CN109505033A - The preparation method of Cellulose nanocrystal enhancing alginic acid composite fibre - Google Patents
The preparation method of Cellulose nanocrystal enhancing alginic acid composite fibre Download PDFInfo
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- CN109505033A CN109505033A CN201811566790.4A CN201811566790A CN109505033A CN 109505033 A CN109505033 A CN 109505033A CN 201811566790 A CN201811566790 A CN 201811566790A CN 109505033 A CN109505033 A CN 109505033A
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- cnc
- alginic acid
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
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- Engineering & Computer Science (AREA)
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Abstract
The present invention relates to cellulose technology fields, more particularly to a kind of preparation method of Cellulose nanocrystal enhancing alginic acid composite fibre.Cellulose nanocrystal enhances the preparation method of alginic acid composite fibre, includes the following steps: the preparation of (1) CNC；(2) preparation of alginic acid-CNC composite fibre.The present invention prepares Cellulose nanocrystal by acid hydrolyzation with microcrystalline cellulose, and CNC is added into sodium alginate soln, spinning solution is made, using calcium chloride solution as coagulating bath, a series of alginic acid-CNC composite fibres are prepared using wet spinning technology, manufactured CNC even molecular weight distribution, average grain diameter is in 115.5 nm, and dispersion stabilization is good in water.The addition of CNC improves the mechanical property of alginic acid fibre.
Description
Technical field
The present invention relates to cellulose technology fields, enhance alginic acid composite fibre more particularly to a kind of Cellulose nanocrystal
Preparation method.
Background technique
Sodium alginate is the natural polysaccharide extracted from seaweed, the alginic acid be prepared by it by wet spinning
Fiber has many excellent performances such as good biocompatibility, degradability, nontoxic, adsorptivity and anti-flammability, and makees
The fields such as hospital gauze and textile garment are widely used in for high performance green fiber.However due to alginic acid fibre Dan Qiang
It is low, curling less, cohesive force it is poor, greatly limit its application range.The method for improving alginic acid fibre mechanical property at present is main
It is by being modified to it.
Representative of the Cellulose nanocrystal as cellulose based nano material, not only remains the property of native cellulose, together
When assign nanoparticle with characteristics such as high intensity, high crystalline, high-specific surface area, high-tensiles.It is poured on the market using solution
Note legal system obtains aqueous polyurethane/Cellulose nanocrystal composite membrane (WBPU/CNC), to the mechanical property of composite membrane and other performances
It is analyzed, CNC, which is added, in discovery can effectively improve the tensile strength, Young's modulus and storage modulu of WBPU, the increasing to WBPU
Potent fruit is obvious；Therefore, nano cellulose crystal has good application value as the reinforced phase of composite material.
Summary of the invention
The present invention is directed in view of the above-mentioned problems, proposing a kind of preparation side of nanocrystalline enhancing alginic acid composite fibre of dimension element
Method.
Technical program of the present invention lies in:
Cellulose nanocrystal enhances the preparation method of alginic acid composite fibre, includes the following steps:
(1) preparation of CNC；
It takes MCC to mix with deionized water, is placed in ice bath, dense H is added dropwise while stirring2SO4；After being added dropwise to complete, it is heated
To 45 ~ 50 DEG C, 100 ~ 110 min of acidolysis reaction, CNC is obtained, stops heating and being added 10 times of deionized water dilution and terminates instead
It answers；Supernatant liquor is removed after gained suspension is put into supercentrifuge, until generating without precipitating；The centrifugation of last time is produced
Object is put into bag filter, and dialysis is no longer changed to pH value, and the liquid after the completion of dialysis is put into freeze drier and is obtained
Final product；
(2) preparation of alginic acid-CNC composite fibre；
The sodium alginate soln for preparing mass fraction 5 ~ 8%, it is above-mentioned CNC is evenly dispersed in water then itself and sodium alginate is molten
Successively blending and stirring is uniform for liquid, obtains alginic acid-CNC composite fiber spinning stoste；Spinning solution is spun after deaeration through self-control
Silk machine uniformly squeezes out, the solidification forming in coagulating bath, obtains alginic acid-CNC composite fibre after drawn and washing.
