provided, the technical solution for meeting the purpose of the present invention is:

A kind of preparation method of high-strength viscose fiber, described preparation method comprises the following steps:

A The primary dispersion is made according to the ratio of mass fraction NaOH 4.5%, viscose collagen solution 8% and water 87.5%;

B Add one of the inorganic nano-whiskers or organic nano-whiskers to the primary dispersion, wherein the mass fractions are:

Nano whiskers 20-50%,

Primary dispersion 50-80%,

After mixing, put it into a blender and stir evenly, wherein the stirring temperature is 15-30°C, the stirring time is 1-6 hours, and the speed of the blender is 100-2000 rpm to make a nano-whisker dispersion;

C Then the nano whisker dispersion is blended with the viscose collagen solution with a methyl fiber content of 8%, wherein it is respectively by mass fraction:

50-99% viscose collagen solution, 1-50% nano-whisker dispersion liquid, and stir to form a blended solution evenly through a mixer, wherein the stirring temperature is 20-22°C, the stirring time is 2-8 hours, and the speed of the mixer is 100- 2000 revolutions per minute;

D Filter the blended solution twice, put it into a defoaming kettle, keep it warm at 20-22°C, and defoam for 6-8 hours;

E The blended solution after filtration and defoaming is subjected to wet spinning to obtain high-strength viscose fiber. The composition of the coagulation bath is: sulfuric acid 10-20g/L, sodium sulfate 400-420g/L, zinc sulfate 10 ~30g/L.

The inorganic nano-whiskers are one of nano-silicon carbide or carbon nanotubes or nano-zinc oxide;

The organic nano whisker is a kind of nano protein whisker or nano cellulose whisker.

Owing to adopting above technical scheme, the beneficial technical effect of the present invention is:

1 The present invention utilizes the advantages of high strength, high modulus and high elongation of nano-whiskers to make inorganic (or organic) nano-whiskers into a dispersion and blend them with viscose to obtain a blended solution. , static defoaming, filtration, spinning and other processes to produce high-strength viscose fibers. Viscose and dispersion do not react under alkaline conditions, it is a physical blending process, which does not damage the properties of high strength, high modulus and high elongation of nano whiskers. Moreover, inorganic (or organic) nano-whiskers come from a wide range of sources, with many options and little follow-up process adjustment.

2. The high-strength viscose fiber prepared by the present invention not only has higher strength, but the strength of the obtained viscose fiber is 20-50% higher than that spun by traditional techniques; and it has good elasticity, hygroscopicity, dyeability, Corrosion resistance, fluffiness, etc., widely used.

3 The preparation method of a high-strength viscose fiber according to the present invention can be directly adjusted on the viscose production process; high-strength viscose fibers can be produced on ordinary viscose production and spinning processing equipment without special equipment Viscose fiber; the operation process is convenient and easy to control, and it is easy to realize industrial production.

Detailed ways

A kind of preparation method of high-strength viscose fiber, described preparation method comprises the following steps:

A The primary dispersion liquid is made according to the ratio of mass fraction NaOH 4.5%, viscose collagen solution 8% and water 87.5%;

B Add one of the inorganic nano-whiskers or organic nano-whiskers to the primary dispersion, wherein the mass fractions are:

Nano whiskers 20-50%,

Primary dispersion 50-80%,

After mixing, put it into a blender and stir evenly, wherein the stirring temperature is 15-30°C, the stirring time is 1-6 hours, and the speed of the blender is 100-2000 rpm to make a nano-whisker dispersion;

C Then the nano whisker dispersion is blended with the viscose collagen solution with a methyl fiber content of 8%, wherein it is respectively by mass fraction:

Viscose collagen solution 50-99%,

Nano whisker dispersion 1~50%,

Stir with a mixer to form a blended solution evenly, wherein the stirring temperature is 20-22°C, the stirring time is 2-8 hours, and the rotation speed of the mixer is 100-2000 rpm;

D Filter the blended solution twice, put it into a defoaming kettle, keep it warm at 20-22°C, and defoam for 6-8 hours;

E The blended solution after filtration and defoaming is subjected to wet spinning to obtain high-strength viscose fiber. The composition of the coagulation bath is: sulfuric acid 10-20g/L, sodium sulfate 400-420g/L, zinc sulfate 10 ~30g/L.

