CN110230111A - A method of Lyocell fibers are prepared by raw material of poplar - Google Patents
A method of Lyocell fibers are prepared by raw material of poplar Download PDFInfo
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- CN110230111A CN110230111A CN201910466049.9A CN201910466049A CN110230111A CN 110230111 A CN110230111 A CN 110230111A CN 201910466049 A CN201910466049 A CN 201910466049A CN 110230111 A CN110230111 A CN 110230111A
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- lyocell fibers
- poplar
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
-
- 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
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
Abstract
The present invention relates to a kind of methods for preparing Lyocell fibers as raw material using poplar, using poplar as raw material, it is sawed and is broken into wood powder, wood pulp cellulose is made using Sealed steam cooking, alkali process, the dissolution of LiCl/ dimethyl acetamide mixed solvent and the processes such as precipitation；Then wood pulp cellulose is dissolved in N-methylmorpholine-N- oxide and spinning solution is made, spinning solution is entered into spinning system and carries out spinning；The process such as finally fiber wire is washed, washed, oiled and dried through alcohol, Lyocell fibers are made.The success that the present invention extracts cellulose from poplar greatly reduces the production cost of Lyocell fibers；The purifying technique of wood pulp cellulose and the production technology of Lyocell fibers are environmentally protective, simple process, have preferable popularization and application prospect.
Description
Technical field
The invention belongs to Lyocell fibers technical fields, and in particular to one kind prepares Lyocell fibers by raw material of poplar
Method.
Background technique
For Chemical Fibre Industry of China, although yield already takes up the whole world seventy percent, still there are some scientific and technological contents
Fiber species high, that added value is high cannot achieve complete " domestic ", especially fiber art used for textiles we still there are many
Blank needs are filled up, such as: Lyocell fibers.The spies such as Lyocell fibers have natural environmental-protective, moisture absorption pro-skin, softness is glossy
Point, can match in excellence or beauty natural fiber, be many high-grade clothings, family's textile fabric and the fiber product for defending the favor of material field.But this
One first grade goods of sample, for many years, the raw material of Lyocell fibers relies on always import, and the primary raw material of foreign Lyocell fibers is
Trees.
In order to realize the primary raw material production domesticization of Lyocell fibers, in conjunction with the actual features of our countries, poplar can be made
It pays attention to for the primary raw material of Lyocell fibers.Poplar distribution is wide, North gets LiaoNing, China south, the Inner Mongol, south to the Changjiang river
Basin, using the Yellow River middle and lower reaches as normal region；Poplar growth is very fast, and adaptable, saline-alkali tolerant sets greatly resistance to water-wet, deep-rootedness, root
System is flourishing, and rhizosphere sprout tillers is strong, resistance to flue dust, antipollution.In addition, the content of cellulose is higher in poplar, up to 40% or more.
Therefore, poplar has the potential quality as Lyocell fibers primary raw material.
Summary of the invention
For Lyocell fibers feedstock purification difficulty, big, raw material variety source complexity problem, the present invention are with poplar
Raw material prepares Lyocell fibers.The purpose of the present invention is overcoming the shortcomings of conventional art, one kind is provided using poplar as raw material
The method for preparing Lyocell fibers, the method comprises the following steps:
(1) preparation of spinning solution: by mass fraction be 50~55% N-methylmorpholine-N- oxide (NMMO) it is water-soluble
Liquid is evaporated under reduced pressure to the aqueous solution of 80~90% NMMO, and wood pulp cellulose is dissolved in the aqueous solution of NMMO, in a kettle in
105~120 DEG C of vacuum stirrings dissolve 4~5 hours, and the spinning solution for the homogeneous transparent that mass fraction is 10~18% is made；
(2) spinning of Lyocell fibers: screw extruder is added in step (1) treated spinning solution, at 95~110 DEG C
Lower further dissolution, is then filtered, into spinning system, wherein gas length is 6~9cm, and spinning speed is 35~50m/
Min, the hole diameter of spinneret are 10~110 μm, 300~900 μm of hole long capillary tube；The perpendicular stretching in air of the silk thread of ejection,
Into coagulating tank, solidification forming, the aqueous solution for the NMMO that solidification bath concentration is 12~15%, coagulation bath temperature is 2~9 DEG C；
(3) alcohol of fiber is washed: step (2) treated fiber being immersed the ethanol solution that concentration is 75~95%, is immersed
Time is 3~4 hours, and solution temperature is room temperature, 1 ︰ 30~40 of bath raio；
(4) washing of fiber: step (3) treated fiber being immersed in 75~95 DEG C of hot water, and the time is 2~3 small
When, 1 ︰ 40~50 of bath raio；
(5) fiber oils: by the oil bath solution of step (4) treated fiber immerses 3~4g/L, oil bath temperature 80
~85 DEG C, the time is 2~4 hours, 1 ︰ 20~30 of bath raio；
(6) drying of fiber: by step (5), treated, and fiber obtains Lyocell fibers after drying and processing.
