CN110230111B - Method for preparing lyocell fibers by taking poplar as raw material - Google Patents
Method for preparing lyocell fibers by taking poplar as raw material Download PDFInfo
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- CN110230111B CN110230111B CN201910466049.9A CN201910466049A CN110230111B CN 110230111 B CN110230111 B CN 110230111B CN 201910466049 A CN201910466049 A CN 201910466049A CN 110230111 B CN110230111 B CN 110230111B
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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
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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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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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
- 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
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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
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
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- 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 invention relates to a method for preparing lyocell fiber by taking poplar as a raw material, which comprises the steps of taking the poplar as the raw material, sawing the poplar into wood powder, and preparing wood pulp cellulose by adopting the technical methods of sealed cooking, alkali treatment, LiCl/dimethylacetamide mixed solvent dissolution, precipitation and the like; then dissolving wood pulp cellulose in N-methylmorpholine-N-oxide to prepare spinning solution, and feeding the spinning solution into a spinning system for spinning; finally, the fiber silk is processed by the processes of alcohol washing, water washing, oiling, drying and the like to prepare the lyocell fiber. The success of extracting the cellulose from the poplar greatly reduces the production cost of the lyocell fiber; the purification process of the wood pulp cellulose and the production process of the lyocell are both green and environment-friendly, and the process is simple and has better popularization and application prospects.
Description
Technical Field
The invention belongs to the technical field of lyocell fibers, and particularly relates to a method for preparing lyocell fibers by taking poplar as a raw material.
Background
For the chemical fiber industry in China, although the yield occupies seven parts of the world, some fiber varieties with high technological content and high added value cannot be completely made in China, and particularly in the field of fibers for textiles, a plurality of gaps are still needed to be filled, such as: lyocell fibers. The lyocell fiber has the characteristics of nature, environmental protection, moisture absorption, skin friendliness, softness, luster and the like, can be compared with natural fiber, and is a fiber product favored in the fields of high-grade clothes, home textile fabrics and sanitary materials. However, for many years, the raw material of lyocell fiber has been imported for such a premium product, and the main raw material of lyocell fiber in foreign countries is trees.
In order to realize the localization of the main raw materials of the lyocell fibers, the poplar can be considered as the main raw material of the lyocell fibers by combining the actual characteristics of China. The poplar is widely distributed, the southern part and inner Mongolia of Liaoning in China in the north, the south to the Yangtze river basin, and the middle and lower reaches of the yellow river are suitable for growing; the poplar grows faster, has strong adaptability, is salt and alkali resistant, resists water and moisture of a big tree, has deep root property, developed root system, strong sprout tillering property of the rhizosphere, smoke and dust resistance and pollution resistance. In addition, the content of cellulose in the poplar is higher and can reach more than 40%. Thus, aspen wood has the potential to be the main raw material for lyocell fibers.
Disclosure of Invention
Aiming at the problems of high difficulty in purifying the raw material of the lyocell fiber and complex source of raw material varieties, the invention prepares the lyocell fiber by taking poplar as the raw material. The invention aims to overcome the defects of the prior art and provides a method for preparing lyocell fibers by taking poplar as a raw material, which comprises the following steps:
(1) preparing a spinning solution: distilling an aqueous solution of N-methylmorpholine-N-oxide (NMMO) with the mass fraction of 50-55% to an aqueous solution of NMMO with the mass fraction of 80-90%, dissolving wood pulp cellulose in the aqueous solution of NMMO, and stirring and dissolving in a reaction kettle at 105-120 ℃ in vacuum for 4-5 hours to prepare a uniform and transparent spinning solution with the mass fraction of 10-18%;
(2) spinning of lyocell fibers: adding the spinning solution treated in the step (1) into a screw extruder, further dissolving at 95-110 ℃, then filtering, and entering a spinning system, wherein the length of an air gap is 6-9 cm, the spinning speed is 35-50 m/min, the aperture of a spinneret plate is 10-110 mu m, and the length of a pore capillary is 300-900 mu m; the sprayed silk threads are vertically stretched in the air, enter a coagulating bath, and are coagulated and formed, wherein the concentration of the coagulating bath is 12-15% of the aqueous solution of NMMO, and the temperature of the coagulating bath is 2-9 ℃;
(3) alcohol washing of the fibers: immersing the fibers treated in the step (2) into 75-95% ethanol solution at room temperature for 3-4 hours at a bath ratio of 1: 30-40;
(4) and (3) water washing of the fiber: immersing the fiber treated in the step (3) into hot water at the temperature of 75-95 ℃ for 2-3 hours at a bath ratio of 1: 40-50;
(5) oiling the fibers: immersing the fibers treated in the step (4) into 3-4 g/L oil bath solution, wherein the oil bath temperature is 80-85 ℃, the time is 2-4 hours, and the bath ratio is 1: 20-30;
(6) drying the fibers: and (5) drying the fiber treated in the step (5) to obtain the lyocell fiber.