The inorganic nano-whiskers are one of nano-silicon carbide or carbon nanotubes or nano-zinc oxide;

The organic nano whisker is a kind of nano protein whisker or nano cellulose whisker.

Example 1

A. Preparation of inorganic nano-silicon carbide dispersion

Put the inorganic nano-silicon carbide and the primary dispersion in the following mass percentages: 20% of the inorganic nano-silicon carbide and 80% of the primary dispersion, put them into a mixer and stir evenly, the stirring temperature is 15°C, and the stirring time is 1 hour. The rotation speed is 100 r/min to form an inorganic nano-silicon carbide dispersion liquid for later use.

B. Preparation of blended solution of viscose collagen solution and inorganic nano-silicon carbide dispersion

Put the viscose collagen solution and the inorganic nano-silicon carbide dispersion prepared by step A in the following mass percentages: 50% of viscose and 50% of the inorganic nano-silicon carbide dispersion, put them into a mixer and stir evenly, and the stirring temperature is 20°C , the stirring time is 2 hours, the rotating speed of the mixer is 100 rpm, and a blended solution is formed, which is set aside.

C. Filtration and defoaming of blended solution

The blended solution prepared in step B was filtered twice, poured into a defoaming kettle, kept at 20°C, and degassed for 6 hours.

D. Spinning of blend solution

The blended solution prepared in step C is filtered, defoamed, and then spun to obtain high-strength viscose fiber. Wherein, the composition of coagulation bath: sulfuric acid 10g/L, sodium sulfate 400g/L, zinc sulfate 10g/L.

Example 2

A. Preparation of inorganic nano-silicon carbide dispersion

Put the inorganic nano-silicon carbide and the primary dispersion liquid in the following mass percentages: 50% of the inorganic nano-silicon carbide and 50% of the primary dispersion liquid, put them into a blender and stir evenly, the stirring temperature is 30°C, and the stirring time is 6 hours. The rotating speed is 2000 r/min to form an inorganic nano-silicon carbide dispersion, which is ready for use.

B. Preparation of blended solution of viscose collagen solution and inorganic nano-silicon carbide dispersion

Put the viscose collagen solution and the inorganic nano-silicon carbide dispersion prepared in step A according to the following mass percentages: viscose 99%, inorganic nano-silicon carbide dispersion 1%, put them into a mixer and stir evenly, and the stirring temperature is 22°C , the stirring time is 8 hours, the rotational speed of the mixer is 2000 rpm, and a blended solution is formed for later use.

C. Filtration and defoaming of blended solution

The blended solution prepared in step B was filtered twice, poured into a defoaming kettle, kept at 22°C, and degassed for 8 hours.

D. Spinning of blend solution

The blended solution prepared in step C is filtered, defoamed, and then spun to obtain high-strength viscose fiber. Wherein, the composition of coagulation bath: sulfuric acid 20g/L, sodium sulfate 420g/L, zinc sulfate 30g/L.

Example 3

A. Preparation of Inorganic Carbon Nanotube Dispersion

Put the inorganic carbon nanotubes and the primary dispersion in the following mass percentages: 20% of the inorganic carbon nanotubes and 80% of the primary dispersion, put them into a mixer and stir evenly, the stirring temperature is 15°C, and the stirring time is 1 hour. The rotational speed is 100 r/min to form an inorganic carbon nanotube dispersion, which is ready for use.

B. Preparation of blended solution of viscose collagen solution and inorganic carbon nanotube dispersion

Put the viscose collagen solution and the inorganic carbon nanotube dispersion prepared in step A in the following mass percentages: 50% viscose and 50% inorganic carbon nanotube dispersion, put them into a mixer and stir evenly, and the stirring temperature is 20°C , the stirring time is 2 hours, the rotating speed of the mixer is 100 rpm, and a blended solution is formed, which is set aside.

