CN113529210B - Lignin fiber for textile material and preparation method thereof - Google Patents
Lignin fiber for textile material and preparation method thereof Download PDFInfo
- Publication number
- CN113529210B CN113529210B CN202110718572.3A CN202110718572A CN113529210B CN 113529210 B CN113529210 B CN 113529210B CN 202110718572 A CN202110718572 A CN 202110718572A CN 113529210 B CN113529210 B CN 113529210B
- Authority
- CN
- China
- Prior art keywords
- lignin
- fiber
- spinning
- fibers
- preparing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 109
- 229920005610 lignin Polymers 0.000 title claims abstract description 91
- 239000000463 material Substances 0.000 title claims abstract description 37
- 239000004753 textile Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 238000009987 spinning Methods 0.000 claims abstract description 48
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000003513 alkali Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 18
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 17
- 239000012046 mixed solvent Substances 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 37
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 19
- 239000002202 Polyethylene glycol Substances 0.000 claims description 19
- 229920001223 polyethylene glycol Polymers 0.000 claims description 19
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 claims description 17
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000003999 initiator Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 14
- 230000021736 acetylation Effects 0.000 claims description 14
- 238000006640 acetylation reaction Methods 0.000 claims description 14
- 239000003153 chemical reaction reagent Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000002347 injection Methods 0.000 claims description 10
- 239000007924 injection Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 8
- 238000011282 treatment Methods 0.000 claims description 8
- 229960000583 acetic acid Drugs 0.000 claims description 7
- FXXACINHVKSMDR-UHFFFAOYSA-N acetyl bromide Chemical compound CC(Br)=O FXXACINHVKSMDR-UHFFFAOYSA-N 0.000 claims description 7
- 239000012362 glacial acetic acid Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 230000003472 neutralizing effect Effects 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000012345 acetylating agent Substances 0.000 claims description 2
- 229920000297 Rayon Polymers 0.000 abstract description 9
- 230000000397 acetylating effect Effects 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000002861 polymer material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 241000592342 Tracheophyta Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000012815 thermoplastic material Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
Images
Classifications
-
- 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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Abstract
The present invention relates to lignin fibers for textile materials and a method for their preparation. The lignin fiber can be prepared by the following method: acetylating alkali lignin to obtain acetylated alkali lignin, dissolving the acetylated alkali lignin in a mixed solvent of dimethylformamide and ethanol, and adding a prepared spinning auxiliary agent to prepare a spinning solution; and finally, carrying out electrostatic spinning on the electrostatic spinning machine, and carrying out the procedures of washing, oiling and drying to obtain the product. The dry breaking strength of the lignin fiber prepared by the method is 39-40 cN/tex, the dry breaking elongation is 11-12%, the wet breaking strength is 31-32 cN/tex, and the wet breaking elongation is 12-13%. The mechanical property of the lignin fiber prepared by the invention is superior to that of purchased viscose fiber, and the lignin fiber is a qualified fiber for textile materials and has good application prospect.
Description
Technical Field
The invention belongs to the technical field of fiber preparation, and particularly relates to a lignin fiber for textile materials and a preparation method thereof.
Background
Lignin is a complex class of organic polymers that forms an important structural material in the supporting tissues of vascular plants and some algae. Lignin is particularly important in the formation of cell walls, particularly in wood and bark, because it imparts rigidity and is not prone to decay. Chemically, lignin is a cross-linked phenolic polymer. Lignin is a degradable natural polymer material, which is the second most abundant natural resource on earth. At present, petroleum resources are greatly consumed, and the problems of serious environmental pollution and the like are caused. Therefore, researchers in various countries strive to find new materials capable of replacing petrochemical resources, and bio-based natural materials naturally become research hotspots. The lignin has the advantages of good thermal stability, no toxicity, weather resistance and the like, and the biomass-based high polymer material prepared by using the lignin is widely applied to various fields. As a highly-aromatized natural thermoplastic material, the blending of the lignin and the high polymer material can effectively improve some application properties of the material, including biodegradability, hygroscopicity, mechanical properties and the like, and can also reduce the use amount of the synthetic high polymer material, thereby reducing the cost.