The preparation method of the wood pulp cellulose in the step (1) comprises the following steps:
step 01: sawing poplar into wood powder, putting the wood powder and water into a sealed cooking pot according to a certain ratio for cooking, wherein the ratio of the wood powder to the water is 1: 20-30;
preferably, the cooking temperature in the step 01 is 170-210 ℃, the pressure is 5-10 atm, and the treatment time is 3-5 hours; sieving the wood powder by using a 50-200 mesh sieve;
step 02: soaking the filter residue treated in the step (01) into 10-20 g/L sodium hydroxide solution at a bath ratio of 1: 20-25, at a treatment temperature of 65-80 ℃ for 2-3 hours; immersing in a sodium hypochlorite solution of 5-8 g/L, wherein the treatment temperature is 45-55 ℃, and the immersion time is 3-4 hours;
step 03: dissolving the filter residue treated in the step 02 in a mixed solvent of LiCl/dimethylacetamide, heating and stirring to dissolve the filter residue, wherein the treatment temperature is 100-105 ℃, and the immersion time is 3-4 hours; and (3) filtering the solution while the solution is hot when the solution is cooled to 40-50 ℃, dropwise adding the filtrate into an excessive stirred ice water bath, wherein the volume ratio of the ice water bath to the solution is as follows: 100-200: 1, and the precipitated substance is cellulose;
preferably, the preparation method of the LiCl/dimethylacetamide mixed solvent in the step 03 comprises the following steps: dissolving LiCl in dimethylacetamide to enable the mass fraction of LiCl to be 5-10%;
the invention has the following remarkable advantages:
(1) the invention adopts the technical methods of sealed cooking, alkali treatment, LiCl/dimethylacetamide mixed solvent dissolution and precipitation and the like to prepare the wood pulp cellulose; the method is efficient, simple, cheap and less in environmental pollution.
(2) The success of extracting the cellulose from the poplar greatly reduces the production cost of the lyocell fiber and lays a good foundation for the market popularization of the lyocell fiber.
(3) The purification process of the wood pulp cellulose and the production process of the lyocell are both green and environment-friendly, have short flow and are beneficial to popularization and application.
Drawings
FIG. 1 an electron micrograph of lyocell fibers prepared according to the present invention
Detailed Description
The examples described below illustrate the invention in detail.
Example 1
In this embodiment, a method for preparing lyocell fiber from poplar wood comprises the following steps:
(1) preparing a spinning solution: distilling an aqueous solution of NMMO with the mass fraction of 52.1% to an aqueous solution of NMMO with the mass fraction of 83.4%, dissolving 1000g of wood pulp cellulose in 8L of the aqueous solution of NMMO, and stirring and dissolving in a reaction kettle at 105-120 ℃ in vacuum for 4-5 hours to prepare a uniform and transparent spinning solution with the mass fraction of 11.11%;
the preparation method of the wood pulp cellulose in the step (1) comprises the following steps:
step 01: sawing poplar into wood powder, and sieving the wood powder by using a 50-mesh sieve; placing wood powder and water at a ratio of 1: 22 into a sealed digester, and steaming at 190 deg.C under 8atm for 4 hr;
step 02: soaking the filter residue treated in the step 01 in 15g/L sodium hydroxide solution at a bath ratio of 1: 23, at a treatment temperature of 70 ℃ for 2.5 hours; immersing in 6g/L sodium hypochlorite solution at 50 ℃ for 3.5 hours;
step 03: dissolving the filter residue treated in the step 02 in a LiCl/dimethylacetamide mixed solvent, wherein the mass fraction of LiCl in the LiCl/dimethylacetamide mixed solvent is 6%; heating and stirring to dissolve the materials, wherein the treatment temperature is 103 ℃, and the immersion time is 3.5 hours; filtering when the solution is cooled to 40 ℃, dropwise adding the filtrate into an excessive stirred ice water bath, wherein the volume ratio of the ice water bath to the solution is as follows: at a ratio of 100: 1, the precipitated substance is cellulose;
(2) spinning of lyocell fibers: adding the spinning solution treated in the step (1) into a screw extruder, further dissolving at 100 ℃, then filtering, and entering a spinning system, wherein the length of an air gap is 7cm, the spinning speed is 40m/min, the aperture of a spinneret plate is 50 mu m, and the length of a pore capillary is 400 mu m; the sprayed silk threads are vertically stretched in the air, enter a coagulating bath, and are coagulated and formed, wherein the concentration of the coagulating bath is 13% of the aqueous solution of NMMO, and the temperature of the coagulating bath is 3-5 ℃;
(3) alcohol washing of the fibers: immersing the fiber treated in the step (2) into an ethanol solution with the concentration of 80%, wherein the immersion time is 3.5 hours, the solution temperature is room temperature, and the bath ratio is 1: 35;
(4) and (3) water washing of the fiber: immersing the fiber treated in the step (3) in hot water at 90 ℃ for 2.5 hours at a bath ratio of 1: 45;
(5) oiling the fibers: immersing the fibers treated in the step (4) into 3.5g/L oil bath solution, wherein the oil bath temperature is 84 ℃, the time is 2.5 hours, and the bath ratio is 1: 25;
(6) drying the fibers: and (3) drying the fiber treated in the step (5) to obtain the lyocell fiber, wherein an electron microscope image of the lyocell fiber is shown in figure 1.