C. Filtration and defoaming of blended solution

The blended solution prepared in step B was filtered twice, poured into a defoaming kettle, kept at 20°C, and degassed for 6 hours.

D. Spinning of blend solution

The blended solution prepared in step C is filtered, defoamed, and then spun to obtain high-strength viscose fiber. Wherein, the composition of coagulation bath: sulfuric acid 10g/L, sodium sulfate 400g/L, zinc sulfate 10g/L.

Example 4

A. Preparation of Inorganic Carbon Nanotube Dispersion

Put the inorganic carbon nanotubes and the primary dispersion liquid in the following mass percentages: 50% of the inorganic carbon nanotubes and 50% of the primary dispersion liquid, put them into a mixer and stir evenly, the stirring temperature is 30°C, and the stirring time is 6 hours. The rotating speed is 2000 r/min to form an inorganic carbon nanotube dispersion liquid, which is set aside.

B. Preparation of blended solution of viscose collagen solution and inorganic carbon nanotube dispersion

Put the viscose collagen solution and the inorganic carbon nanotube dispersion prepared by step A in the following mass percentages: 99% of viscose and 1% of the inorganic carbon nanotube dispersion, put them into a mixer and stir evenly, and the stirring temperature is 22°C , the stirring time is 8 hours, the rotational speed of the mixer is 2000 rpm, and a blended solution is formed for later use.

C. Filtration and defoaming of blended solution

The blended solution prepared in step B was filtered twice, poured into a defoaming kettle, kept at 22°C, and degassed for 8 hours.

D. Spinning of blend solution

The blended solution prepared in step C is filtered, defoamed, and then spun to obtain high-strength viscose fiber. Wherein, the composition of coagulation bath: sulfuric acid 20g/L, sodium sulfate 420g/L, zinc sulfate 30g/L.

Example 5

A. Preparation of Inorganic Nano ZnO Dispersion

Put the inorganic nano-zinc oxide and the primary dispersion in the following mass percentages: 20% of the inorganic nano-zinc oxide and 80% of the primary dispersion, put them into a mixer and stir evenly, the stirring temperature is 15°C, and the stirring time is 1 hour. The rotation speed is 100 r/min to form an inorganic nano-zinc oxide dispersion liquid, which is ready for use.

B. Preparation of blended solution of viscose collagen solution and inorganic nano-zinc oxide dispersion

Put the viscose collagen solution and the inorganic nano-zinc oxide dispersion liquid prepared in step A in the following mass percentages: viscose 50%, inorganic nano-zinc oxide dispersion liquid 50%, put them into a mixer and stir evenly, and the stirring temperature is 20°C , the stirring time is 2 hours, the rotating speed of the mixer is 100 rpm, and a blended solution is formed, which is set aside.

C. Filtration and defoaming of blended solution

The blended solution prepared in step B was filtered twice, poured into a defoaming kettle, kept at 20°C, and degassed for 6 hours.

D. Spinning of blend solution

The blended solution prepared in step C is filtered, defoamed, and then spun to obtain high-strength viscose fiber. Wherein, the composition of coagulation bath: sulfuric acid 10g/L, sodium sulfate 400g/L, zinc sulfate 10g/L.

Example 6

A. Preparation of Inorganic Nano ZnO Dispersion

Put the inorganic nano-zinc oxide and the primary dispersion liquid in the following mass percentages: 50% of the inorganic nano-zinc oxide and 50% of the primary dispersion liquid, put them into a blender and stir evenly, the stirring temperature is 30°C, and the stirring time is 6 hours. The rotating speed is 2000 r/min to form an inorganic nano-zinc oxide dispersion liquid, which is ready for use.

