CN107869008B - A kind of preparation method of cellulose not weaving fabric of superfine fiber - Google Patents
A kind of preparation method of cellulose not weaving fabric of superfine fiber Download PDFInfo
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- CN107869008B CN107869008B CN201711071049.6A CN201711071049A CN107869008B CN 107869008 B CN107869008 B CN 107869008B CN 201711071049 A CN201711071049 A CN 201711071049A CN 107869008 B CN107869008 B CN 107869008B
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- cellulose
- methylmorpholine
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
- D04H3/10—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between yarns or filaments made mechanically
- D04H3/11—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between yarns or filaments made mechanically by fluid jet
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/013—Regenerated cellulose series
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
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Abstract
The present invention provides a kind of preparation methods of cellulose not weaving fabric of superfine fiber, comprise the following steps: cellulose pulp being dissolved in N-methylmorpholine-N- oxide hydrate, cellulose solution is obtained；The cellulose solution is subjected to spinning, obtains the cellulose fibre strand net of the oxide of-N- containing N-methylmorpholine；Spun lacing processing is carried out to the cellulose fibre strand net of the oxide of-N- containing N-methylmorpholine, obtains cellulose not weaving fabric of superfine fiber.Present invention combination spining technology and spun lacing technology successfully can obtain cellulose not weaving fabric of superfine fiber when using non-volatile solvents N-methylmorpholine-N- oxide.
Description
Technical field
The present invention relates to spinning process technical field more particularly to a kind of preparation sides of cellulose not weaving fabric of superfine fiber
Method.
Background technique
Cellulose is reserves natural polymer the most abundant in nature, has renewable, advantages of environment protection.It is fine
Cellulose fiber has low-density, biggish specific surface area, high intensity and the excellent properties such as biodegradable and hydrophily, In
Artificial skin, artificial blood vessel, nerve suture protection housing, training micro- surgery models, animal wound dressing, make up paper membrane,
The fields such as food additives, additive for paper making and bioengineering show good prospect.
With the development of fiber technology of preparing, the technology of preparing of superfine fibre or even nanofiber is developed rapidly.
Due to having many advantages, such as that diameter is small, large specific surface area, superfine fibre is considered as a kind of high-performance, high added value fiber product,
Have in fields such as filtering material, heat insulating material, oil absorption material, medical and health, battery separator and acoustic materials extensive
Using.
Solution jet spinning technology is a kind of novel nano fiber technology of preparing, and the basic principle of this method is to utilize high speed
Air-flow carries out superthin drafting to polymer solution, while being gradually formed by curing not weaving fabric of superfine fiber with the volatilization of solvent,
The advantages that technology has processing flow short, and process flow is simple, and condition is easy to control, and is easy to large-scale production.In recent years should
Technology has become the effective ways of large-scale production nanofiber.However, mainly utilizing the volatility of solvent in the technology
So that solvent gradually volatilizees in solution thread drawing process and polymer is made to be cured as fiber.But due to the dissolution of cellulose
Property is poor, only finds a few direct solvent at present, as lithium chloride/dimethyl acetamide (LiCl/DMAc), ionic liquid,
N-methylmorpholine-N- oxide (NMMO) etc., and above-mentioned solvent does not have volatile characteristic, accordingly, it is difficult to using existing
Cellulose superfine fibre is made in solution jet spinning technology.
Summary of the invention
It is provided by the invention the purpose of the present invention is to provide a kind of preparation method of cellulose not weaving fabric of superfine fiber
Method can prepare cellulose fibre and its product using solution jet spinning technology when using non-volatile solvents NMMO.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of preparation methods of cellulose not weaving fabric of superfine fiber, comprise the following steps:
Cellulose pulp is dissolved in N-methylmorpholine-N- oxide hydrate, cellulose solution is obtained；
The cellulose solution is subjected to spinning, obtains the cellulose fibre strand net of the oxide of-N- containing N-methylmorpholine；
Spun lacing processing is carried out to the cellulose fibre strand net of the oxide of-N- containing N-methylmorpholine, obtains cellulose
Not weaving fabric of superfine fiber.
Preferably, water content is lower than 13wt.% in the N-methylmorpholine-N- oxide hydrate.
Preferably, the mass concentration of cellulose is 4~15% in the cellulose solution.
It preferably, also include gallate in the cellulose solution；
The mass ratio of the gallate and cellulose is (0.5~1): 100.
Preferably, the spinning is solution jet spinning.
Preferably, the temperature of cellulose solution is 90~120 DEG C in the solution jet spinning, the feed flow of cellulose solution
Rate is 200~300mL/min；High speed attenuating blast temperature is 110~160 DEG C, and outlet pressure is 0.15~0.6MPa.
