CN114045568A - Preparation method of deodorizing far infrared health care regenerated cellulose fiber - Google Patents

Preparation method of deodorizing far infrared health care regenerated cellulose fiber Download PDF

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Publication number
CN114045568A
CN114045568A CN202111462326.2A CN202111462326A CN114045568A CN 114045568 A CN114045568 A CN 114045568A CN 202111462326 A CN202111462326 A CN 202111462326A CN 114045568 A CN114045568 A CN 114045568A
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deodorizing
preparation
far infrared
health care
regenerated cellulose
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Inventor
李昌垒
刘乐
孙东升
秦翠梅
马君志
王东
房德建
李利建
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Weifang Xinlong Biomaterials Co Ltd
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Weifang Xinlong Biomaterials Co Ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/06Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
    • D01F2/08Composition of the spinning solution or the bath
    • D01F2/10Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/02Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention provides a preparation method of deodorizing far infrared health care regenerated cellulose fiber, which comprises the steps of preparation of mixed slurry, preparation of blended spinning solution, spinning and deodorizing finishing. The deodorizing far infrared health care regenerated cellulose fiber prepared by the invention has the dry breaking strength of more than or equal to 2.30cN/dtex, the wet breaking strength of more than or equal to 1.1cN/dtex, the dry breaking elongation of more than or equal to 18.0 percent and the 2-nonenal elimination rate of more than or equal to 90 percent, has the obvious deodorizing function, has the far infrared normal emissivity of more than or equal to 0.80, and has the health care functions of activating cell tissues and promoting blood circulation.

Description

Preparation method of deodorizing far infrared health care regenerated cellulose fiber
Technical Field
The invention relates to a regenerated cellulose fiber and a preparation method thereof, in particular to a regenerated cellulose fiber with deodorization and far infrared health care functions and a preparation method thereof, belonging to the technical field of fibers.
Background
With the continuous progress of the economy and the social civilization of China, the requirements of the masses on the living taste and the social environment are increasingly improved. By middle age, the body functions begin to decline slowly, the oxidation rate of the skin is increased, and besides the age spots are easy to appear, the oxidation of the skin can generate a substance named as 2-nonenal. Meanwhile, the oil secreted on the skin or the taste of some bacteria are mixed to generate the taste, which is commonly called as old taste or old odor. Hygiene and health care become the focus of people's attention.
The viscose fiber material disclosed in the Chinese invention patent CN104947218A and the preparation method thereof, the fiber with the antibacterial and deodorizing functions prepared by the patent technology is obtained by adding one or more of silicate compounds of silicon dioxide, sodium silicate, sodium aluminosilicate, potassium aluminosilicate, calcium silicate, magnesium silicate, potassium magnesium silicate or iron silicate into stock solution for spinning, and some of the substances are water-soluble and seriously lose in the production process. And the added solid substances are not protected and easily run off, so that the functionality and the durability of the product cannot be ensured. The invention discloses CN103556275B a far infrared bamboo charcoal viscose fiber and a preparation method thereof, wherein far infrared ceramic powder added in the patent technology is metal or metal oxide, sedimentation is easy to occur, and bamboo charcoal powder and far infrared ceramic powder are both solid, bamboo charcoal has very limited adsorption capacity on the bamboo charcoal, and the physical and mechanical properties and spinnability of the fiber are seriously influenced, thereby influencing the functionality of the fiber or fabric.
The invention discloses deodorizing fiber and a manufacturing method thereof, which is disclosed by the patent CN109943901A, and the fiber is prepared by adding zeolite powder and lauric acid into chinlon to form fiber master batch, carrying out melt spinning at the highest temperature of 280 ℃, leading the loss of lauric acid component to be serious at higher temperature, leading the prepared deodorizing fiber to have unsatisfactory functionality, and leading the fiber to be synthetic fiber and leading the product to be difficult to naturally degrade. The invention patent CN102839439A discloses a preparation method of a fiber for eliminating sweat and odor, which adopts a blended spinning technology, and takes nano zinc oxide as an odor eliminating agent to degrade the odor by utilizing the photocatalytic reaction. The nano powder is difficult to disperse, and meanwhile, as the nano powder is antibacterial through a photocatalysis mechanism, the antibacterial performance of the fiber cannot play a role under the condition of no illumination.