B. Preparation of blended solution of viscose collagen solution and inorganic nano-zinc oxide dispersion

Put the viscose collagen solution and the inorganic nano-zinc oxide dispersion prepared in step A in the following mass percentages: 99% of viscose and 1% of the inorganic nano-zinc oxide dispersion, put them into a mixer and stir evenly, and the stirring temperature is 22°C , the stirring time is 8 hours, the rotational speed of the mixer is 2000 rpm, and a blended solution is formed for later use.

C. Filtration and defoaming of blended solution

The blended solution prepared in step B was filtered twice, poured into a defoaming kettle, kept at 22°C, and degassed for 8 hours.

D. Spinning of blend solution

The blended solution prepared in step C is filtered, defoamed, and then spun to obtain high-strength viscose fiber. Wherein, the composition of coagulation bath: sulfuric acid 20g/L, sodium sulfate 420g/L, zinc sulfate 30g/L.

Example 7

A. Preparation of organic nanoprotein microcrystal dispersion

The organic nano-protein microcrystals and the primary dispersion are in the following mass percentages: 20% of the organic nano-protein microcrystals and 80% of the primary dispersion, put them into a mixer and stir evenly, the stirring temperature is 15°C, and the stirring time is 1 hour. The rotating speed of the mixer is 100 r/min to form an organic nano-protein microcrystal dispersion, which is ready for use.

B. Preparation of blended solution of viscose collagen solution and organic nanoprotein microcrystal dispersion

Put the viscose collagen solution and the organic nano-protein microcrystal dispersion liquid obtained through A step into the following mass percentages: 50% of viscose, and 50% of the organic nano-protein microcrystal dispersion liquid, put them into a mixer and stir evenly, and the stirring temperature is 20°C, the stirring time is 2 hours, and the rotation speed of the mixer is 100 rpm to form a blended solution for later use.

C. Filtration and defoaming of blended solution

The blended solution prepared in step B was filtered twice, poured into a defoaming kettle, kept at 20°C, and degassed for 6 hours.

D. Spinning of blend solution

The blended solution prepared in step C is filtered, defoamed, and then spun to obtain high-strength viscose fiber. Wherein, the composition of coagulation bath: sulfuric acid 10g/L, sodium sulfate 400g/L, zinc sulfate 10g/L.

Example 8

A. Preparation of organic nanoprotein microcrystal dispersion

The organic nano-protein microcrystals and the primary dispersion are in the following mass percentages: 50% of the organic nano-protein microcrystals and 50% of the primary dispersion are put into a mixer and stirred evenly, the stirring temperature is 30°C, and the stirring time is 6 hours. The rotating speed of the mixer is 2000 r/min to form an organic nano-protein microcrystal dispersion, which is ready for use.

B. Preparation of blended solution of viscose collagen solution and organic nanoprotein microcrystal dispersion

Put the viscose collagen solution and the organic nano-protein microcrystal dispersion prepared through A step into the following mass percentages: 99% of viscose and 1% of the organic nano-protein microcrystal dispersion, put them into a mixer and stir evenly, and the stirring temperature is 22°C, the stirring time is 8 hours, and the rotation speed of the mixer is 2000 rpm to form a blended solution for later use.

C. Filtration and defoaming of the blended solution The blended solution prepared in step B was filtered twice, put into a defoaming kettle, kept at 22° C., and defoamed for 8 hours.

D. Spinning of blend solution

The blended solution prepared in step C is filtered, defoamed, and then spun to obtain high-strength viscose fiber. Wherein, the composition of coagulation bath: sulfuric acid 20g/L, sodium sulfate 420g/L, zinc sulfate 30g/L.

Example 9

A. Preparation of organic nanocellulose dispersion

Put the organic nanocellulose and the primary dispersion in the following mass percentages: 20% of the organic nanocellulose and 80% of the primary dispersion, put them into a blender and stir evenly, the stirring temperature is 15°C, and the stirring time is 1 hour. The rotating speed is 100 r/min, and the organic nanocellulose dispersion liquid is formed, which is set aside.