In the step (1) wood pulp cellulose the preparation method comprises the following steps:
Step 01: white poplar wood saw being broken into wood powder, wood powder and water are put into Sealed steam cooking pot with certain proportion and steamed
It boils, the ratio of wood powder and water is 1 ︰ 20~30；
Preferably, boiling temperature is 170~210 DEG C in the step 01, and pressure is 5~10atm, and the processing time is 3~5
Hour；The wood powder is sieved using the sieve of 50~200 mesh；
Step 02: the filter residue that step 01 is handled immerses the sodium hydroxide solution of 10~20g/L, 1 ︰ 20~25 of bath raio, place
65~80 DEG C of temperature of reason is handled the time 2~3 hours；The liquor natrii hypochloritis of 5~8g/L is immersed, treatment temperature is 45~55 DEG C,
Immersing the time is 3~4 hours；
Step 03: the filter residue that step 02 is handled is dissolved in the in the mixed solvent of LiCl/ dimethyl acetamide, heating stirring
It makes it dissolve, treatment temperature is 100~105 DEG C, and immersing the time is 3~4 hours；The mistake while hot when solution is cooled to 40~50 DEG C
Filter, by the excessive ice-water bath of filtrate added drop-wise to stirring, the volume of ice-water bath and the volume ratio of solution are as follows: 100~200 ︰ 1, analysis
Substance out is cellulose；
Preferably, in the step 03 LiCl/ dimethyl acetamide mixed solvent the preparation method comprises the following steps: LiCl is dissolved in
Dimethyl acetamide makes the mass fraction 5~10% of LiCl；
The present invention has the following obvious advantages:
(1) present invention to poplar using Sealed steam cooking, alkali process, LiCl/ dimethyl acetamide mixed solvent dissolution with
Wood pulp cellulose is made in the processes such as precipitation；This method is that a kind of extraction efficient, simple, cheap, that environmental pollution is small is fine
The method for tieing up element.
(2) success that cellulose is extracted from poplar greatly reduces the production cost of Lyocell fibers, is lyocell
The marketing of fiber is laid a good foundation.
(3) purifying technique of wood pulp cellulose of the invention and the production technology of Lyocell fibers are environmentally protective, process
It is short, be conducive to promote and apply.
Detailed description of the invention
The electron microscope of Fig. 1 Lyocell fibers prepared by the present invention
Specific embodiment
The present invention is described in detail in embodiment described below.