The lignin fiber is organic fiber obtained by chemical treatment of natural wood, is flocculent in appearance and is white or grey white. The fiber is prepared into fibers with different lengths and thicknesses through screening, splitting, high-temperature treatment, bleaching, chemical treatment, neutralization and screening so as to meet the requirements of different application materials. The processing temperature is up to more than 250 ℃, so the fiber is a chemically very stable substance under the common condition, is not corroded by common solvents, acids and alkalis, has the excellent quality of no toxicity, no odor, no pollution and no radioactivity, does not influence the environment, is harmless to the human body, belongs to a green and environment-friendly product, and is not possessed by other mineral quality fibers. The microstructure of the fiber is strip-shaped and bent, uneven and porous, the cross part is flat, and the fiber has good toughness, dispersibility and chemical stability, strong water absorption capacity and very excellent thickening and anti-cracking performance.
The lignin fiber is widely used in the fields of asphalt roads, concrete, mortar, gypsum products, wood pulp sponge and the like, and has good effects of preventing coating cracking, improving water retention, improving production stability and construction convenience, increasing strength, enhancing adhesion to the surface and the like. The technical effects are as follows: thixotropic, protective, absorptive, carrier and filler. In pavement paving, the fiber stabilizer is lignin fiber, and cotton flocculent fiber or granular fiber is formed by factories.
Although the lignin fiber is widely used in many fields, the lignin fiber is difficult to be used as a fiber for textile materials because the lignin fiber is poorly formed when being precipitated from a solution and is difficult to be agglomerated.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a lignin fiber for textile materials and a preparation method thereof. The lignin fiber can be used for textile materials, and has the advantages of low price, reproducibility, good strength performance and the like.
The invention aims to provide a lignin fiber for textile materials, which can be prepared by the following method: acetylating alkali lignin to obtain acetylated alkali lignin, dissolving the acetylated alkali lignin in a mixed solvent of dimethylformamide and ethanol, and adding a prepared spinning auxiliary agent to prepare a spinning solution; carrying out electrostatic spinning on an electrostatic spinning machine, and carrying out the procedures of water washing, oiling and drying to obtain the product.
Another object of the present invention is to provide a method for preparing a lignin fiber for textile materials, comprising the steps of:
(1) acetylation treatment of alkali lignin: adding alkali lignin into a round-bottom flask containing an acetylation reagent, sealing, heating and stirring at 50-60 ℃ for 2-4 h, and quickly evaporating a solvent in a rotary evaporator after the reaction is finished to obtain a solid, namely the acetylated alkali lignin.
Preferably, in the step (1), the acetylating reagent consists of acetyl bromide and glacial acetic acid, and the volume ratio of the acetyl bromide to the glacial acetic acid is as follows: 1: 9-11.
Preferably, the ratio of alkali lignin (g) to acetylating agent (mL) in step (1) is: 1: 90-110.
(2) Preparing a spinning auxiliary agent: weighing allyl polyethylene glycol, allyl glycidyl ether and an ammonium persulfate initiator, dissolving the 1/2 total allyl polyethylene glycol, allyl glycidyl ether and ammonium persulfate initiator in a proper amount of deionized water, controlling the temperature to be 75-85 ℃, and stirring for 1-2 h; and then dissolving the rest 1/2 of allyl polyethylene glycol, allyl glycidyl ether and ammonium persulfate initiator in a small amount of deionized water, and then dropwise adding the solution into the mixed solution which is just stirred, wherein the dropwise adding time is controlled to be 2-3 h, after the dropwise adding is finished, preserving the heat for 2-3 h, and after the heat preservation is finished, neutralizing the solution with NaOH until the pH is = 7-8 to obtain the spinning auxiliary agent.
Preferably, the ratio of allyl polyethylene glycol (mol), allyl glycidyl ether (mol) and ammonium persulfate (g) in the step (2) is: 1: 2 to 4: 9 to 11.
Preferably, the molecular weight of the allyl polyethylene glycol in the step (2) is 500, 1000 or 2000.
(3) Preparing a spinning solution: and (3) dissolving the acetylated alkali lignin in a mixed solvent of dimethylformamide and ethanol, adding the spinning auxiliary agent prepared in the step (2), and stirring for 20-30 minutes to prepare a spinning solution.
Preferably, the volume ratio of ethanol to dimethylformamide in the mixed solvent in the step (3) is: 1: 10-20. Preferably, the volume ratio of the spinning aid in the step (3) to the mixed solvent is: 1 to 3 percent.