Preferably, the diameter of fiber is 1~3 μ in the oxide fibre of-N- containing the N-methylmorpholine cellulose fiber strand net
m。
Preferably, the pressure of the spun lacing processing is 1~10MPa.
Preferably, the fibre diameter of the cellulose not weaving fabric of superfine fiber is 400~2000nm.
The present invention provides a kind of preparation methods of cellulose not weaving fabric of superfine fiber, comprise the following steps: by fiber
Plain pulp is dissolved in N-methylmorpholine-N- oxide hydrate, obtains cellulose solution；The cellulose solution is spun
Silk, obtains the cellulose fibre strand net of the oxide of-N- containing N-methylmorpholine；To the oxide of-N- containing N-methylmorpholine
Cellulose fibre strand net carries out spun lacing processing, obtains cellulose not weaving fabric of superfine fiber.Present invention combination spining technology and
Spun lacing technology successfully can obtain cellulose superfine fibre when using non-volatile solvents N-methylmorpholine-N- oxide
Non-woven cloth.
N-methylmorpholine-N- oxide (NMMO) has very strong dipole N+O-, close with high electronics at O atom
Degree, the oxygen atom of the group can also form class with cellulose with the formation hydrogen bond such as some substances containing-OH such as water, alcohol
As hydrogen bond, therefore to cellulose have good dissolubility.The NMMO solvent of low-water-content is known as very strong dissolution to fiber
Ability can be made into the concentration cellulose element spinning solution with false modeling behavior when solution temperature is at 90~120 DEG C (up to
40%), and cellulose hardly happens depolymerization.Moreover, NMMO fusing point with higher, the fusing point of pure NMMO is 172 DEG C, one
The fusing point of hydrate is 78 DEG C, and NMMO is easily soluble in water, this is to prepare the ultra-fine fibre of cellulose using solution jet spinning technology
Dimension non-woven cloth provides possibility.
Specific embodiment
The present invention provides a kind of preparation methods of cellulose not weaving fabric of superfine fiber, comprise the following steps:
Cellulose pulp is dissolved in N-methylmorpholine-N- oxide hydrate, cellulose solution is obtained；
The cellulose solution is subjected to spinning, obtains the cellulose fibre strand net of the oxide of-N- containing N-methylmorpholine；
Spun lacing processing is carried out to the cellulose fibre strand net of the oxide of-N- containing N-methylmorpholine, obtains cellulose
Not weaving fabric of superfine fiber.
Cellulose pulp is dissolved in N-methylmorpholine-N- oxide (NMMO) hydrate by the present invention, and it is molten to obtain cellulose
Liquid.The present invention does not have any particular/special requirement to the source of the cellulose pulp, and use is well-known to those skilled in the art
Cellulose pulp.In the present invention, the degree of polymerization of the cellulose pulp is preferably 600~1200, more preferably 700~
1100, most preferably 900~1000.In the specific embodiment of the invention, the cellulose pulp is specially wood pulps or cotton pulp
The dregs of rice.
In the present invention, water content is preferably shorter than 13wt.% in the N-methylmorpholine-N- oxide hydrate, more excellent
It is selected as lower than 10wt.%, most preferably less than 5wt.%.
In the present invention, the mass concentration of cellulose is preferably 4~15% in the cellulose solution, more preferably 6~
12%, most preferably 8~10%.
It in the present invention, preferably also include gallate in the cellulose solution；The gallate and fiber
The mass ratio of element is preferably (0.5~1): 100, more preferably (0.6~0.9): 100, most preferably (0.7~0.8): 100.In
In the present invention, the addition of the gallate enables to the product finally obtained to have antioxygenic property.
After obtaining the cellulose solution, the cellulose solution is carried out spinning by the present invention, is obtained containing N-methylmorpholine-
The cellulose fibre strand net of N- oxide.In the present invention, the spinning is preferably solution jet spinning.In the present invention,
The temperature of cellulose solution is preferably 90~120 DEG C in the solution jet spinning, and more preferably 95~110 DEG C, most preferably
100~105 DEG C；The feed flow rate of the cellulose solution is preferably 200~300mL/min, more preferably 220~280mL/
Min, most preferably 240~260mL/min.
In the present invention, the solution jet spinning high speed attenuating blast temperature is preferably 110~160 DEG C, more preferably
It is 120~150 DEG C, most preferably 130~140 DEG C；Outlet pressure is preferably 0.15~0.6MPa, more preferably 0.3~
0.5MPa；High speed attenuating blast flow velocity is preferably 90~180m/s, more preferably 100~160m/s, most preferably 120~
140m/s。
In the present invention, the wire hole internal diameter of spinning plate is preferably 0.18~0.5mm in the solution jet spinning, more preferably
For 0.25~0.45mm, most preferably 0.3~0.4mm；Reception distance in the solution jet spinning is preferably 1.5~3m,
More preferably 2~2.5m.