B. Preparation of blend solution of viscose collagen solution and organic nanocellulose dispersion

Put the viscose collagen solution and the organic nanocellulose dispersion prepared in step A according to the following mass percentages: 50% viscose and 50% organic nanocellulose dispersion, put them into a mixer and stir evenly, and the stirring temperature is 20°C , the stirring time is 2 hours, the rotating speed of the mixer is 100 rpm, and a blended solution is formed, which is set aside.

C. Filtration and defoaming of blended solution

The blended solution prepared in step B was filtered twice, poured into a defoaming kettle, kept at 20°C, and degassed for 6 hours.

D. Spinning of blend solution

The blended solution prepared in step C is filtered, defoamed, and then spun to obtain high-strength viscose fiber. Wherein, the composition of coagulation bath: sulfuric acid 10g/L, sodium sulfate 400g/L, zinc sulfate 10g/L.

Example 10

A. Preparation of organic nanocellulose dispersion

Put the organic nanocellulose and the primary dispersion in the following mass percentages: 50% of the organic nanocellulose and 50% of the primary dispersion, put them into a blender and stir evenly, the stirring temperature is 30°C, and the stirring time is 6 hours. The rotating speed is 2000 r/min, and the organic nanocellulose dispersion liquid is formed, which is set aside.

B. Preparation of blend solution of viscose collagen solution and organic nanocellulose dispersion

Put the viscose collagen solution and the organic nanocellulose dispersion prepared in step A according to the following mass percentages: 99% viscose and 1% organic nanocellulose dispersion, put them into a mixer and stir evenly, and the stirring temperature is 22°C , the stirring time is 8 hours, the rotational speed of the mixer is 2000 rpm, and a blended solution is formed for later use.

C. Filtration and defoaming of blended solution

The blended solution prepared in step B was filtered twice, poured into a defoaming kettle, kept at 22°C, and degassed for 8 hours.

D. Spinning of blend solution

The blended solution prepared in step C is filtered, defoamed, and then spun to obtain high-strength viscose fiber. Wherein, the composition of coagulation bath: sulfuric acid 20g/L, sodium sulfate 420g/L, zinc sulfate 30g/L. the

Claims (2)

1. a preparation method for polynosic fibre, is characterized in that, described preparation method comprises the following steps:

A presses mass fraction NaOH 4.5%, and the ratio of viscose glue stoste 8% and water 87.5% makes initial dispersion;

One in inorganic nano whisker or organic nano whisker joins in initial dispersion by B, is wherein respectively by mass fraction:

Nano whisker 20 ~ 50%,

Initial dispersion 50 ~ 80%,

Put into mixer after mixing to stir, wherein whipping temp is 15 ~ 30 DEG C, and mixing time is 1 ~ 6 hour, and the rotating speed of mixer is 100 ~ 2000 turns of ∕ minute, makes nano whisker dispersion liquid;

Then C by the viscose glue dope blending of fine to nano whisker dispersion liquid and first content 8%, is wherein respectively by mass fraction:

Viscose glue stoste 50 ~ 99%,

Nano whisker dispersion liquid 1 ~ 50%,

To be stirred formation blend solution by mixer, wherein whipping temp is 20 ~ 22 DEG C, and mixing time is 2 ~ 8 hours, and the rotating speed of mixer is 100 ~ 2000 turns of ∕ minute;

Blend solution filters through twice by D, squeezes in deaeration still, is incubated under 20 ~ 22 DEG C of conditions, deaeration 6 ~ 8 hours;

Blend solution after filtration, deaeration is carried out wet spinning by E, obtained polynosic fibre, wherein, and the composition of coagulating bath: sulfuric acid 10 ~ 20g ∕ L, sodium sulphate 400 ~ 420g/L, zinc sulfate 10 ~ 30g/L.

2. the preparation method of a kind of polynosic fibre as claimed in claim 1, is characterized in that:

Described inorganic nano whisker is the one in nanometer silicon carbide or CNT or nano zine oxide;

Described organic nano whisker is the one of nanoprotein whisker or nano-cellulose whisker.