Preferably, the ratio of the acetylated alkali lignin (g) to the mixed solvent (mL) in the step (3) is: 1: 3-5.
(4) Preparing the silk thread: and (4) performing electrostatic spinning on the spinning solution prepared in the step (3) on an electrostatic spinning machine.
Preferably, the spinning conditions in the step (4) are as follows: the voltage is 5-10 KV, the injection speed is 3-5 mL/h, and the injection distance is 80-100 mm.
(5) And (3) water washing of the fiber: and (3) soaking the fiber treated in the step (4) into hot water at the temperature of 60-70 ℃ for washing, wherein the washing time is 1-2 minutes, and the bath ratio is 1: 10-20.
(6) Oiling the fibers: and (3) immersing the fibers treated in the step (5) into an oil bath solution of 2-3 g/L, wherein the oil bath temperature is 60-70 ℃, the time is 1-2 minutes, and the bath ratio is 1: 10-20.
(7) Drying the fibers: and (4) drying the fiber treated in the step (6) to obtain the lignin fiber for the textile material.
The invention has the following remarkable characteristics:
(1) the invention self-prepares the spinning auxiliary agent, and the addition of the auxiliary agent creates conditions for preparing spinning solution with proper viscosity.
(2) The inventor of the application unexpectedly finds that a small amount of ethanol is added into the spinning solution when the spinning solution is prepared, the addition of the ethanol provides conditions for the rapid separation of solid and liquid in the spinning process, and the problems of poor forming and high agglomeration forming difficulty when the lignin fiber is separated out from the solution are solved.
(3) The dry breaking strength of the lignin fiber prepared by the method is 39-40 cN/tex, the dry breaking elongation is 11-12%, the wet breaking strength is 31-32 cN/tex, and the wet breaking elongation is 12-13%. From the test result of mechanical property, the mechanical property of the lignin fiber is better than that of purchased viscose fiber, so that the lignin fiber prepared by the invention is a qualified fiber for textile materials.
Drawings
FIG. 1 is a schematic view of an electrospinning apparatus prepared in example 1 (1. power supply; 2. receiving shaft; 3. jet; 4. needle; 5. holder; 6. catheter; 7. polymer solution; 8. syringe; 9. propeller);
fig. 2 electron microscope image of lignin fiber a for textile material prepared in example 1.
Detailed Description
The examples described below illustrate the invention in detail.
Example 1
In this example, the lignin fiber for textile material was prepared by the following method, including the following steps:
(1) acetylation treatment of alkali lignin: adding 10g of alkali lignin into a round-bottom flask containing 1000mL of acetylation reagent, sealing, heating and stirring at 55 ℃ for 3h, and quickly evaporating the solvent to dryness in a rotary evaporator after the reaction is finished to obtain solid, namely acetylated alkali lignin; the acetylation reagent consists of 100mL of acetyl bromide and 900mL of glacial acetic acid.
(2) Preparing a spinning auxiliary agent: weighing 0.01mol of allyl polyethylene glycol with the molecular weight of 1000, 0.03mol of allyl glycidyl ether and 0.1g of ammonium persulfate initiator, dissolving the allyl polyethylene glycol, the allyl glycidyl ether and the ammonium persulfate initiator accounting for 1/2 of the total amount in 200mL of deionized water, controlling the temperature to be 80 ℃, and stirring for 1.5 h; and then dissolving the rest 1/2 of allyl polyethylene glycol, allyl glycidyl ether and ammonium persulfate initiator in 100mL of deionized water, and then dropwise adding the solution into the mixed solution which is just stirred, wherein the dropwise adding time is controlled to be 2.5h, after the dropwise adding is finished, preserving the heat for 2.5h, and after the heat preservation is finished, neutralizing the solution with NaOH until the pH is = 7-8, thus preparing the spinning auxiliary agent.
(3) Preparing a spinning solution: dissolving 10g of acetylated alkali lignin in 40mL of mixed solvent of dimethylformamide and ethanol, adding 1mL of spinning auxiliary agent prepared in the step (2), and stirring for 25 minutes to prepare spinning solution; the volume ratio of ethanol to dimethylformamide in the mixed solvent is as follows: 1: 15.
