CN102926015A - Method for preparing hydroxyethyl cellulose fibers by adopting pre-gel method - Google Patents
Method for preparing hydroxyethyl cellulose fibers by adopting pre-gel method Download PDFInfo
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Abstract
The invention discloses a method for preparing hydroxyethyl cellulose fibers by adopting pre-gel method. The method comprises the following steps: dissolving hydroxyethyl celluloses with low degree of substitution in uniform mixed aqueous solution containing 4-12 wt% of sodium hydroxide, 1-10 wt% of thiourea and 1-15 wt% of urea at negative 15 to 10 degrees centigrade, filtering and defoaming to obtain spinning solution with solid content of 2-20%; making the spinning solution stand at negative 5-0 degrees centigrade for 10-30 min to perform pre-gel treatment, then spinning by a wet spinning machine, solidifying, regenerating and performing stretching orientation to obtain the hydroxyethyl cellulose fibers. The method performs the pre-gel treatment to the spinning solution, part of molecular chains of the solution are wound with each other at low temperature, and a light cross-linking network structure still exists when the temperature is increased to the spinning temperature so as to effectively reduce swelling of silks generated in the washing process and increase spinning property and spinning speed of the spinning solution. Therefore, the obtained novel fibers have the advantages of compact structure and excellent mechanical property.
Description
Technical field
The present invention relates to a kind of method that adopts pre-gel to prepare hydroxyethyl cellulose, belong to the material technology field.
Background technology
Cellulose is the abundantest renewable resource of occurring in nature, is the widest natural carbohydrate that distributes at present, and whole world annual production is about 150,000,000,000 tons.Its source mainly comprises cotton, fiber crops, timber, bamboo, and other higher plants, such as reed, stalk, bagasse etc.At present, cellulose is mainly for the production of regrown material (fiber, film etc.) and processing synthetic cellulose derivative.And the advantage such as day by day in short supply current of cotton resource, wearability is similar to cotton because having for regenerated celulose fibre, environmental friendliness and raw material (cellulose) are renewable has caused people's great attention.But because in the crystal structure of cellulose densification and the complicated molecule thereof and intermolecular hydrogen bonding, make it be difficult to be dissolved in the common solvent or carry out melt-processed, directly hindered development and the application of material of regenerated cellulose.Present most regenerated celulose fibre still adopts traditional viscose process production, but this technique discharges a large amount of poisonous H in process of production
2S and CS
2, in serious environment pollution, also damaged health.Current, many scholars are doing a large amount of work aspect the exploitation cellulose solvent, and have found many cellulosic novel dissolvents, such as LiCl/DMAc, NH
3/ NH
4The SCN aqueous solution, PF/DMSO, Ca (SCN)
2/ NaSCN the aqueous solution, ZnCl
2The aqueous solution, ionic liquid system etc., but these solvents are owing to the shortcomings such as solvent is expensive, recovery is difficult, dissolution conditions is harsh can't realize industrialization so far.The advantages such as alkali/urea solvent is because having low price, and toxicity is lower, and directly dissolving cellulos generates without derivative, and the rare degraded of cellulose is dissolved rapidly, and technique is simple have good application prospect aspect the traditional adhering process of replacement.Professor Zhang Lina of Wuhan University adopts NaOH and urea mixed aqueous solution, NaOH and thiocarbamide mixed aqueous solution dissolving cellulos and successfully prepares regenerated cellulose film and fiber, but because dissolution with solvents is limited in one's ability, be only applicable to the not high cellulose of the degree of polymerization, the solid content of solution is lower, causes the material of regenerated cellulose mechanical property for preparing relatively poor.Donghua University turns round and look at sharp rosy clouds etc. take NaOH, thiocarbamide, urea mixed aqueous solution as solvent, cellulose had stronger solvability, and successfully make regenerated cellulose film and fiber, but do not solve equally the problems such as cellulosic degree of polymerization and solid content be on the low side, gained regrown material mechanical property still has to be hoisted.Simultaneously, use the cellulose solution character of alkali/urea solvent preparation unstable, easily form irreversible gel, for follow-up spinning process has increased difficulty, be unfavorable for suitability for industrialized production.
