CN103255488B - Preparation method of high-strength viscose fiber - Google Patents
Preparation method of high-strength viscose fiber Download PDFInfo
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Abstract
The invention relates to a preparation method of high-strength viscose fiber, belonging to the technical field of textile fiber processing. The preparation method mainly comprises the steps of dispersing inorganic nano whisker or organic nano whisker through dispersion liquid, then blending with a viscose stock solution, and preparing high-strength viscose fiber filament or staple fiber through the process flows of stirring, standing for deaeration, filtering, spinning and the like. The strength of the prepared viscose fiber is higher than that of the viscose fiber spun by a traditional process by above 20-50%. The preparation method provided by the invention is simple in process, convenient to operate and control, and easy to realize industrialized production, and does not need special equipment. The strength of the viscose fiber prepared by the preparation method is higher than that of the viscose fiber prepared by a conventional method, and the viscose fiber is wide in application.
Description
Technical field
The present invention relates to a kind of preparation method of polynosic fibre, belong to textile fabric processing technique field.
Background technology
Viscose is with a long history, and as far back as 19 end of the centurys, scientist Cross, Bevan, Beadle of Britain have just invented the method preparing cellulose sulfonic acid fat.Over more than 100 year, due to viscose raw material native cellulose wide material sources, belong to regenerated resources; Product wearability is good, has moisture absorption, ventilative, softness, easy dyeing, the series of advantages such as antistatic, makes it wear as snug as a bug in a rug; And viscose energy natural degradation, can not environmental pollution be caused.Although viscose has above-mentioned series of advantages, its shortcoming is apparent: its brute force is low, especially wet poor by force; Washing shrinkage is high; Poor flexibility, dress or washing after crease easily, arch camber, affect fabric attractive in appearance.
China publication CN101775671A, publication date on July 14th, 2010, invention and created name is a kind of polynosic fibre and production method thereof, this application case discloses a kind of polynosic fibre and production method thereof, it is characterized in that being mixed with rayon spinning solution by bacteria cellulose and making viscose.Its production method comprises step: carry out preliminary treatment to sheet bacteria cellulose, then adopts ball-milling method to pulverize the bacterial cellulose powder obtaining micro/nano level; Above-mentioned bacterial cellulose powder is added in viscose spinning solution and be uniformly dispersed and deaeration, obtain spinning solution; Above-mentioned spinning solution is made polynosic fibre.The viscose prepared by this inventive method, its intensity is high, and washing shrinkage is little, good springiness, can with cotton, hair and other synthetic fiber blending, intertexture, for the field such as high-grade fabric and fabrics for industrial use.But the method needs first sheet bacteria cellulose to be made bacterial cellulose powder, then directly bacterial cellulose powder to be joined in viscose spinning solution, the method operating process is loaded down with trivial details, technique length consuming time, and bacterial cellulose powder particle mixes uneven with viscose spinning solution, easily affect the performance of fiber.
Therefore, how effectively to prepare polynosic fibre, and technical process is simple and easy to control, there is great Social and economic benef@, be conducive to the industrial upgrading promoting China's chemical fibre industry.
Summary of the invention
For above-mentioned existing problems, the object of the invention is to overcome above-mentioned defect, a kind of preparation method of polynosic fibre be provided, for the technical solution meeting the object of the invention is:
A preparation method for polynosic fibre, 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.
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.
Owing to have employed above technical scheme, Advantageous Effects of the present invention is:
1 the present invention utilizes the advantage of the high strength of nano whisker, high-modulus and high elongation rate, obtain blend solution with viscose glue dope blending after inorganic (or organic) nano whisker is made dispersion liquid, obtain polynosic fibre by technological processes such as stirring, standing and defoaming, filtration, spinning.Viscose glue and dispersion liquid do not react in the basic conditions, are a kind of physical blending processes, do not injure the performance of nano whisker high strength, high-modulus and high elongation rate.And inorganic (or organic) nano whisker wide material sources, alternative more, and subsequent technique adjustment is little.