The above patents do not mention the elimination of 2-nonenal, the far infrared health care regenerated cellulose fiber produced by the invention has the far infrared function of increasing the function of human body and delaying aging, and the selected effective component of the deodorizer JYKZOT-92 is mainly silicate water dispersion liquid, is nontoxic and tasteless, and has good deodorization effect. However, the spinning forming process of the cellulose fiber is a strong acid system, and if the deodorant is directly added into the spinning solution without protection treatment, the loss is large, and the ideal deodorization effect cannot be achieved.
Disclosure of Invention
Aiming at the problems and the defects in the prior art, the invention provides a preparation method of deodorizing far infrared health care regenerated cellulose fiber, which realizes the following purposes: reduce the loss of the deodorizing agent, improve the deodorizing performance of the fiber and ensure the mechanical performance of the fiber at the same time.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of deodorizing far infrared health care regenerated cellulose fiber comprises the steps of preparation of mixed slurry, preparation of blended spinning solution, spinning, post-treatment and deodorization finishing.
The preparation method comprises the following specific steps:
1. preparation of Mixed slurry
Slowly adding the bamboo charcoal powder and the deodorizing agent into deionized water in sequence under continuous stirring, stirring for 30min, adding a dispersing agent, grinding and dispersing for 30-60min by using a sand mill, and preparing slurry with the mass fraction of 20-35%, the particle size of less than or equal to 2um, and preferably 1.67-1.842 um.
The mass ratio of the bamboo charcoal to the deodorant in the mixed slurry is 2: 1;
the type of the deodorant is JYKZOT-92;
the dispersing agent is one or more of sodium hexametaphosphate, sodium tripolyphosphate, nano cellulose and animal gelatin;
the addition amount of the dispersant is 0.5-2wt% (relative to the weight of the dispersion).
2. Preparation of blended spinning solution
Cellulose pulp is used as a raw material, and a cellulose spinning solution is prepared by a conventional viscose preparation process and comprises the following components: 9.0-11% of alpha cellulose, 5.0-6.5% of sodium hydroxide and 50-70 s of falling ball viscosity, and adding the prepared mixed slurry into a viscose spinning solution through a dynamic or static mixer according to 1-10wt% of effective components (for alpha cellulose) to obtain a blended spinning solution.
3. Spinning
Spinning the blended spinning stock solution through a coagulating bath, wherein the coagulating bath comprises 80-90 g/L of sulfuric acid, 20-30 g/L of zinc sulfate and 260-320 g/L of sodium sulfate, and the temperature is 35-40 ℃. The fiber is slowly formed by a low-concentration low-temperature coagulating bath, so that the internal structure of fiber molecules is ensured to be neat, the orientation degree is higher, and the fiber has higher strength and elongation.
4. Deodorizing finishing
And cutting, desulfurizing and washing the spun tows, dewatering by a padder, performing a deodorizing finishing process for padding treatment, and finally oiling and drying to obtain the deodorizing far infrared health-care cellulose fiber. The deodorizing finishing process comprises the following steps: the moisture regain of the fiber before deodorization finishing is less than or equal to 120 percent, preferably is 103-120 percent; the concentration of the finishing liquid of the deodorizing agent is 5-10%, the temperature is 40-50 ℃, the time is 2-4min, and the moisture regain of the mangle fiber after deodorizing treatment is 100-.
Compared with the prior art, the invention has the beneficial effects that:
1. the deodorizing far infrared health care regenerated cellulose fiber prepared by the invention has the dry breaking strength of more than or equal to 2.30cN/dtex, preferably 2.3-2.36 cN/dtex, the wet breaking strength of more than or equal to 1.1cN/dtex, preferably 1.13-1.18 cN/dtex, the dry breaking elongation of more than or equal to 18.0 percent, preferably 18.2-18.5 percent, the 2-nonenal elimination rate of more than or equal to 90 percent, preferably 90-96 percent, has a remarkable deodorizing function, and the far infrared normal emissivity of more than or equal to 0.80, preferably 0.8-0.85, and has the health care functions of activating cell tissues and promoting blood circulation.