(4) Preparing the silk thread: performing electrostatic spinning on the spinning solution prepared in the step (3) on an electrostatic spinning machine, wherein the schematic diagram of the electrostatic spinning machine is shown in figure 1; the spinning conditions were: the voltage is 8KV, the injection speed is 4mL/h, and the injection distance is 90 mm.
(5) And (3) water washing of the fiber: soaking the fiber treated in the step (4) into hot water at 65 ℃ for washing, wherein the washing time is 1.5 minutes, and the bath ratio is 1: 15;
(6) oiling the fibers: immersing the fibers treated in the step (5) into an oil bath solution of 2.5g/L, wherein the oil bath temperature is 65 ℃, the time is 1.5 minutes, and the bath ratio is 1: 15;
(7) drying the fibers: and (3) drying the fibers treated in the step (6) to obtain the lignin fibers a for the textile material, wherein an electron microscope image of the lignin fibers a for the textile material is shown in fig. 2.
Example 2
In this example, the lignin fiber for textile material was prepared by the following method, including the following steps:
(1) acetylation treatment of alkali lignin: adding 10g of alkali lignin into a round-bottom flask containing 900mL of acetylation reagent, sealing, heating and stirring at 55 ℃ for 3h, and quickly evaporating the solvent to dryness in a rotary evaporator after the reaction is finished to obtain solid, namely acetylated alkali lignin; the acetylation reagent consists of 90mL of acetyl bromide and 810mL of glacial acetic acid.
(2) Preparing a spinning auxiliary agent: weighing 0.01mol of allyl polyethylene glycol with the molecular weight of 1000, 0.02mol of allyl glycidyl ether and 0.1g of ammonium persulfate initiator, dissolving the allyl polyethylene glycol, the allyl glycidyl ether and the ammonium persulfate initiator accounting for 1/2 of the total amount in 200mL of deionized water, controlling the temperature to be 80 ℃, and stirring for 1.5 h; and then dissolving the rest 1/2 of allyl polyethylene glycol, allyl glycidyl ether and ammonium persulfate initiator in 100mL of deionized water, and then dropwise adding the solution into the mixed solution which is just stirred, wherein the dropwise adding time is controlled to be 2.5h, after the dropwise adding is finished, preserving the heat for 2.5h, and after the heat preservation is finished, neutralizing the solution with NaOH until the pH is = 7-8, thus preparing the spinning auxiliary agent.
(3) Preparing a spinning solution: dissolving 10g of acetylated alkali lignin in 30mL of mixed solvent of dimethylformamide and ethanol, adding 1mL of the spinning auxiliary prepared in the step (2), and stirring for 25 minutes to prepare spinning solution; the volume ratio of ethanol to dimethylformamide in the mixed solvent is as follows: 1: 10.
(4) Preparing the silk thread: performing electrostatic spinning on the spinning solution prepared in the step (3) on an electrostatic spinning machine, wherein the schematic diagram of the electrostatic spinning machine is shown in figure 1; the spinning conditions were: the voltage is 8KV, the injection speed is 4mL/h, and the injection distance is 90 mm.
(5) And (3) water washing of the fiber: soaking the fiber treated in the step (4) into hot water at 65 ℃ for washing, wherein the washing time is 1.5 minutes, and the bath ratio is 1: 15;
(6) oiling the fibers: immersing the fibers treated in the step (5) into an oil bath solution of 2.5g/L, wherein the oil bath temperature is 65 ℃, the time is 1.5 minutes, and the bath ratio is 1: 15;
(7) drying the fibers: and (4) drying the fiber treated in the step (6) to obtain the lignin fiber b for the textile material.
Example 3
In this example, the lignin fiber for textile material was prepared by the following method, including the following steps:
(1) acetylation treatment of alkali lignin: adding 10g of alkali lignin into a round-bottom flask containing 1100mL of acetylation reagent, sealing, heating and stirring at 55 ℃ for 3h, and quickly evaporating the solvent to dryness in a rotary evaporator after the reaction is finished to obtain solid, namely acetylated alkali lignin; the acetylation reagent consists of 100mL of acetyl bromide and 1000mL of glacial acetic acid.