Polynosic fibre obtained by 2 the present invention not only has higher intensity, and gained viscose fiber strength is intensity that traditional handicraft is spun high more than 20 ~ 50% comparatively; And there are good elasticity, hygroscopicity, stainability, corrosion resistance, bulkiness etc., be widely used.
The preparation method of 3 a kind of polynosic fibres of the present invention, can directly at the enterprising Row sum-equal matrix of viscose glue production technology; Without the need to special installation, produce at common viscose glue and spinning process equipment can produce polynosic fibre; The convenient easily control of operating process, is easy to realize suitability for industrialized production.
Detailed description of the invention
A preparation method for polynosic fibre, 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.
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.
Embodiment 1
A. the preparation of inorganic nano silicon carbide dispersion
Inorganic nano carborundum and initial dispersion are pressed following mass percent: inorganic nano carborundum 20%, the ratio of initial dispersion 80%, put into mixer to stir, whipping temp is 15 DEG C, mixing time is 1 hour, the rotating speed of mixer is that 100 turns of ∕ divide, and forms inorganic nano silicon carbide dispersion, for subsequent use.
B. prepared by the blend solution of viscose glue stoste and inorganic nano silicon carbide dispersion
Viscose glue stoste and the inorganic nano silicon carbide dispersion obtained through step A are pressed following mass percent: viscose glue 50%, the ratio of inorganic nano silicon carbide dispersion 50%, put into mixer to stir, whipping temp is 20 DEG C, mixing time is 2 hours, the rotating speed of mixer is that 100 turns of ∕ divide, and forms blend solution, for subsequent use.
C. the filtration of blend solution, deaeration
The blend solution prepared through step B is filtered through twice, squeezes in deaeration still, 20 DEG C of insulations, deaeration 6 hours.
D. the spinning of blend solution
By through the obtained blend solution of step C after filtration, carry out spinning, obtained polynosic fibre after deaeration.Wherein, the composition of coagulating bath: sulfuric acid 10g ∕ L, sodium sulphate 400g/L, zinc sulfate 10g/L.
Embodiment 2
A. the preparation of inorganic nano silicon carbide dispersion
Inorganic nano carborundum and initial dispersion are pressed following mass percent: inorganic nano carborundum 50%, the ratio of initial dispersion 50%, put into mixer to stir, whipping temp is 30 DEG C, mixing time is 6 hours, the rotating speed of mixer is that 2000 turns of ∕ divide, and forms inorganic nano silicon carbide dispersion, for subsequent use.
B. prepared by the blend solution of viscose glue stoste and inorganic nano silicon carbide dispersion
Viscose glue stoste and the inorganic nano silicon carbide dispersion obtained through step A are pressed following mass percent: viscose glue 99%, the ratio of inorganic nano silicon carbide dispersion 1%, put into mixer to stir, whipping temp is 22 DEG C, mixing time is 8 hours, the rotating speed of mixer is that 2000 turns of ∕ divide, and forms blend solution, for subsequent use.
C. the filtration of blend solution, deaeration
The blend solution prepared through step B is filtered through twice, squeezes in deaeration still, 22 DEG C of insulations, deaeration 8 hours.
D. the spinning of blend solution
By through the obtained blend solution of step C after filtration, carry out spinning, obtained polynosic fibre after deaeration.Wherein, the composition of coagulating bath: sulfuric acid 20g ∕ L, sodium sulphate 420g/L, zinc sulfate 30g/L.
Embodiment 3
A. the preparation of inorganic carbon nano tube dispersion liquid
DIC nanotube and initial dispersion are pressed following mass percent: DIC nanotube 20%, the ratio of initial dispersion 80%, put into mixer to stir, whipping temp is 15 DEG C, mixing time is 1 hour, the rotating speed of mixer is that 100 turns of ∕ divide, and forms inorganic carbon nano tube dispersion liquid, for subsequent use.
B. prepared by the blend solution of viscose glue stoste and inorganic carbon nano tube dispersion liquid
Viscose glue stoste and the inorganic carbon nano tube dispersion liquid obtained through step A are pressed following mass percent: viscose glue 50%, the ratio of inorganic carbon nano tube dispersion liquid 50%, put into mixer to stir, whipping temp is 20 DEG C, mixing time is 2 hours, the rotating speed of mixer is that 100 turns of ∕ divide, and forms blend solution, for subsequent use.