2. The bamboo charcoal powder is prepared by firing alpine moso bamboos which are over three years old as raw materials at high temperature of nearly thousand ℃, the moso bamboos form a special pore structure in the high-temperature pyrolysis process, the specific surface area is large, the adsorption capacity is strong, the deodorant is well protected, and the loss in the production process is avoided.
3. According to the production process, the mixed slurry of the bamboo charcoal powder and the deodorizing agent is added into the viscose spinning solution through a dynamic or static mixer for spinning, and then deodorizing finishing is carried out in the post-treatment process, so that the loss of the deodorizing agent in the spinning process is reduced, and the durability of the function of the deodorizing agent is improved.
4. The deodorant JYKZOT-92 mainly comprises silicate water dispersion liquid, does not influence the physical and mechanical properties of fibers in the using process, and has a durable deodorant effect on 2-nonenal compared with other deodorants.
Detailed Description
Example 1
1. Preparation of Mixed slurry
Slowly adding the bamboo charcoal powder and the deodorizing agent into deionized water in sequence under continuous stirring, stirring for 30min, adding dispersing agents of sodium hexametaphosphate and nanocellulose, grinding and dispersing for 30min by a sand mill, detecting the particle size D90 of the slurry to be 1.676 μm, and preparing into mixed slurry with the mass fraction of 20%.
The addition amount of the dispersing agent is 0.5wt% (relative to the weight of the dispersing liquid), the mass ratio of the sodium hexametaphosphate to the nano-cellulose is 1:1, and the mass ratio of the bamboo charcoal to the deodorizing agent in the mixed slurry is 2: 1.
The type of the deodorant is JYKZOT-92.
2. Preparation of blended spinning solution
Cellulose pulp is used as a raw material, and a cellulose spinning solution is prepared by a conventional viscose preparation process and comprises the following components: 9.65% of alpha cellulose, 5.30% of sodium hydroxide and 50s of falling ball viscosity, adding the prepared mixed slurry into the viscose spinning solution through a dynamic mixer according to the condition that the mass percent of the effective components of the mixed slurry to the alpha cellulose in the spinning solution is 1wt%, thereby obtaining the blended spinning solution.
3. Spinning
Spinning the blended spinning solution through a coagulating bath, wherein the coagulating bath comprises 80g/L of sulfuric acid, 20g/L of zinc sulfate and 260g/L of sodium sulfate, and the temperature is 35 ℃.
4. Post-treatment deodorizing finishing
And cutting, desulfurizing and washing the spun tows, dewatering by a padder, performing a deodorizing finishing process for padding treatment, and finally oiling and drying to obtain the deodorizing far infrared health-care cellulose fiber. The deodorizing finishing process comprises the following steps: the fiber moisture regain before deodorization finishing is 120%, the finishing liquor concentration of a deodorization agent (JYKZOT-92) is 5%, the temperature is 40 ℃, the time is 2min, and the mangle fiber moisture regain after deodorization processing is 105%.
The deodorizing far infrared health care regenerated cellulose fiber has the advantages of 2.36 cN/dtex of dry breaking strength, 1.18 cN/dtex of wet breaking strength, 18.5% of dry breaking elongation and 90% of 2-nonenal elimination rate, has obvious deodorizing function and 0.80 of far infrared normal emissivity.
Example 2
1. Preparation of Mixed slurry
Slowly adding the bamboo charcoal powder and the deodorizing agent into deionized water in sequence under continuous stirring, stirring for 30min, adding dispersing agent sodium hexametaphosphate and animal gelatin, grinding and dispersing for 45min by a sand mill, detecting that the particle size D90 of the slurry is 1.842 μm, and preparing into slurry with mass fraction of 25%.
The addition amount of the dispersing agent is 1.5wt% (based on the weight of the dispersing liquid), the mass ratio of the sodium hexametaphosphate to the animal gelatin is 1:1, and the mass ratio of the bamboo charcoal to the deodorant in the mixed slurry is 2: 1.
The type of the deodorant is JYKZOT-92.