(2) Preparing a spinning auxiliary agent: weighing 0.01mol of allyl polyethylene glycol with the molecular weight of 1000, 0.04mol of allyl glycidyl ether and 0.1g of ammonium persulfate initiator, dissolving the allyl polyethylene glycol, the allyl glycidyl ether and the ammonium persulfate initiator accounting for 1/2 of the total amount in 200mL of deionized water, controlling the temperature to be 80 ℃, and stirring for 1.5 h; and then dissolving the rest 1/2 of allyl polyethylene glycol, allyl glycidyl ether and ammonium persulfate initiator in 100mL of deionized water, and then dropwise adding the solution into the mixed solution which is just stirred, wherein the dropwise adding time is controlled to be 2.5h, after the dropwise adding is finished, preserving the heat for 2.5h, and after the heat preservation is finished, neutralizing the solution with NaOH until the pH is = 7-8, thus preparing the spinning auxiliary agent.
(3) Preparing a spinning solution: dissolving 10g of acetylated alkali lignin in 50mL of mixed solvent of dimethylformamide and ethanol, adding 1mL of the spinning auxiliary prepared in the step (2), and stirring for 25 minutes to prepare spinning solution; the volume ratio of ethanol to dimethylformamide in the mixed solvent is as follows: 1: 20.
(4) Preparing the silk thread: performing electrostatic spinning on the spinning solution prepared in the step (3) on an electrostatic spinning machine, wherein the schematic diagram of the electrostatic spinning machine is shown in figure 1; the spinning conditions were: the voltage is 8KV, the injection speed is 4mL/h, and the injection distance is 90 mm.
(5) And (3) water washing of the fiber: soaking the fiber treated in the step (4) into hot water at 65 ℃ for washing, wherein the washing time is 1.5 minutes, and the bath ratio is 1: 15;
(6) oiling the fibers: immersing the fibers treated in the step (5) into an oil bath solution of 2.5g/L, wherein the oil bath temperature is 65 ℃, the time is 1.5 minutes, and the bath ratio is 1: 15;
(7) drying the fibers: and (4) drying the fiber treated in the step (6) to obtain the lignin fiber c for the textile material.
Comparative example 1
In the comparative example, no textile auxiliary was added during the preparation, and the specific method was not to carry out "(2) preparation of the spinning auxiliary", and "1 mL of the spinning auxiliary prepared in step (2)" was added "was deleted at the same time; other preparation methods referring to example 1, lignin fiber d for textile material was prepared.
Comparative example 2
In this comparative example, in the production process, no ethanol was added, that is, "10 g of acetylated alkali lignin was dissolved in 40mL of a mixed solvent of dimethylformamide and ethanol" was adjusted to "10 g of acetylated alkali lignin was dissolved in 40mL of a dimethylformamide solvent" other production method Lignin fiber e for textile materials was produced with reference to example 1.
And (3) performance testing:
testing the mechanical properties of the fibers: the lignin fibers a, b, c, d and e for the textile materials prepared in the above specific examples 1 to 3 and comparative examples 1 to 2 were subjected to a strength performance test, and the test method refers to GB/T-24218.3-2010 "test method for textiles and nonwovens part 3: determination of breaking strength and breaking elongation, a FAVIMAT-BOBOBOT 2 full-automatic single fiber universal tester is adopted to determine the strength performance of the test samples, no less than 30 test samples are tested, and the test average value is taken. The test results are shown in table 1, wherein the lignin fibers a, b, c, d for textile materials are abbreviated as fibers a, b, c, d, and the viscose fibers on the market are from the textile company of seoxing dan and au.
TABLE 1 mechanical Properties of the fibers a, b, c, d, e and of the viscose fibers on the market
As can be seen from Table 1, the dry breaking strength of the lignin fiber prepared in the example is between 39 and 40cN/tex, which is slightly higher than that of the viscose fiber on the procurement market, and the dry breaking elongation of the lignin fiber prepared in the example is between 11 and 12 percent, which is slightly higher than that of the viscose fiber on the procurement market; the wet breaking strength of the lignin fiber prepared in the embodiment is between 31 and 32cN/tex and is slightly higher than that of viscose fiber on the procurement market, and the wet breaking elongation of the lignin fiber prepared in the embodiment is between 12 and 13 percent and is slightly higher than that of the viscose fiber on the procurement market. The primary performance parameters of the lignin fibers prepared in the comparative examples were lower than those of the lignin fibers prepared in the examples. The results of the examples and comparative examples can be considered as: the addition of the textile auxiliary agent and the doping of the ethanol solvent have important influence on the performance of the lignin fiber. From the test result of mechanical property, the mechanical property of the lignin fiber is superior to that of purchased viscose fiber, so that the lignin fiber prepared by the method is qualified.