C. the filtration of blend solution, deaeration
The blend solution prepared through step B is filtered through twice, squeezes in deaeration still, 20 DEG C of insulations, deaeration 6 hours.
D. the spinning of blend solution
By through the obtained blend solution of step C after filtration, carry out spinning, obtained polynosic fibre after deaeration.Wherein, the composition of coagulating bath: sulfuric acid 10g ∕ L, sodium sulphate 400g/L, zinc sulfate 10g/L.
Embodiment 4
A. the preparation of inorganic carbon nano tube dispersion liquid
DIC nanotube and initial dispersion are pressed following mass percent: DIC nanotube 50%, the ratio of initial dispersion 50%, put into mixer to stir, whipping temp is 30 DEG C, mixing time is 6 hours, the rotating speed of mixer is that 2000 turns of ∕ divide, and forms inorganic carbon nano tube dispersion liquid, for subsequent use.
B. prepared by the blend solution of viscose glue stoste and inorganic carbon nano tube dispersion liquid
Viscose glue stoste and the inorganic carbon nano tube dispersion liquid obtained through step A are pressed following mass percent: viscose glue 99%, the ratio of inorganic carbon nano tube dispersion liquid 1%, put into mixer to stir, whipping temp is 22 DEG C, mixing time is 8 hours, the rotating speed of mixer is that 2000 turns of ∕ divide, and forms blend solution, for subsequent use.
C. the filtration of blend solution, deaeration
The blend solution prepared through step B is filtered through twice, squeezes in deaeration still, 22 DEG C of insulations, deaeration 8 hours.
D. the spinning of blend solution
By through the obtained blend solution of step C after filtration, carry out spinning, obtained polynosic fibre after deaeration.Wherein, the composition of coagulating bath: sulfuric acid 20g ∕ L, sodium sulphate 420g/L, zinc sulfate 30g/L.
Embodiment 5
A. the preparation of inorganic nano zinc oxide fluid dispersion
Inorganic nano zinc oxide and initial dispersion are pressed following mass percent: inorganic nano zinc oxide 20%, the ratio of initial dispersion 80%, put into mixer to stir, whipping temp is 15 DEG C, mixing time is 1 hour, the rotating speed of mixer is that 100 turns of ∕ divide, and forms inorganic nano zinc oxide fluid dispersion, for subsequent use.
B. prepared by the blend solution of viscose glue stoste and inorganic nano zinc oxide fluid dispersion
Viscose glue stoste and the inorganic nano zinc oxide fluid dispersion obtained through step A are pressed following mass percent: viscose glue 50%, the ratio of inorganic nano zinc oxide fluid dispersion 50%, put into mixer to stir, whipping temp is 20 DEG C, mixing time is 2 hours, the rotating speed of mixer is that 100 turns of ∕ divide, and forms blend solution, for subsequent use.
C. the filtration of blend solution, deaeration
The blend solution prepared through step B is filtered through twice, squeezes in deaeration still, 20 DEG C of insulations, deaeration 6 hours.
D. the spinning of blend solution
By through the obtained blend solution of step C after filtration, carry out spinning, obtained polynosic fibre after deaeration.Wherein, the composition of coagulating bath: sulfuric acid 10g ∕ L, sodium sulphate 400g/L, zinc sulfate 10g/L.
Embodiment 6
A. the preparation of inorganic nano zinc oxide fluid dispersion
Inorganic nano zinc oxide and initial dispersion are pressed following mass percent: inorganic nano zinc oxide 50%, the ratio of initial dispersion 50%, put into mixer to stir, whipping temp is 30 DEG C, mixing time is 6 hours, the rotating speed of mixer is that 2000 turns of ∕ divide, and forms inorganic nano zinc oxide fluid dispersion, for subsequent use.