2. Preparation of blended spinning solution
Cellulose pulp is used as a raw material, and a cellulose spinning solution is prepared by a conventional viscose preparation process and comprises the following components: 10.3 percent of alpha cellulose, 6.0 percent of sodium hydroxide and 62s of falling ball viscosity, adding the prepared mixed slurry into the viscose spinning solution through a static mixer according to the mass percent of 5 percent of the effective components in the alpha cellulose in the spinning solution to obtain the blended spinning solution.
3. Spinning
Spinning the blended spinning stock solution through a coagulating bath, wherein the coagulating bath comprises 85g/L sulfuric acid, 25 g/L zinc sulfate and 285g/L sodium sulfate, and the temperature is 38 ℃.
4. Post-treatment deodorizing finishing
And cutting, desulfurizing and washing the spun tows, dewatering by a padder, performing a deodorizing finishing process for padding treatment, and finally oiling and drying to obtain the deodorizing far infrared health-care cellulose fiber. The deodorizing finishing process comprises the following steps: the fiber moisture regain before deodorization finishing is 115%, the finishing liquor concentration of the deodorization agent is 7%, the temperature is 45 ℃, the time is 3min, and the mangle fiber moisture regain after deodorization processing is 112%.
The deodorizing far infrared health care regenerated cellulose fiber has the advantages of 2.32 cN/dtex of dry breaking strength, 1.16 cN/dtex of wet breaking strength, 18.3% of dry breaking elongation and 92% of 2-nonenal elimination rate, has obvious deodorizing function and 0.82 of far infrared normal emissivity.
Example 3
1. Preparation of bamboo charcoal slurry
Slowly adding the bamboo charcoal powder and the deodorizing agent into deionized water in sequence under continuous stirring, stirring for 30min, adding dispersing agent sodium tripolyphosphate and nano cellulose, grinding and dispersing for 60min by a sand mill, detecting the particle size D90 of the slurry to be 1.765 μm, and preparing the slurry with the mass fraction of the bamboo charcoal powder being 35%.
The addition amount of the dispersing agent is 2.0wt% (relative to the weight of the dispersing solution), the mass ratio of the sodium tripolyphosphate to the nano cellulose is 1:1, and the mass ratio of the bamboo charcoal to the deodorant in the mixed slurry is 2: 1.
The type of the deodorant is JYKZOT-92.
2. Preparation of blended spinning solution
Cellulose pulp is used as a raw material, and a cellulose spinning solution is prepared by a conventional viscose preparation process and comprises the following components: 10.8 percent of alpha cellulose, 6.4 percent of sodium hydroxide and 70s of falling ball viscosity, adding the prepared slurry into the viscose spinning solution through a dynamic mixer according to the mass percent of the active ingredients accounting for 10 percent by weight of the alpha cellulose in the spinning solution to obtain the blended spinning solution.
3. Spinning
Spinning the blended spinning solution through a coagulating bath, wherein the coagulating bath comprises 90g/L of sulfuric acid, 30 g/L of zinc sulfate and 315g/L of sodium sulfate, and the temperature is 40 ℃.
4. Post-treatment deodorizing finishing
And cutting, desulfurizing and washing the spun tows, dewatering by a padder, performing a deodorizing finishing process for padding treatment, and finally oiling and drying to obtain the deodorizing far infrared health-care cellulose fiber. The deodorizing finishing process comprises the following steps: the fiber moisture regain before deodorization finishing is 103%, the finishing liquor concentration of the deodorization agent is 10%, the temperature is 50 ℃, the time is 4min, and the mangle fiber moisture regain after deodorization processing is 118%.
The deodorizing far infrared health care regenerated cellulose fiber has the advantages of 2.30cN/dtex of dry breaking strength, 1.13 cN/dtex of wet breaking strength, 18.2% of dry breaking elongation and 96% of 2-nonenal elimination rate, has obvious deodorizing function and has 0.85 of far infrared normal emissivity.