In the present invention, the oxide fibre of-N- containing the N-methylmorpholine cellulose fiber strand net is by cellulose fibre silk
The mixed and disorderly intertexture of item stacks the network structure formed；In the oxide fibre cellulose fiber strand net of-N- containing N-methylmorpholine
The diameter of fiber is preferably 1~3 μm, and more preferably 2 μm.
After obtaining the cellulose fibre strand net of the oxide of-N- containing N-methylmorpholine, the present invention is to the methyl containing N-
The cellulose fibre strand net of quinoline-N- oxide carries out spun lacing processing, obtains cellulose not weaving fabric of superfine fiber.In the present invention
In, the pressure of the spun lacing processing is preferably 1~10MPa, more preferably 2~8MPa, most preferably 4~6MPa.
In the present invention, the spun lacing processing preferably comprises the processing of 2~5 spun lacings, specifically can be 2,3,4
Or 5.In the present invention, when spun lacing processing preferably comprises the processing of 2~5 spun lacings, the pressure of per pass spun lacing processing is only
It is on the spot preferably 1~10MPa, more preferably 2~8MPa, most preferably 4~6MPa.In the present invention, the spun lacing handles energy
N-methylmorpholine-N- oxide in the cellulose fibre strand net of the enough removal oxides of-N- containing N-methylmorpholine.
Preferably to spun lacing, treated that product is dried by the present invention, obtains that dry cellulose superfine fibre is non-to be knitted
Make cloth.In the present invention, the temperature of the drying process is preferably 110~150 DEG C, and more preferably 120~140 DEG C, most preferably
It is 125~135 DEG C.The present invention does not have any particular/special requirement to the time of the drying process, can dry the cellulose
Not weaving fabric of superfine fiber.
In the present invention, the fibre diameter of the cellulose not weaving fabric of superfine fiber is preferably 400~2000nm, more excellent
It is selected as 1000~1500nm.
It is carried out below with reference to preparation method of the embodiment to cellulose not weaving fabric of superfine fiber provided by the invention detailed
Explanation, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
The cotton pulp cellulose pulp that the degree of polymerization is 600 (DP) is dissolved in NMMO at 100 DEG C and obtains mass fraction
12% solution obtains uniform spinning solution after deaeration.It is subjected to spinning, spinning parameter using solution jet spinning technology
Are as follows: spinning solution delivery rate is 200mL/min, and drawing-off wind pressure (injection pressure) is set as 0.6MPa, and wind-warm syndrome is 130 DEG C.It spins
Silk solution thread refines under high-temperature high-speed airflow, and aggregation forms reticular structure after cooling on porous reception lace curtaining, in net
Under curtain support, spun lacing area is delivered into, successively passes through three water jets, pressure is respectively 3MPa, 6MPa and 10MPa, is gone
Except the cellulose not weaving fabric of superfine fiber of NMMO, dry cellulose superfine fibre is obtained through cylinder penetration drying machine drying
Non-woven cloth, it is 620~1100nm that SEM, which observes its distribution of fiber diameters,.
Embodiment 2
Polymer poly right (DP) wood pulp cellulose pulp for being 1200 is dissolved in NMMO at 120 DEG C and obtains quality
8% solution of score, obtains uniform spinning solution after deaeration.It is subjected to spinning, spinning ginseng using solution jet spinning technology
Number are as follows: spinning solution delivery rate is 300mL/min, and drawing-off wind pressure (injection pressure) is set as 0.5MPa, and wind-warm syndrome is 110 DEG C.
Spinning solution thread refines under high-temperature high-speed airflow, and aggregation forms reticular structure, In after cooling on porous reception lace curtaining
Under lace curtaining support, spun lacing area is delivered into, successively passes through four water jets, pressure is respectively 3MPa, 6MPa, 6MPa and 10MPa,
The cellulose not weaving fabric of superfine fiber of removal NMMO is obtained, it is super to obtain dry cellulose through cylinder penetration drying machine drying
Fine fibre non-woven cloth, it is 810~1300nm that SEM, which observes its distribution of fiber diameters,.
Embodiment 3
Polymer poly right (DP) cotton pulp cellulose pulp for being 700 is dissolved in NMMO at 100 DEG C and obtains quality
11% solution of score, obtains uniform spinning solution after deaeration.It is subjected to spinning, spinning ginseng using solution jet spinning technology
Number are as follows: spinning solution delivery rate is 300mL/min, and drawing-off wind pressure (injection pressure) is set as 0.5MPa, and wind-warm syndrome is 110 DEG C.