Claims (6)
1. A method for preparing lignin fibers for textile materials, characterized in that said method comprises the steps of:
(1) acetylation treatment of alkali lignin: adding alkali lignin into a round-bottom flask containing an acetylation reagent, sealing, heating and stirring at 50-60 ℃ for 2-4 h, and quickly evaporating a solvent to dryness in a rotary evaporator after the reaction is finished to obtain solid, namely acetylated alkali lignin;
(2) preparing a spinning auxiliary agent: weighing allyl polyethylene glycol, allyl glycidyl ether and an ammonium persulfate initiator, dissolving the 1/2 total allyl polyethylene glycol, allyl glycidyl ether and ammonium persulfate initiator in a proper amount of deionized water, controlling the temperature to be 75-85 ℃, and stirring for 1-2 h; then dissolving the rest 1/2 allyl polyethylene glycol, allyl glycidyl ether and ammonium persulfate initiator in a small amount of deionized water, and then dropwise adding the solution into the mixed solution which is just stirred, wherein the dropwise adding time is controlled to be 2-3 h, after the dropwise adding is finished, preserving the heat for 2-3 h, and after the heat preservation is finished, neutralizing the solution with NaOH until the pH is = 7-8 to obtain the spinning auxiliary agent;
(3) preparing a spinning solution: dissolving acetylated alkali lignin in a mixed solvent of dimethylformamide and ethanol, adding the spinning auxiliary prepared in the step (2), and stirring for 20-30 minutes to prepare a spinning solution;
(4) preparing the silk thread: performing electrostatic spinning on the spinning solution prepared in the step (3) on an electrostatic spinning machine;
(5) and (3) water washing of the fiber: soaking the fiber treated in the step (4) into hot water at the temperature of 60-70 ℃ for washing, wherein the washing time is 1-2 minutes, and the bath ratio is 1: 10-20;
(6) oiling the fibers: immersing the fibers treated in the step (5) into an oil bath solution of 2-3 g/L, wherein the oil bath temperature is 60-70 ℃, the time is 1-2 minutes, and the bath ratio is 1: 10-20;
(7) drying the fibers: and (4) drying the fiber treated in the step (6) to obtain the lignin fiber for the textile material.
2. The method of preparing lignin fibers for textile materials according to claim 1, wherein: the acetylation reagent in the step (1) consists of acetyl bromide and glacial acetic acid, and the volume ratio of the acetyl bromide to the glacial acetic acid is as follows: 1: 9-11; the ratio of alkali lignin to acetylating agent is: 1g to (90-110) mL.
3. The method of preparing lignin fibers for textile materials according to claim 1, wherein: in the step (2), the dosage ratio of allyl polyethylene glycol, allyl glycidyl ether and ammonium persulfate is as follows: 1mol, (2-4) mol, (9-11) g; the molecular weight of allyl polyethylene glycol is 500, 1000 or 2000.
4. The method of preparing lignin fibers for textile materials according to claim 1, wherein: the volume ratio of ethanol to dimethylformamide in the mixed solvent in the step (3) is as follows: 1: 10-20; the volume ratio of the spinning auxiliary agent to the mixed solvent is as follows: 1-3%; the ratio of acetylated alkali lignin to mixed solvent was: 1g to (3-5) mL.
5. The method of preparing lignin fibers for textile materials according to claim 1, wherein: the spinning conditions in the step (4) are as follows: the voltage is 5-10 KV, the injection speed is 3-5 mL/h, and the injection distance is 80-100 mm.