Example 2
In this embodiment, a method for preparing lyocell fiber from poplar wood comprises the following steps:
(1) preparing a spinning solution: distilling an aqueous solution of NMMO with the mass fraction of 51.7% to an aqueous solution of NMMO with the mass fraction of 88.3% under reduced pressure, dissolving 1400g of wood pulp cellulose in 8L of the aqueous solution of NMMO, and dissolving in a reaction kettle at 115 ℃ for 4 hours under vacuum stirring to prepare a uniform and transparent spinning solution with the mass fraction of 14.89%;
the preparation method of the wood pulp cellulose in the step (1) comprises the following steps:
step 01: sawing poplar into wood powder, and sieving the wood powder by using a 100-mesh sieve; placing wood powder and water at a ratio of 1: 23 into a sealed digester, steaming at 200 deg.C under 9atm for 4 hr;
step 02: soaking the filter residue treated in the step 01 in 18g/L sodium hydroxide solution at a bath ratio of 1: 22, at a treatment temperature of 70 ℃ for 2 hours; immersing in a sodium hypochlorite solution of 7g/L, wherein the treatment temperature is 52 ℃, and the immersion time is 3 hours;
step 03: dissolving the filter residue treated in the step 02 in a LiCl/dimethylacetamide mixed solvent, wherein the mass fraction of LiCl in the LiCl/dimethylacetamide mixed solvent is 6%; heating and stirring to dissolve the mixture, wherein the treatment temperature is 105 ℃, and the immersion time is 4 hours; filtering when the solution is cooled to 50 ℃, dropwise adding the filtrate into an excessive stirred ice water bath, wherein the volume ratio of the ice water bath to the solution is as follows: at a ratio of 150: 1, wherein the precipitated substance is cellulose;
(2) spinning of lyocell fibers: adding the spinning solution treated in the step (1) into a screw extruder, further dissolving at 106 ℃, then filtering, and entering a spinning system, wherein the length of an air gap is 8cm, the spinning speed is 43m/min, the aperture of a spinneret plate is 40 mu m, and the length of a pore capillary is 400 mu m; the sprayed silk threads are vertically stretched in the air, enter a coagulating bath, and are coagulated and formed, wherein the concentration of the coagulating bath is 13% of the aqueous solution of NMMO, and the temperature of the coagulating bath is 6-7 ℃;
(3) alcohol washing of the fibers: immersing the fiber treated in the step (2) into 75% ethanol solution at room temperature for 3 hours at a bath ratio of 1: 30;
(4) and (3) water washing of the fiber: immersing the fiber treated in the step (3) in hot water at 75 ℃ for 2 hours at a bath ratio of 1: 40;
(5) oiling the fibers: immersing the fibers treated in the step (4) into 3g/L oil bath solution, wherein the oil bath temperature is 80 ℃, the time is 2 hours, and the bath ratio is 1: 20;
(6) drying the fibers: and (5) drying the fiber treated in the step (5) to obtain the lyocell fiber.