Embodiment 1
In the present embodiment, a method of preparing Lyocell fibers by raw material of poplar, include the following steps:
(1) preparation of spinning solution: the aqueous solution by mass fraction for 52.1% NMMO is evaporated under reduced pressure to 83.4%
1000g wood pulp cellulose is dissolved in the aqueous solution of 8L NMMO by the aqueous solution of NMMO, in a kettle in 105~120 DEG C of vacuum
Stirring and dissolving 4~5 hours, the spinning solution for the homogeneous transparent that mass fraction is 11.11% is made；
In the step (1) wood pulp cellulose the preparation method comprises the following steps:
Step 01: white poplar wood saw being broken into wood powder, is sieved using the sieve of 50 mesh；Wood powder and water are put with the ratio of 1 ︰ 22
Enter and carry out boiling in Sealed steam cooking pot, boiling temperature is 190 DEG C, pressure 8atm, and the processing time is 4 hours；
Step 02: the filter residue that step 01 is handled immerses the sodium hydroxide solution of 15g/L, 1 ︰ 23 of bath raio, treatment temperature 70
DEG C, it handles the time 2.5 hours；The liquor natrii hypochloritis of 6g/L is immersed, treatment temperature is 50 DEG C, and immersing the time is 3.5 hours；
Step 03: the filter residue that step 02 is handled is dissolved in the in the mixed solvent of LiCl/ dimethyl acetamide, LiCl/ bis-
The mass fraction of methylacetamide in the mixed solvent LiCl is 6%；Heating stirring makes it dissolve, and treatment temperature is 103 DEG C, immerses
Time is 3.5 hours；It is filtered while hot when solution is cooled to 40 DEG C, by the excessive ice-water bath of filtrate added drop-wise to stirring, ice water
The volume of bath and the volume ratio of solution are as follows: 100 ︰ 1, the substance of precipitation are cellulose；
(2) spinning of Lyocell fibers: being added screw extruder for step (1) treated spinning solution, at 100 DEG C into
The dissolution of one step, is then filtered, into spinning system, wherein gas length 7cm, spinning speed 40m/min, spinneret hole
Diameter is 50 μm, 400 μm of hole long capillary tube；The perpendicular stretching in air of the silk thread of ejection, into coagulating tank, solidification forming,
The aqueous solution for the NMMO that bath concentration is 13% is solidified, coagulation bath temperature is 3~5 DEG C；
(3) alcohol of fiber is washed: step (2) treated fiber being immersed the ethanol solution that concentration is 80%, immerses the time
It is 3.5 hours, solution temperature is room temperature, 1 ︰ 35 of bath raio；
(4) washing of fiber: step (3) treated fiber being immersed in 90 DEG C of hot water, and the time is 2.5 hours, bath
Than 1 ︰ 45；
(5) fiber oils: by the oil bath solution of step (4) treated fiber immerses 3.5g/L, oil bath temperature 84
DEG C, the time is 2.5 hours, 1 ︰ 25 of bath raio；
(6) drying of fiber: by step (5), treated, and fiber obtains Lyocell fibers after drying and processing, the Lay
The electron microscope of Sai Er fiber is as shown in Figure 1.
Embodiment 2
In the present embodiment, a method of preparing Lyocell fibers by raw material of poplar, include the following steps:
(1) preparation of spinning solution: the aqueous solution by mass fraction for 51.7% NMMO is evaporated under reduced pressure to 88.3%
1400g wood pulp cellulose is dissolved in the aqueous solution of 8L NMMO by the aqueous solution of NMMO, molten in 115 DEG C of vacuum stirrings in a kettle
The spinning solution for the homogeneous transparent that mass fraction is 14.89% is made in solution 4 hours；
In the step (1) wood pulp cellulose the preparation method comprises the following steps:
Step 01: white poplar wood saw being broken into wood powder, is sieved using the sieve of 100 mesh；By wood powder and water with the ratio of 1 ︰ 23
It is put into Sealed steam cooking pot and carries out boiling, boiling temperature is 200 DEG C, pressure 9atm, and the processing time is 4 hours；
Step 02: the filter residue that step 01 is handled immerses the sodium hydroxide solution of 18g/L, 1 ︰ 22 of bath raio, treatment temperature 70
DEG C, handle time 2 h；The liquor natrii hypochloritis of 7g/L is immersed, treatment temperature is 52 DEG C, and immersing the time is 3 hours；
Step 03: the filter residue that step 02 is handled is dissolved in the in the mixed solvent of LiCl/ dimethyl acetamide, LiCl/ bis-