B. prepared by the blend solution of viscose glue stoste and inorganic nano zinc oxide fluid dispersion
Viscose glue stoste and the inorganic nano zinc oxide fluid dispersion obtained through step A are pressed following mass percent: viscose glue 99%, the ratio of inorganic nano zinc oxide fluid dispersion 1%, put into mixer to stir, whipping temp is 22 DEG C, mixing time is 8 hours, the rotating speed of mixer is that 2000 turns of ∕ divide, and forms blend solution, for subsequent use.
C. the filtration of blend solution, deaeration
The blend solution prepared through step B is filtered through twice, squeezes in deaeration still, 22 DEG C of insulations, deaeration 8 hours.
D. the spinning of blend solution
By through the obtained blend solution of step C after filtration, carry out spinning, obtained polynosic fibre after deaeration.Wherein, the composition of coagulating bath: sulfuric acid 20g ∕ L, sodium sulphate 420g/L, zinc sulfate 30g/L.
Embodiment 7
A. the preparation of organic nano albumen microcrystalline dispersion liquid
Organic nano albumen crystallite and initial dispersion are pressed following mass percent: organic nano albumen crystallite 20%, the ratio of initial dispersion 80%, put into mixer to stir, whipping temp is 15 DEG C, mixing time is 1 hour, the rotating speed of mixer is that 100 turns of ∕ divide, and forms organic nanoprotein microcrystalline dispersion liquid, for subsequent use.
B. prepared by the blend solution of viscose glue stoste and organic nano albumen microcrystalline dispersion liquid
Viscose glue stoste and the organic nano albumen microcrystalline dispersion liquid obtained through step A are pressed following mass percent: viscose glue 50%, the ratio of organic nano albumen microcrystalline dispersion liquid 50%, put into mixer to stir, whipping temp is 20 DEG C, mixing time is 2 hours, the rotating speed of mixer is that 100 turns of ∕ divide, and forms blend solution, for subsequent use.
C. the filtration of blend solution, deaeration
The blend solution prepared through step B is filtered through twice, squeezes in deaeration still, 20 DEG C of insulations, deaeration 6 hours.
D. the spinning of blend solution
By through the obtained blend solution of step C after filtration, carry out spinning, obtained polynosic fibre after deaeration.Wherein, the composition of coagulating bath: sulfuric acid 10g ∕ L, sodium sulphate 400g/L, zinc sulfate 10g/L.
Embodiment 8
A. the preparation of organic nano albumen microcrystalline dispersion liquid
Organic nano albumen crystallite and initial dispersion are pressed following mass percent: organic nano albumen crystallite 50%, the ratio of initial dispersion 50%, put into mixer to stir, whipping temp is 30 DEG C, mixing time is 6 hours, the rotating speed of mixer is that 2000 turns of ∕ divide, and forms organic nanoprotein microcrystalline dispersion liquid, for subsequent use.
B. prepared by the blend solution of viscose glue stoste and organic nano albumen microcrystalline dispersion liquid
Viscose glue stoste and the organic nano albumen microcrystalline dispersion liquid obtained through step A are pressed following mass percent: viscose glue 99%, the ratio of organic nano albumen microcrystalline dispersion liquid 1%, put into mixer to stir, whipping temp is 22 DEG C, mixing time is 8 hours, the rotating speed of mixer is that 2000 turns of ∕ divide, and forms blend solution, for subsequent use.
The blend solution prepared through step B filters through twice by the C. filtration of blend solution, deaeration, squeezes in deaeration still, 22 DEG C of insulations, and deaeration 8 hours.
D. the spinning of blend solution
By through the obtained blend solution of step C after filtration, carry out spinning, obtained polynosic fibre after deaeration.Wherein, the composition of coagulating bath: sulfuric acid 20g ∕ L, sodium sulphate 420g/L, zinc sulfate 30g/L.
Embodiment 9
A. the preparation of organic nanofibers element dispersion liquid
Organic nanofibers element is pressed following mass percent with initial dispersion: organic nanofibers element 20%, the ratio of initial dispersion 80%, put into mixer to stir, whipping temp is 15 DEG C, mixing time is 1 hour, the rotating speed of mixer is that 100 turns of ∕ divide, and forms organic nano-cellulose dispersion liquid, for subsequent use.