The revolving speed of the supercentrifuge is 10000 ~ 12000r/min, and centrifugation time is 10 ~ 15 min.
The CNC it is evenly dispersed in water when by ultrasonic wave.
In the preparation process of the alginic acid-CNC composite fibre, the mass fraction of CNC be 0%, 0.5%, 2%, 8% and
16%。
The coagulating bath is the CaCl of mass fraction 5 ~ 8%2Coagulating bath.
The acidolysis reaction carries out under electric stirring.
The technical effects of the invention are that:
The present invention prepares Cellulose nanocrystal by acid hydrolyzation with microcrystalline cellulose, and CNC is added into sodium alginate soln
Spinning solution is made, it is compound that a series of alginic acid-CNC are prepared using wet spinning technology using calcium chloride solution as coagulating bath
Fiber, manufactured CNC even molecular weight distribution, average grain diameter is in 115.5 nm, and dispersion stabilization is good in water.CNC's
Addition improves the mechanical property of alginic acid fibre.
Specific embodiment
Embodiment 1
Cellulose nanocrystal enhances the preparation method of alginic acid composite fibre, includes the following steps:
(1) preparation of CNC
It takes MCC to mix with deionized water, is placed in ice bath, dense H is added dropwise while stirring2SO4；After being added dropwise to complete, it is heated
To 45 ~ 50 DEG C, 100 ~ 110 min of acidolysis reaction is carried out under electric stirring, obtains CNC, stop heating and be added 10 times and go
Ionized water dilution terminates reaction；Gained suspension is put into after supercentrifuge and removes supernatant liquor, supercentrifuge rotating speed is
10000 ~ 12000r/min, centrifugation time is 10 ~ 15 min, until generating without precipitating；The centrifugation product of last time is put into
In bag filter, dialysis is no longer changed to pH value, and the liquid after the completion of dialysis is put into freeze drier and is finally produced
Object；
(2) preparation of alginic acid-CNC composite fibre
The sodium alginate soln for preparing mass fraction 5 ~ 8%, above-mentioned CNC is evenly dispersed by ultrasonic wave for 2% with mass fraction
In water, then by it with sodium alginate soln successively blending and stirring is uniform, obtains alginic acid-CNC composite fiber spinning stoste；It spins
Silk stock solution is made by oneself spinning machine and is uniformly squeezed out, in the CaCl of mass fraction 5 ~ 8% after deaeration2Solidification forming in coagulating bath,
Alginic acid-CNC composite fibre is obtained after drawn and washing, CNC can preferably disperse in sodium alginate soln, CNC's
Addition improves the mechanical property of alginic acid fibre.
Embodiment 2
Cellulose nanocrystal enhances the preparation method of alginic acid composite fibre, includes the following steps:
(1) preparation of CNC
It takes MCC to mix with deionized water, is placed in ice bath, dense H is added dropwise while stirring2SO4；After being added dropwise to complete, it is heated
To 45 ~ 50 DEG C, 100 ~ 110 min of acidolysis reaction is carried out under electric stirring, obtains CNC, stop heating and be added 10 times and go
Ionized water dilution terminates reaction；Gained suspension is put into after supercentrifuge and removes supernatant liquor, supercentrifuge rotating speed is
10000 ~ 12000r/min, centrifugation time is 10 ~ 15 min, until generating without precipitating；The centrifugation product of last time is put into
In bag filter, dialysis is no longer changed to pH value, and the liquid after the completion of dialysis is put into freeze drier and is finally produced
Object；
(2) preparation of alginic acid-CNC composite fibre
The sodium alginate soln for preparing mass fraction 5 ~ 8%, above-mentioned CNC is evenly dispersed by ultrasonic wave for 8% with mass fraction
In water, then by it with sodium alginate soln successively blending and stirring is uniform, obtains alginic acid-CNC composite fiber spinning stoste；It spins
Silk stock solution is made by oneself spinning machine and is uniformly squeezed out, in the CaCl of mass fraction 5 ~ 8% after deaeration2Solidification forming in coagulating bath,
Alginic acid-CNC composite fibre is obtained after drawn and washing, the tensile break strength of alginic acid fibre increases 46.8%, fracture
Elongation increases 111.9%.