The mass fraction of methylacetamide in the mixed solvent LiCl is 6%；Heating stirring makes it dissolve, and treatment temperature is 105 DEG C, immerses
Time is 4 hours；It is filtered while hot when solution is cooled to 50 DEG C, by the excessive ice-water bath of filtrate added drop-wise to stirring, ice-water bath
Volume and solution volume ratio are as follows: 150 ︰ 1, the substance of precipitation are cellulose；
(2) spinning of Lyocell fibers: being added screw extruder for step (1) treated spinning solution, at 106 DEG C into
The dissolution of one step, is then filtered, into spinning system, wherein gas length 8cm, spinning speed 43m/min, spinneret hole
Diameter is 40 μm, 400 μm of hole long capillary tube；The perpendicular stretching in air of the silk thread of ejection, into coagulating tank, solidification forming,
The aqueous solution for the NMMO that bath concentration is 13% is solidified, coagulation bath temperature is 6~7 DEG C；
(3) alcohol of fiber is washed: step (2) treated fiber being immersed the ethanol solution that concentration is 75%, immerses the time
It is 3 hours, solution temperature is room temperature, 1 ︰ 30 of bath raio；
(4) washing of fiber: step (3) treated fiber being immersed in 75 DEG C of hot water, and the time is 2 hours, bath raio
1 ︰ 40；
(5) fiber oils: by the oil bath solution of step (4) treated fiber immerses 3g/L, oil bath temperature is 80 DEG C,
Time is 2 hours, 1 ︰ 20 of bath raio；
(6) drying of fiber: by step (5), treated, and fiber obtains Lyocell fibers after drying and processing.
Embodiment 3
In the present embodiment, a method of preparing Lyocell fibers by raw material of poplar, include the following steps:
(1) preparation of spinning solution: the aqueous solution by mass fraction for 53.6% NMMO is evaporated under reduced pressure to 88.9%
1700g wood pulp cellulose is dissolved in the aqueous solution of 8L NMMO by the aqueous solution of NMMO, molten in 120 DEG C of vacuum stirrings in a kettle
The spinning solution for the homogeneous transparent that mass fraction is 17.53% is made in solution 5 hours；
In the step (1) wood pulp cellulose the preparation method comprises the following steps:
Step 01: white poplar wood saw being broken into wood powder, is sieved using 150 purpose sieve；By wood powder and water with the ratio of 1 ︰ 30
Example, which is put into Sealed steam cooking pot, carries out boiling, and boiling temperature is 190 DEG C, pressure 8atm, and the processing time is 4 hours；
Step 02: the filter residue that step 01 is handled immerses the sodium hydroxide solution of 18g/L, 1 ︰ 24 of bath raio, treatment temperature 75
DEG C, it handles the time 3 hours；The liquor natrii hypochloritis of 7g/L is immersed, treatment temperature is 50 DEG C, and immersing the time is 3 hours；
Step 03: the filter residue that step 02 is handled is dissolved in the in the mixed solvent of LiCl/ dimethyl acetamide, LiCl/ bis-
The mass fraction of methylacetamide in the mixed solvent LiCl is 9%；Heating stirring makes it dissolve, and treatment temperature is 105 DEG C, immerses
Time is 3 hours；It is filtered while hot when solution is cooled to 48 DEG C, by the excessive ice-water bath of filtrate added drop-wise to stirring, ice-water bath
Volume and solution volume ratio are as follows: 200 ︰ 1, the substance of precipitation are cellulose；
(2) spinning of Lyocell fibers: being added screw extruder for step (1) treated spinning solution, at 106 DEG C into
The dissolution of one step, is then filtered, into spinning system, wherein gas length 8cm, spinning speed 48m/min, spinneret hole
Diameter is 80 μm, 800 μm of hole long capillary tube；The perpendicular stretching in air of the silk thread of ejection, into coagulating tank, solidification forming,
The aqueous solution for the NMMO that bath concentration is 14% is solidified, coagulation bath temperature is 2~3 DEG C；
(3) alcohol of fiber is washed: step (2) treated fiber being immersed the ethanol solution that concentration is 95%, immerses the time
It is 4 hours, solution temperature is room temperature, 1 ︰ 40 of bath raio；
(4) washing of fiber: step (3) treated fiber being immersed in 95 DEG C of hot water, and the time is 3 hours, bath raio
1 ︰ 50；
(5) fiber oils: by the oil bath solution of step (4) treated fiber immerses 4g/L, oil bath temperature is 85 DEG C,
Time is 4 hours, 1 ︰ 30 of bath raio；
(6) drying of fiber: by step (5), treated, and fiber obtains Lyocell fibers after drying and processing.