Example 3
In this embodiment, a method for preparing lyocell fiber from poplar wood comprises the following steps:
(1) preparing a spinning solution: distilling the aqueous solution of NMMO with the mass fraction of 53.6% to an aqueous solution of NMMO with the mass fraction of 88.9% under reduced pressure, dissolving 1700g of wood pulp cellulose in the aqueous solution of NMMO with the mass fraction of 8L, and stirring and dissolving the solution in a reaction kettle at 120 ℃ in vacuum for 5 hours to prepare a uniform and transparent spinning solution with the mass fraction of 17.53%;
the preparation method of the wood pulp cellulose in the step (1) comprises the following steps:
step 01: sawing poplar into wood powder, and sieving the wood powder by using a 150-mesh sieve; placing wood powder and water at a ratio of 1: 30 into a sealed digester for steaming at 190 deg.C under 8atm for 4 hr;
step 02: soaking the filter residue treated in the step 01 in 18g/L sodium hydroxide solution at a bath ratio of 1: 24, at a treatment temperature of 75 ℃ for 3 hours; immersing in a sodium hypochlorite solution of 7g/L at the treatment temperature of 50 ℃ for 3 hours;
step 03: dissolving the filter residue treated in the step 02 in a LiCl/dimethylacetamide mixed solvent, wherein the mass fraction of LiCl in the LiCl/dimethylacetamide mixed solvent is 9%; heating and stirring to dissolve the mixture, wherein the treatment temperature is 105 ℃, and the immersion time is 3 hours; filtering when the solution is cooled to 48 ℃, dropwise adding the filtrate into an excessive stirred ice water bath, wherein the volume ratio of the ice water bath to the solution is as follows: at a ratio of 200: 1, wherein the precipitated substances are cellulose;
(2) spinning of lyocell fibers: adding the spinning solution treated in the step (1) into a screw extruder, further dissolving at 106 ℃, then filtering, and entering a spinning system, wherein the length of an air gap is 8cm, the spinning speed is 48m/min, the aperture of a spinneret plate is 80 mu m, and the length of a pore capillary is 800 mu m; the sprayed silk threads are vertically stretched in the air, enter a coagulating bath, and are coagulated and formed, wherein the concentration of the coagulating bath is 14% of the aqueous solution of NMMO, and the temperature of the coagulating bath is 2-3 ℃;
(3) alcohol washing of the fibers: immersing the fiber treated in the step (2) into 95% ethanol solution at room temperature for 4 hours at a bath ratio of 1: 40;
(4) and (3) water washing of the fiber: immersing the fiber treated in the step (3) in hot water at 95 ℃ for 3 hours at a bath ratio of 1: 50;
(5) oiling the fibers: immersing the fibers treated in the step (4) into 4g/L of oil bath solution, wherein the oil bath temperature is 85 ℃, the time is 4 hours, and the bath ratio is 1: 30;
(6) drying the fibers: and (5) drying the fiber treated in the step (5) to obtain the lyocell fiber.
Claims (3)
1. A method for preparing lyocell fibers by taking poplar as a raw material is characterized by comprising a preparation method of wood pulp cellulose and a preparation method of spinning solution for preparing the lyocell fibers, wherein the preparation method comprises the following steps:
preparation of a spinning solution for the preparation of lyocell fibers: distilling an aqueous solution of NMMO with the mass fraction of 50-55% under reduced pressure to an aqueous solution of NMMO with the mass fraction of 80-90%, dissolving wood pulp cellulose in the aqueous solution of NMMO, and stirring and dissolving in a reaction kettle at 105-120 ℃ in vacuum for 4-5 hours to prepare a uniform and transparent spinning solution;
the preparation method of the wood pulp cellulose comprises the following steps:
step 01: sawing poplar into wood powder, sieving the wood powder by using a 50-200 mesh screen, putting the wood powder and water into a sealed cooking pot for cooking, wherein the cooking temperature is 170-210 ℃, the pressure is 5-10 atm, and the treatment time is 3-5 hours, so as to obtain filter residue, and the ratio of the wood powder to the water is 1: 20-30;
step 02: soaking the filter residue treated in the step (01) into 10-20 g/L sodium hydroxide solution at a bath ratio of 1: 20-25, at a treatment temperature of 65-80 ℃ for 2-3 hours; immersing in a sodium hypochlorite solution of 5-8 g/L, wherein the treatment temperature is 45-55 ℃, and the immersion time is 3-4 hours;
step 03: dissolving the filter residue treated in the step 02 in a mixed solvent of LiCl/dimethylacetamide, heating and stirring to dissolve the filter residue, wherein the treatment temperature is 100-105 ℃, and the immersion time is 3-4 hours; and (3) filtering the solution while the solution is hot when the solution is cooled to 40-50 ℃, dropwise adding the filtrate into a stirred ice water bath, wherein the volume ratio of the ice water bath to the solution is as follows: and (3) 100-200: 1, wherein the precipitated substance is cellulose.
2. The method for preparing lyocell fiber from poplar as a raw material according to claim 1, wherein the method comprises the following steps: the mass fraction of the prepared uniform and transparent spinning solution is 10-18%.
3. The method for preparing lyocell fiber from poplar as a raw material according to claim 1, wherein the method comprises the following steps: the preparation method of the LiCl/dimethylacetamide mixed solvent in the step 03 comprises the following steps: LiCl is dissolved in dimethylacetamide so that the mass fraction of LiCl is 5-10%.
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| KR20130035738A (en) * | 2011-09-30 | 2013-04-09 | 코오롱인더스트리 주식회사 | Dope for spinning lyocell, method for preparing lyocell filament fiber, and lyocell filament fiber prepared therefrom |
| 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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