6. A lignin fiber for textile materials, characterized by being produced by the method for producing a lignin fiber for textile materials according to any one of claims 1 to 5.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110718572.3A CN113529210B (en) | 2021-06-28 | 2021-06-28 | Lignin fiber for textile material and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110718572.3A CN113529210B (en) | 2021-06-28 | 2021-06-28 | Lignin fiber for textile material and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN113529210A CN113529210A (en) | 2021-10-22 |
CN113529210B true CN113529210B (en) | 2022-04-26 |
Family
ID=78096968
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110718572.3A Active CN113529210B (en) | 2021-06-28 | 2021-06-28 | Lignin fiber for textile material and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN113529210B (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113930967B (en) * | 2021-11-15 | 2023-04-07 | 武汉纺织大学 | Lignin-containing composite emulsion for sun-blocking clothes and preparation method and application thereof |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104120507A (en) * | 2014-07-22 | 2014-10-29 | 南京工业大学 | Preparation method of lignin-based electrostatic blended materials |
CN105002583A (en) * | 2015-06-23 | 2015-10-28 | 北京林业大学 | Preparation method for wood acetate fiber nanometer precursor |
CN109137139A (en) * | 2018-07-27 | 2019-01-04 | 北京林业大学 | A kind of preparation method of lignin-base fiber |
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 |
-
2021
- 2021-06-28 CN CN202110718572.3A patent/CN113529210B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104120507A (en) * | 2014-07-22 | 2014-10-29 | 南京工业大学 | Preparation method of lignin-based electrostatic blended materials |
CN105002583A (en) * | 2015-06-23 | 2015-10-28 | 北京林业大学 | Preparation method for wood acetate fiber nanometer precursor |
CN109137139A (en) * | 2018-07-27 | 2019-01-04 | 北京林业大学 | A kind of preparation method of lignin-base fiber |
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 |
Non-Patent Citations (1)
Title |
---|
乙酰化处理对碱木质素在四氢呋喃中微结构的影响;李浩等;《物理化学学报》;20150115(第01期);128-136 * |
Also Published As
Publication number | Publication date |
---|---|
CN113529210A (en) | 2021-10-22 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US3897206A (en) | Method of preparing cellulosic textile materials having improved soil release and stain resistance properties | |
CN101435119B (en) | Preparation of modified polyacrylonitrile fibre | |
CN100393935C (en) | High water-absorption fiber and its preparing method | |
CN113529210B (en) | Lignin fiber for textile material and preparation method thereof | |
CN104630923A (en) | Method for preparing carbon nano tube modified polyacrylonitrile fibers with solution in-situ polymerization technology | |
US4038027A (en) | Cellulosic textile materials having improved soil release and stain resistance properties | |
CN111334880B (en) | Photochromic lyocell fibers and method for making same | |
CN106633049A (en) | Vat dye ozone-proof fastness improver as well as preparation method and application thereof | |
CN106591993B (en) | A kind of gelatin fiber spinning process | |
CN102691211B (en) | Water-soluble sizing agent used for carbon fiber and preparation method thereof | |
CN108822258B (en) | Preparation method and application of modified carboxymethyl cellulose | |
CN103030700A (en) | Compound modified starch and preparation method and application thereof | |
CN110903606B (en) | Plant oil-based composite material and preparation method thereof | |
CN108998857A (en) | A kind of preparation method of anti-corrosion and high strength tencel | |
CN110230212B (en) | Polyester textile dyeing method | |
CN105544193B (en) | The hydrophilic modification method of a kind of bromoethane and PVA to polyester fiber | |
CN104451930A (en) | Preparation method of whisker-reinforced regenerative cellulose fiber | |
CN108866674A (en) | A kind of nanometer oil suction fibre of high oil absorption amount and preparation method thereof | |
CN111394828A (en) | Spinning method of polyacrylonitrile fiber | |
CN110606911A (en) | Water-based sizing agent for all-cotton spinning and preparation method thereof | |
CN110820321A (en) | Polyester fiber finishing agent, preparation method and fiber finishing method | |
CN108977930A (en) | A kind of high strength acid resistant alkali tencel | |
CN109161982A (en) | A kind of textile fabric of high strength acid resistant caustic corrosion | |
CN1142952C (en) | Polyacrylonitrile polymer treatment | |
CN111005090B (en) | Preparation method of chitosan/gallnut tannin composite fiber |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
TR01 | Transfer of patent right | ||
TR01 | Transfer of patent right |
Effective date of registration: 20240117 Address after: 230000 floor 1, building 2, phase I, e-commerce Park, Jinggang Road, Shushan Economic Development Zone, Hefei City, Anhui Province Patentee after: Dragon totem Technology (Hefei) Co.,Ltd. Address before: 430074 No. 1 Textile Road, Hongshan District, Hubei, Wuhan Patentee before: Wuhan Textile University |