Embodiment 3
Cellulose nanocrystal enhances the preparation method of alginic acid composite fibre, includes the following steps:
(1) preparation of CNC
It takes MCC to mix with deionized water, is placed in ice bath, dense H is added dropwise while stirring2SO4；After being added dropwise to complete, it is heated
To 45 ~ 50 DEG C, 100 ~ 110 min of acidolysis reaction is carried out under electric stirring, obtains CNC, stop heating and be added 10 times and go
Ionized water dilution terminates reaction；Gained suspension is put into after supercentrifuge and removes supernatant liquor, supercentrifuge rotating speed is
10000 ~ 12000r/min, centrifugation time is 10 ~ 15 min, until generating without precipitating；The centrifugation product of last time is put into
In bag filter, dialysis is no longer changed to pH value, and the liquid after the completion of dialysis is put into freeze drier and is finally produced
Object；
(2) preparation of alginic acid-CNC composite fibre
The sodium alginate soln for preparing mass fraction 5 ~ 8%, above-mentioned CNC is evenly dispersed by ultrasonic wave for 16% with mass fraction
In water, then by it with sodium alginate soln successively blending and stirring is uniform, obtains alginic acid-CNC composite fiber spinning stoste；It spins
Silk stock solution is made by oneself spinning machine and is uniformly squeezed out, in the CaCl of mass fraction 5 ~ 8% after deaeration2Solidification forming in coagulating bath,
Alginic acid-CNC composite fibre is obtained after drawn and washing, CNC forms aggregation in sodium alginate soln, causes fracture strong
It spends and fracture elongation is as the addition of CNC constantly declines.
Claims (6)
1. the preparation method of Cellulose nanocrystal enhancing alginic acid composite fibre, characterized by the following steps:
(1) preparation of CNC；
It takes MCC to mix with deionized water, is placed in ice bath, dense H is added dropwise while stirring2SO4；After being added dropwise to complete, it is heated to
45 ~ 50 DEG C, 100 ~ 110 min of acidolysis reaction, CNC is obtained, stops heating and being added 10 times of deionized water dilution and terminates reaction；
Supernatant liquor is removed after gained suspension is put into supercentrifuge, until generating without precipitating；By the centrifugation product of last time
It is put into bag filter, dialysis is no longer changed to pH value, and the liquid after the completion of dialysis is put into freeze drier and is obtained most
Final product；
(2) preparation of alginic acid-CNC composite fibre；
The sodium alginate soln for preparing mass fraction 5 ~ 8%, it is above-mentioned CNC is evenly dispersed in water then itself and sodium alginate is molten
Successively blending and stirring is uniform for liquid, obtains alginic acid-CNC composite fiber spinning stoste；Spinning solution is spun after deaeration through self-control
Silk machine uniformly squeezes out, the solidification forming in coagulating bath, obtains alginic acid-CNC composite fibre after drawn and washing.
2. the preparation method of Cellulose nanocrystal enhancing alginic acid composite fibre according to claim 1, it is characterised in that:
The revolving speed of the supercentrifuge is 10000 ~ 12000r/min, and centrifugation time is 10 ~ 15 min.
3. the preparation method of Cellulose nanocrystal enhancing alginic acid composite fibre according to claim 2, it is characterised in that:
The CNC it is evenly dispersed in water when by ultrasonic wave.
4. the preparation method of Cellulose nanocrystal enhancing alginic acid composite fibre according to claim 3, it is characterised in that:
In the preparation process of the alginic acid-CNC composite fibre, the mass fraction of CNC is 0%, 0.5%, 2%, 8% and 16%.