It is etherification modified to utilize oxirane that cellulose is carried out, and can make the hydroxyethylcellulose of low molar substitution, strengthens solvent molecule to the accessibility of hydroxyl by hydrogen bond action between the reduction cellulose macromolecule, can realize improving the purpose of solution solid content.The hydroxyethylcellulose of low molar substitution has unique alkali solubility, and solution has good film forming, fibre forming property.NaOH described in the patent CN101412815A, thiocarbamide, urea mixed aqueous solution, hydroxyethylcellulose had stronger solvability, can obtain the hydroxy ethyl fiber cellulose solution of high-dissolvability (solubility can reach 100%), high solids content, and solution property is stable, modest viscosity, strainability are good, the gel heat that forms is reversible, is with a wide range of applications.But when being applied to wet spinning, the strand water-washing process easily produces swollen, affects the stability of spinning process, has reduced spinning speed, is unfavorable for the industrialization steady production.
Summary of the invention
The purpose of this invention is to provide a kind of method that adopts pre-gel to prepare hydroxyethyl cellulose, the problem such as the spinnability that excessive swollen causes when washing because of strand to solve in the existing spinning technique is poor.
For achieving the above object, the invention provides a kind of method that adopts pre-gel to prepare hydroxyethyl cellulose, it is characterized in that concrete steps are as follows:
1): preparation contains 4～12wt% NaOH by weight percentage, 1～10wt% thiocarbamide, and the aqueous solution of 1～15wt% urea (being alkali/urea solvent), and be chilled in advance-15～10 ℃; With the degree of polymerization be 300～2000, to be 0.15～0.85 hydroxyethylcellulose mixed with the alkali of precooling/urea solvent molar substitution in 5: 95 in mass ratio～20: 80, under-10～20 ℃, stir, until dissolve the hydroxy ethyl fiber cellulose solution that forms homogeneous transparent fully;
2): filtration step 1) the hydroxy ethyl fiber cellulose solution of gained, at room temperature utilize supercentrifuge to the centrifugal 10-60min of filtrate, slough bubble;
3) the centrifugal rear spinning solution that: with step 2) obtains leaves standstill 10～30min and carries out the pregel processing under-5～0 ℃, then be warming up to 25 ℃; Spinning solution is transferred to vacuum defoamation 30～200min in the spinning machine;
4): with nitrogen spinning solution is pressurizeed, make it by metering pump of spinning machine, gooseneck and spinneret cap, enter and be solidified into strand in the coagulating bath;
5): solidify strand after the drawing-off through the twice water-bath washing, then enter with in the baking oven of coiler device in 50～80 ℃ lower dry, at last by winder winding around obtaining white, softness, glossiness fiber.
Preferably, the coagulating bath described step 4) is mixed aqueous solution or 3～15wt% aqueous hydrochloric acid solution of aqueous acetic acid, 3～25wt% sulfuric acid and the 3～25wt% sodium sulphate of 8～25wt%; Coagulation bath temperature is controlled at 10～30 ℃.
The present invention places certain hour at low temperatures with spinning solution, carries out pregel and processes.Because intermolecular distance reduces under the low temperature, cellulose macromolecule is easily assembled, the part molecular entanglement, when rising to spinning temperature, solution temperature still has certain gel degree, there is lightly crosslinked network structure, spinning solution viscosity rise 5%～15%, but still have flowability; This solution is extruded by spinning head, can effectively be reduced the swollen that strand produces in water-washing process, improve spinnability and the spinning speed of spinning solution, the fibre structure that makes is fine and close, good mechanical performance.The method is simple to operate, and cost is low, and is environmentally friendly, is fit to suitability for industrialized production.The present invention can effectively reduce the swollen that strand produces in water-washing process, improve spinnability and the spinning speed of spinning solution, and the cellulosic fibrous structure that obtains is fine and close, and good mechanical performance has higher TENSILE STRENGTH.
Compared with prior art, the advantage that has of the present invention is as follows:
The low degree of substitution hydroxy ethyl fiber cellulose solution of the high solids content that (1) the present invention relates to, by carrying out etherification modified to cellulose, the solvability of the etherification product that obtains in alkali solvent especially alkali/urea solvent significantly improves, prepared solution has higher solid content, better stability and better strainability, and the gel heat that solution forms is reversible, has a extensive future.