Comparative example 1
On the basis of the embodiment 1, only the type of the deodorant is changed, other types of liquid deodorant are selected, and the other steps and the process parameters are the same as those of the embodiment 1, so that the prepared fiber has the following effect indexes:
Figure DEST_PATH_IMAGE001
comparative example 2
The fiber 2-nonenal produced in the same manner as in example 1 except that the post-treatment deodorizing finishing step was not carried out in addition to example 1 had an elimination rate of 63%.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that they can still make modifications to the technical solutions described in the foregoing embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (9)

1. A preparation method of deodorizing far infrared health care regenerated cellulose fiber is characterized by comprising the following steps: the preparation method comprises the steps of preparation of mixed slurry, preparation of blended spinning solution, spinning and deodorization finishing.
2. The preparation method of the deodorizing far infrared health care regenerated cellulose fiber according to claim 1, characterized in that: the preparation of the mixed slurry comprises the steps of slowly adding the bamboo charcoal powder and the deodorizing agent into deionized water in sequence, stirring, adding the dispersing agent, grinding and dispersing to prepare the mixed slurry with the mass fraction of 20-35% and the particle size of less than or equal to 2 um.
3. The preparation method of the deodorizing far infrared health care regenerated cellulose fiber according to claim 2, characterized in that: the mass content of the dispersant in the mixed slurry is 0.5-2wt%, and the dispersant is one or more of sodium hexametaphosphate, sodium tripolyphosphate, nano-cellulose and animal gelatin.
4. The preparation method of the deodorizing far infrared health care regenerated cellulose fiber according to claim 2, characterized in that: the mass ratio of the bamboo charcoal to the deodorizing agent is 2: 1.
5. The preparation method of the deodorizing far infrared health care regenerated cellulose fiber according to claim 2 or 4, characterized in that: the type of the deodorant is JYKZOT-92.
6. The preparation method of the deodorizing far infrared health care regenerated cellulose fiber according to claim 1, characterized in that: preparing the blended spinning solution, namely adding the mixed slurry into a spinning stock solution to obtain the blended spinning stock solution; the mass percentage of the effective components in the mixed slurry relative to the alpha fibers in the spinning solution is 1-10 wt%.
7. The preparation method of the deodorizing far infrared health care regenerated cellulose fiber according to claim 6, characterized in that: the spinning solution contains 9-11wt% of alpha cellulose, 5.0-6.5wt% of sodium hydroxide and 50-70 s of falling ball viscosity.
8. The preparation method of the deodorizing far infrared health care regenerated cellulose fiber according to claim 1, characterized in that: the spinning and coagulating bath comprises 80-90 g/L of sulfuric acid, 20-30 g/L of zinc sulfate and 260-320 g/L of sodium sulfate, and the temperature is 35-40 ℃.
9. The preparation method of the deodorizing far infrared health care regenerated cellulose fiber according to claim 1, characterized in that: in the deodorization finishing, the fiber moisture regain is less than or equal to 120% before the deodorization finishing, the finishing liquor concentration of the deodorization agent is 5-10%, the temperature is 40-50 ℃, the time is 2-4min, and the mangle fiber moisture regain after the deodorization treatment is 120% of 100-.
CN202111462326.2A 2021-12-02 2021-12-02 Preparation method of deodorizing far infrared health care regenerated cellulose fiber Pending CN114045568A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001098412A (en) * 1999-10-04 2001-04-10 Minabegawamura Shinrin Kumiai Deodorizing viscose rayon fiber and production of the same
JP2003253557A (en) * 2002-03-01 2003-09-10 Akebono Toba Fiber material having excellent deodorization and absorption of far infrared ray and organic chlorine compound, its fiber product and method for producing the same
CN103556275A (en) * 2013-10-31 2014-02-05 宜宾海丝特纤维有限责任公司 Far infrared bamboo charcoal viscose fiber and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001098412A (en) * 1999-10-04 2001-04-10 Minabegawamura Shinrin Kumiai Deodorizing viscose rayon fiber and production of the same
JP2003253557A (en) * 2002-03-01 2003-09-10 Akebono Toba Fiber material having excellent deodorization and absorption of far infrared ray and organic chlorine compound, its fiber product and method for producing the same
CN103556275A (en) * 2013-10-31 2014-02-05 宜宾海丝特纤维有限责任公司 Far infrared bamboo charcoal viscose fiber and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
马正升: "消臭抗菌整理剂的研发及应用", 《针织工业》 *

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