B. prepared by the blend solution of viscose glue stoste and organic nanofibers element dispersion liquid
Viscose glue stoste and the organic nanofibers element dispersion liquid obtained through step A are pressed following mass percent: viscose glue 50%, the ratio of organic nanofibers element dispersion liquid 50%, put into mixer to stir, whipping temp is 20 DEG C, mixing time is 2 hours, the rotating speed of mixer is that 100 turns of ∕ divide, and forms blend solution, for subsequent use.
C. the filtration of blend solution, deaeration
The blend solution prepared through step B is filtered through twice, squeezes in deaeration still, 20 DEG C of insulations, deaeration 6 hours.
D. the spinning of blend solution
By through the obtained blend solution of step C after filtration, carry out spinning, obtained polynosic fibre after deaeration.Wherein, the composition of coagulating bath: sulfuric acid 10g ∕ L, sodium sulphate 400g/L, zinc sulfate 10g/L.
Embodiment 10
A. the preparation of organic nanofibers element dispersion liquid
Organic nanofibers element is pressed following mass percent with initial dispersion: organic nanofibers element 50%, the ratio of initial dispersion 50%, put into mixer to stir, whipping temp is 30 DEG C, mixing time is 6 hours, the rotating speed of mixer is that 2000 turns of ∕ divide, and forms organic nano-cellulose dispersion liquid, for subsequent use.
B. prepared by the blend solution of viscose glue stoste and organic nanofibers element dispersion liquid
Viscose glue stoste and the organic nanofibers element dispersion liquid obtained through step A are pressed following mass percent: viscose glue 99%, the ratio of organic nanofibers element dispersion liquid 1%, put into mixer to stir, whipping temp is 22 DEG C, mixing time is 8 hours, the rotating speed of mixer is that 2000 turns of ∕ divide, and forms blend solution, for subsequent use.
C. the filtration of blend solution, deaeration
The blend solution prepared through step B is filtered through twice, squeezes in deaeration still, 22 DEG C of insulations, deaeration 8 hours.
D. the spinning of blend solution
By through the obtained blend solution of step C after filtration, carry out spinning, obtained polynosic fibre after deaeration.Wherein, the composition of coagulating bath: sulfuric acid 20g ∕ L, sodium sulphate 420g/L, zinc sulfate 30g/L.
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.
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CN103643334B (en) * | 2013-12-17 | 2016-04-13 | 青岛大学 | The preparation method of Fire resistant viscose fiber |
EP2889400A1 (en) * | 2013-12-24 | 2015-07-01 | SAPPI Netherlands Services B.V. | Cellulosic fibres or filaments reinforced with inorganic particles and method for the production thereof |
CN104877145B (en) * | 2014-02-28 | 2017-12-08 | 恒天海龙(潍坊)新材料有限责任公司 | Preparation method of natural organic whisker dispersion liquid and application of dispersion liquid prepared by using method |
CN104451930B (en) * | 2014-11-20 | 2017-07-14 | 江苏金太阳纺织科技股份有限公司 | A kind of preparation method of whisker reinforcement regenerated celulose fibre |
CN105113034A (en) * | 2015-08-06 | 2015-12-02 | 北京林业大学 | Regenerated cellulose fiber and preparing method thereof |
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TW202042777A (en) * | 2019-02-12 | 2020-12-01 | 大江生醫股份有限公司 | A rayon fiber mask containing integrated fruit and vegetable and berry ferments for moisturizing and anti-aging |
CN110042491A (en) * | 2019-05-28 | 2019-07-23 | 冉国庆 | A kind of manufacturing method of carbon nanotube (CNT) viscose rayon |
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CN112030251B (en) * | 2020-08-25 | 2021-07-13 | 四川大学 | Holocellulose nano composite fiber and preparation method thereof |
CN116657264A (en) * | 2023-06-01 | 2023-08-29 | 潍坊欣龙生物材料有限公司 | Method for improving color depth and glossiness of black cellulose fiber |
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