(2) the present invention adopts pre-gel to make the hydroxyethylcellulose spinning solution of high solids content form slight cross-linked structure, reaches in advance certain gel degree, but still has flowability.But the spinnability of the method Effective Raise spinning solution reduces the run-inflation effect that strand produces in water-washing process, the Effective Raise spinning speed, and the fibre structure that obtains after the spinning is fine and close, good mechanical performance.And the method is simple to operate, and cost is low, and is environmentally friendly, is fit to suitability for industrialized production.
(3) regenerated celulose fibre that makes of the present invention, cross section are circular, have than big difference with existing viscose.Its fibre structure is finer and close, and degree of crystallinity is higher, and mechanical property is better.
The specific embodiment
For the present invention is become apparent, hereby with preferred embodiment, be described in detail below.
Embodiment 1
(1) be that the even mixed aqueous solution of 8wt% NaOH, 6.5wt% thiocarbamide, 8wt% urea is chilled to-5 ℃ in advance with the 455g component, add the 45g degree of polymerization and be 1000, molar substitution is 0.31 hydroxyethylcellulose, at 0～5 ℃ of lower 2h that stirs, hydroxyethylcellulose dissolves the solution that forms homogeneous transparent fully.
(2) filter gained hydroxy ethyl fiber cellulose solution, utilize supercentrifuge to the centrifugal 10min of filtrate under the room temperature, slough bubble.
(3) centrifugal rear spinning solution is left standstill 10min under 0 ℃ and carry out the pregel processing, then be warming up to 25 ℃, spinning solution viscosity rise 5%, solution reach certain gel degree, produce lightly crosslinked structure, but still have flowability; Spinning solution is transferred to vacuum defoamation 60min in the spinning machine.
(4) utilize nitrogen that spinning solution is forced into 0.1Mpa, making it by metering pump of spinning machine, gooseneck and aperture, 24 hole is the spinneret cap of 0.1mm, enter long for being solidified into strand in the first coagulating tank of 100cm, and by the first drawing roller of adjustable speed strand is carried out preliminary draft at first coagulating tank tail end, employed coagulating bath is the mixed aqueous solution of 12wt% sulfuric acid and 10wt% sodium sulphate, coagulation bath temperature is 20 ℃, and the first drawing roller is 80% to the preliminary draft ratio of strand.
(5) then strand enters with carry out drying in the baking oven of coiler device under 70 ℃ through the twice water-bath washings after the drawing-off, at last by winder winding around regenerated celulose fibre.
This fiber is white, and is soft glossy.According to ASTM D2256-80, the intensity that is recorded regenerated celulose fibre of the present invention by the electronics strength tester is 2.49cN/dtex, and the spinning solution of not processing through pregel under the same terms is 1.71cN/dtex through solidifying the fibre strength that obtains after the drawing-off.
Embodiment 2
(1) be that the even mixed aqueous solution of 6wt% NaOH, 4wt% thiocarbamide, 1wt% urea is chilled to-10 ℃ in advance with the 450g component, add the 50g degree of polymerization and be 1200, molar substitution is 0.49 hydroxyethylcellulose, at-5～0 ℃ of lower 2h that stirs, hydroxyethylcellulose dissolves the solution that forms homogeneous transparent fully.
(2) filter gained hydroxy ethyl fiber cellulose solution, utilize supercentrifuge to the centrifugal 30min of filtrate under the room temperature, slough bubble.
(3) centrifugal rear spinning solution is left standstill 30min under 0 ℃ and carry out the pregel processing, then be warming up to 25 ℃, spinning solution viscosity rise 7%, solution reach certain gel degree, produce lightly crosslinked structure, but still have flowability; Spinning solution is transferred to vacuum defoamation 90min in the spinning machine.
(4) utilize nitrogen that spinning solution is forced into 0.1Mpa, making it by metering pump of spinning machine, gooseneck and aperture, 24 hole is the spinneret cap of 0.08mm, enter long for being solidified into strand in the first coagulating tank of 100cm, and by the first drawing roller of adjustable speed strand is carried out preliminary draft at first coagulating tank tail end, employed coagulating bath is the mixed aqueous solution of 15wt% sulfuric acid and 10wt% sodium sulphate, coagulation bath temperature is 25 ℃, and the first drawing roller is 110% to the preliminary draft ratio of strand.
(5) then strand enters with carry out drying in the baking oven of coiler device under 60 ℃ through the twice water-bath washings after the drawing-off, at last by winder winding around regenerated celulose fibre.