Claims (4)
1. a kind of method for preparing Lyocell fibers as raw material using poplar, which is characterized in that the preparation including wood pulp cellulose
The preparation method of method and the spinning solution for being used to prepare Lyocell fibers:
It is used to prepare the preparation of the spinning solution of Lyocell fibers: by the aqueous solution decompression steaming for the NMMO that mass fraction is 50~55%
It evaporates to the aqueous solution of 80~90% NMMO, wood pulp cellulose is dissolved in the aqueous solution of NMMO, in a kettle in 105~120
DEG C be stirred under vacuum dissolution 4~5 hours, be made homogeneous transparent spinning solution；
The wood pulp cellulose the preparation method comprises the following steps:
Step 01: white poplar wood saw being broken into wood powder, wood powder and water are put into Sealed steam cooking pot and carry out boiling, filter residue, wood is made
The ratio of powder and water is 1 ︰ 20~30；
Step 02: the filter residue that step 01 is handled immerses the sodium hydroxide solution of 10~20g/L, 1 ︰ 20~25 of bath raio, processing temperature
65~80 DEG C of degree is handled the time 2~3 hours；The liquor natrii hypochloritis of 5~8g/L is immersed, treatment temperature is 45~55 DEG C, is immersed
Time is 3~4 hours；
Step 03: the filter residue that step 02 is handled is dissolved in the in the mixed solvent of LiCl/ dimethyl acetamide, and heating stirring makes it
Dissolution, treatment temperature are 100~105 DEG C, and immersing the time is 3~4 hours；It is filtered while hot when solution is cooled to 40~50 DEG C,
By in the ice-water bath of filtrate added drop-wise to stirring, the volume of ice-water bath and the volume ratio of solution are as follows: 100~200 ︰ 1, the substance of precipitation
As cellulose.
2. a kind of method for preparing Lyocell fibers as raw material using poplar according to claim 1, it is characterised in that: institute
The mass fraction for stating the spinning solution of obtained homogeneous transparent is 10~18%.
3. a kind of method for preparing Lyocell fibers as raw material using poplar according to claim 1, it is characterised in that: institute
Stating boiling temperature in step 01 is 170~210 DEG C, and pressure is 5~10atm, and the processing time is 3~5 hours；The wood powder uses
The sieve of 50~200 mesh is sieved.
4. a kind of method for preparing Lyocell fibers as raw material using poplar according to claim 1, it is characterised in that: institute
State LiCl/ dimethyl acetamide mixed solvent in step 03 the preparation method comprises the following steps: is dissolved in dimethyl acetamide for LiCl, makes
The mass fraction of LiCl is 5~10%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110894621A (en) * | 2019-11-06 | 2020-03-20 | 当阳市鸿阳新材料科技有限公司 | Preparation process and equipment for reducing fibrillation of lyocell fibers |
| WO2022139727A1 (en) * | 2020-12-21 | 2022-06-30 | Bahcesehir Universitesi | Production of dental floss from wood fibers |
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| CN109234826A (en) * | 2018-09-20 | 2019-01-18 | 武汉纺织大学 | A method of Lyocell fibers are prepared by raw material of bamboo |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110894621A (en) * | 2019-11-06 | 2020-03-20 | 当阳市鸿阳新材料科技有限公司 | Preparation process and equipment for reducing fibrillation of lyocell fibers |
| CN110894621B (en) * | 2019-11-06 | 2022-06-21 | 当阳市鸿阳新材料科技有限公司 | Preparation process and equipment for reducing fibrillation of lyocell fibers |
| WO2022139727A1 (en) * | 2020-12-21 | 2022-06-30 | Bahcesehir Universitesi | Production of dental floss from wood fibers |
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