5. the preparation method of Cellulose nanocrystal enhancing alginic acid composite fibre according to claim 4, it is characterised in that:
The coagulating bath is the CaCl of mass fraction 5 ~ 8%2Coagulating bath.
6. the preparation method of Cellulose nanocrystal enhancing alginic acid composite fibre according to claim 5, it is characterised in that:
The acidolysis reaction carries out under electric stirring.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110607569A (en) * | 2019-09-16 | 2019-12-24 | 东华大学 | Method for preparing nano cellulose liquid crystal microfiber through two-dimensional domain-limited self-assembly |
| CN112495349A (en) * | 2020-12-14 | 2021-03-16 | 江南大学 | Cellulose nanocrystal loaded sodium alginate adsorbent and application thereof in enrichment of organic phosphorus in wastewater |
| CN113832560A (en) * | 2021-09-23 | 2021-12-24 | 中南大学 | Clay-cellulose-alginic acid composite flame-retardant macrofiber and preparation and application thereof |
| CN113908328A (en) * | 2021-09-10 | 2022-01-11 | 浙江海洋大学 | Antibacterial hemostatic porous microsphere based on sodium alginate and nanocrystalline cellulose |
| CN114479203A (en) * | 2022-02-23 | 2022-05-13 | 山东大学 | Method for optimizing compatibility of sodium alginate/carrageenan composite thin film by response surface method |
| CN114505059A (en) * | 2021-12-27 | 2022-05-17 | 辽宁大学 | Preparation method of porous cellulose nanocrystalline-sodium alginate gel microspheres |
-
2018
- 2018-12-21 CN CN201811566790.4A patent/CN109505033A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110607569A (en) * | 2019-09-16 | 2019-12-24 | 东华大学 | Method for preparing nano cellulose liquid crystal microfiber through two-dimensional domain-limited self-assembly |
| CN110607569B (en) * | 2019-09-16 | 2022-01-18 | 东华大学 | Method for preparing nano cellulose liquid crystal microfiber through two-dimensional domain-limited self-assembly |
| CN112495349A (en) * | 2020-12-14 | 2021-03-16 | 江南大学 | Cellulose nanocrystal loaded sodium alginate adsorbent and application thereof in enrichment of organic phosphorus in wastewater |
| CN112495349B (en) * | 2020-12-14 | 2021-12-03 | 江南大学 | Cellulose nanocrystal loaded sodium alginate adsorbent and application thereof in enrichment of organic phosphorus in wastewater |
| US11577220B2 (en) | 2020-12-14 | 2023-02-14 | Jiangnan University | Cellulose nanocrystal-supported sodium alginate adsorbent |
| CN113908328A (en) * | 2021-09-10 | 2022-01-11 | 浙江海洋大学 | Antibacterial hemostatic porous microsphere based on sodium alginate and nanocrystalline cellulose |
| CN113908328B (en) * | 2021-09-10 | 2023-01-24 | 浙江海洋大学 | Antibacterial hemostatic porous microsphere based on sodium alginate and nanocrystalline cellulose |
| CN113832560A (en) * | 2021-09-23 | 2021-12-24 | 中南大学 | Clay-cellulose-alginic acid composite flame-retardant macrofiber and preparation and application thereof |
| CN113832560B (en) * | 2021-09-23 | 2023-12-22 | 中南大学 | Clay-cellulose-alginic acid composite flame-retardant large fiber and preparation and application thereof |
| CN114505059A (en) * | 2021-12-27 | 2022-05-17 | 辽宁大学 | Preparation method of porous cellulose nanocrystalline-sodium alginate gel microspheres |
| CN114505059B (en) * | 2021-12-27 | 2024-01-09 | 辽宁大学 | Preparation method of porous cellulose nanocrystalline-sodium alginate gel microsphere |
| CN114479203A (en) * | 2022-02-23 | 2022-05-13 | 山东大学 | Method for optimizing compatibility of sodium alginate/carrageenan composite thin film by response surface method |
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