This fiber is white, and is soft glossy.According to ASTM D2256-80, the intensity that is recorded regenerated celulose fibre of the present invention by the electronics strength tester is 2.32cN/dtex, and the spinning solution of not processing through pregel under the same terms is 1.57cN/dtex through solidifying the fibre strength that obtains after the drawing-off.
Embodiment 3
(1) be that the even mixed aqueous solution of 9wt% NaOH, 1wt% thiocarbamide, 4wt% urea is chilled to 0 ℃ in advance with the 440g component, add the 60g degree of polymerization and be 800, molar substitution is 0.51 hydroxyethylcellulose, at-2～0 ℃ of lower 2h that stirs, hydroxyethylcellulose dissolves the solution that forms homogeneous transparent fully.
(2) filter gained hydroxy ethyl fiber cellulose solution, utilize supercentrifuge to the centrifugal 60min of filtrate under the room temperature, slough bubble.
(3) centrifugal rear spinning solution is left standstill 10min under-5 ℃ and carry out the pregel processing, then be warming up to 25 ℃, spinning solution viscosity rise 8%, solution reach certain gel degree, produce lightly crosslinked structure, but still have flowability; Spinning solution is transferred to vacuum defoamation 100min in the spinning machine.
(4) utilize nitrogen that spinning solution is forced into 0.1Mpa, making it by metering pump of spinning machine, gooseneck and aperture, 30 hole is the spinneret cap of 0.1mm, enter long for being solidified into strand in the first coagulating tank of 100cm, and by the first drawing roller of adjustable speed strand is carried out preliminary draft at first coagulating tank tail end, employed coagulating bath is the 15wt% acetum, coagulation bath temperature is 10 ℃, and the first drawing roller is 90% to the preliminary draft ratio of strand.
(5) then strand enters with carry out drying in the baking oven of coiler device under 80 ℃ through the twice water-bath washings after the drawing-off, at last by winder winding around regenerated celulose fibre.
This fiber is white, and is soft glossy.According to ASTM D2256-80, the intensity that is recorded regenerated celulose fibre of the present invention by the electronics strength tester is 2.18cN/dtex, and the spinning solution of not processing through pregel under the same terms is 1.26cN/dtex through solidifying the fibre strength that obtains after the drawing-off.
Embodiment 4
(1) be that the even mixed aqueous solution of 9wt% NaOH, 4wt% thiocarbamide, 8wt% urea is chilled to 0 ℃ in advance with the 460g component, add the 40g degree of polymerization and be 1400, molar substitution is 0.34 hydroxyethylcellulose, at-5～0 ℃ of lower 2h that stirs, hydroxyethylcellulose dissolves the solution that forms homogeneous transparent fully.
(2) filter gained hydroxy ethyl fiber cellulose solution, utilize supercentrifuge to the centrifugal 20min of filtrate under the room temperature, slough bubble.
(3) centrifugal rear spinning solution is left standstill 30min under-5 ℃ and carry out the pregel processing, then be warming up to 25 ℃, spinning solution viscosity rise 15%, solution reach certain gel degree, produce lightly crosslinked structure, but still have flowability; Spinning solution is transferred to vacuum defoamation 120min in the spinning machine.
(4) utilize nitrogen that spinning solution is forced into 0.1Mpa, making it by metering pump of spinning machine, gooseneck and aperture, 12 hole is the spinneret cap of 0.1mm, enter long for being solidified into strand in the first coagulating tank of 100cm, and by the first drawing roller of adjustable speed strand is carried out preliminary draft at first coagulating tank tail end, employed coagulating bath is the 15wt% hydrochloric acid solution, coagulation bath temperature is 15 ℃, and the first drawing roller is 90% to the preliminary draft ratio of strand.
(5) then strand enters with carry out drying in the baking oven of coiler device under 80 ℃ through the twice water-bath washings after the drawing-off, at last by winder winding around regenerated celulose fibre.
This fiber is white, and is soft glossy.According to ASTM D2256-80, the intensity that is recorded regenerated celulose fibre of the present invention by the electronics strength tester is 2.58cN/dtex, and the spinning solution of not processing through pregel under the same terms is 1.77cN/dtex through solidifying the fibre strength that obtains after the drawing-off.