Spinning solution thread refines under high-temperature high-speed airflow, and aggregation forms reticular structure, In after cooling on porous reception lace curtaining
Under lace curtaining support, spun lacing area is delivered into, successively passes through three water jets, pressure is respectively 3MPa, 8MPa and 10MPa, is obtained
The cellulose not weaving fabric of superfine fiber for removing NMMO, obtains the ultra-fine fibre of dry cellulose through cylinder penetration drying machine drying
Non-woven cloth is tieed up, it is 810~1300nm that SEM, which observes its distribution of fiber diameters,.
As seen from the above embodiment, the present invention provides a kind of preparation method of cellulose not weaving fabric of superfine fiber, packets
Containing following steps: cellulose pulp being dissolved in N-methylmorpholine-N- oxide hydrate, cellulose solution is obtained；It will be described
Cellulose solution carries out spinning, obtains the cellulose fibre strand net of the oxide of-N- containing N-methylmorpholine；To the methyl containing N-
The cellulose fibre strand net of methylmorpholine-N-oxide carries out spun lacing processing, obtains cellulose not weaving fabric of superfine fiber.The present invention
In conjunction with spining technology and spun lacing technology, can successfully be obtained when using non-volatile solvents N-methylmorpholine-N- oxide
Cellulose not weaving fabric of superfine fiber.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of cellulose not weaving fabric of superfine fiber, comprises the following steps:
Cellulose pulp is dissolved in N-methylmorpholine-N- oxide hydrate, cellulose solution is obtained；
The cellulose solution is subjected to spinning, obtains the cellulose fibre strand net of the oxide of-N- containing N-methylmorpholine；
Spun lacing processing is carried out to the cellulose fibre strand net of the oxide of-N- containing N-methylmorpholine, it is ultra-fine to obtain cellulose
Fiber non-woven；
Water content is lower than 13wt.% in the N-methylmorpholine-N- oxide hydrate.
2. preparation method according to claim 1, which is characterized in that the mass concentration of cellulose in the cellulose solution
It is 4~15%.
3. preparation method according to claim 1, which is characterized in that also include gallic acid in the cellulose solution
Ester；
The mass ratio of the gallate and cellulose is (0.5~1): 100.
4. preparation method according to claim 1, which is characterized in that the spinning is solution jet spinning.
5. the preparation method according to claim 4, which is characterized in that the temperature of cellulose solution in the solution jet spinning
Degree is 90~120 DEG C, and the feed flow rate of cellulose solution is 200~300mL/min；High speed attenuating blast temperature is 110~160
DEG C, outlet pressure is 0.15~0.6MPa.
6. preparation method according to claim 5, which is characterized in that the oxide fibre of-N- containing N-methylmorpholine
The diameter of fiber is 1~3 μm in cellulose fiber strand net.
7. preparation method according to claim 1, which is characterized in that the pressure of the spun lacing processing is 1~10MPa.
8. preparation method according to claim 1 or claim 7, which is characterized in that the cellulose not weaving fabric of superfine fiber
Fibre diameter be 400~2000nm.
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| CN201711071049.6A CN107869008B (en) | 2017-11-03 | 2017-11-03 | A kind of preparation method of cellulose not weaving fabric of superfine fiber |
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| CN201711071049.6A CN107869008B (en) | 2017-11-03 | 2017-11-03 | A kind of preparation method of cellulose not weaving fabric of superfine fiber |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071542A (en) * | 2011-02-22 | 2011-05-25 | 天津工业大学 | Method for preparing polymeric nano-micro fiber non-woven fabric |
| CN103556235A (en) * | 2013-10-28 | 2014-02-05 | 山东英利实业有限公司 | Preparation technology of cellulose fiber spinning solution |
| CN105350182A (en) * | 2015-11-25 | 2016-02-24 | 青岛大学 | Technology and equipment for preparing artificial fiber filament non-woven fabric on basis of dry spinning technique |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015111619A1 (en) * | 2014-01-24 | 2015-07-30 | 日東紡績株式会社 | Type i crystal-containing long regenerated cellulose fibers |
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2017
- 2017-11-03 CN CN201711071049.6A patent/CN107869008B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071542A (en) * | 2011-02-22 | 2011-05-25 | 天津工业大学 | Method for preparing polymeric nano-micro fiber non-woven fabric |
| CN103556235A (en) * | 2013-10-28 | 2014-02-05 | 山东英利实业有限公司 | Preparation technology of cellulose fiber spinning solution |
| CN105350182A (en) * | 2015-11-25 | 2016-02-24 | 青岛大学 | Technology and equipment for preparing artificial fiber filament non-woven fabric on basis of dry spinning technique |
Non-Patent Citations (1)
| Title |
|---|
| Solution blowing of submicron-scale cellulose fibers;Xupin Zhuang et al;《Carbohydrate Polymers》;20121001;第90卷(第2期);第982-987页 * |
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