Embodiment 5
(1) be that the even mixed aqueous solution of 9wt% NaOH, 4wt% thiocarbamide, 8wt% urea is chilled to 0 ℃ in advance with the 470g component, add the 30g degree of polymerization and be 600, molar substitution is 0.41 hydroxyethylcellulose, at-5～0 ℃ of lower 2h that stirs, hydroxyethylcellulose dissolves the solution that forms homogeneous transparent fully.
(2) filter gained hydroxy ethyl fiber cellulose solution, utilize supercentrifuge to the centrifugal 50min of filtrate under the room temperature, slough bubble.
(3) centrifugal rear spinning solution is left standstill 20min under 0 ℃ and carry out the pregel processing, then be warming up to 25 ℃, spinning solution viscosity rise 6%, solution reach certain gel degree, produce lightly crosslinked structure, but still have flowability; Spinning solution is transferred to vacuum defoamation 200min in the spinning machine.
(4) utilize nitrogen that spinning solution is forced into 0.1Mpa, making it by metering pump of spinning machine, gooseneck and aperture, 24 hole is the spinneret cap of 0.1mm, enter long for being solidified into strand in the first coagulating tank of 100cm, and by the first drawing roller of adjustable speed strand is carried out preliminary draft at first coagulating tank tail end, employed coagulating bath is the 15wt% hydrochloric acid solution, coagulation bath temperature is 20 ℃, and the first drawing roller is 90% to the preliminary draft ratio of strand.
(5) then strand enters with carry out drying in the baking oven of coiler device under 80 ℃ through the twice water-bath washings after the drawing-off, at last by winder winding around regenerated celulose fibre.
This fiber is white, and is soft glossy.According to ASTM D2256-80, the intensity that is recorded regenerated celulose fibre of the present invention by the electronics strength tester is 1.88cN/dtex, and the spinning solution of not processing through pregel under the same terms is 1.16cN/dtex through solidifying the fibre strength that obtains after the drawing-off.
Claims (2)
1. method that adopts pre-gel to prepare hydroxyethyl cellulose is characterized in that concrete steps are as follows:
1): preparation contains 4～12wt% NaOH by weight percentage, 1～10wt% thiocarbamide, and the aqueous solution of 1～15wt% urea (being alkali/urea solvent), and be chilled in advance-15～10 ℃; With the degree of polymerization be 300～2000, to be 0.15～0.85 hydroxyethylcellulose mixed with the alkali of precooling/urea solvent molar substitution in 5: 95 in mass ratio～20: 80, under-10～20 ℃, stir, until dissolve the hydroxy ethyl fiber cellulose solution that forms homogeneous transparent fully;
2): filtration step 1) the hydroxy ethyl fiber cellulose solution of gained, at room temperature utilize supercentrifuge to the centrifugal 10-60min of filtrate, slough bubble;
3) the centrifugal rear spinning solution that: with step 2) obtains leaves standstill 10～30min and carries out the pregel processing under-5～0 ℃, then be warming up to 25 ℃; Spinning solution is transferred to vacuum defoamation 30～200min in the spinning machine;
4): with nitrogen spinning solution is pressurizeed, make it by metering pump of spinning machine, gooseneck and spinneret cap, enter and be solidified into strand in the coagulating bath;
5): solidify strand after the drawing-off through the twice water-bath washing, then enter with in the baking oven of coiler device in 50～80 ℃ lower dry, at last by winder winding around obtaining white, softness, glossiness fiber.
2. a kind of method that adopts pre-gel to prepare hydroxyethyl cellulose according to claim 1, it is characterized in that described step 4) in coagulating bath be mixed aqueous solution or 3～15wt% aqueous hydrochloric acid solution of aqueous acetic acid, 3～25wt% sulfuric acid and the 3～25wt% sodium sulphate of 8～25wt%; Coagulation bath temperature is controlled at 10～30 ℃.
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| CN105350313A (en) * | 2015-12-24 | 2016-02-24 | 西南大学 | Anti-itching finishing method adopting sodium hydroxide/urea water system for ramie fabric |
| CN105926063A (en) * | 2016-05-23 | 2016-09-07 | 东华大学 | Macro fiber based on bacterial cellulose nanofiber directional arrangement and preparing method thereof |
| CN109610024A (en) * | 2018-11-20 | 2019-04-12 | 华南理工大学 | A kind of cellulose-molybdenum disulfide aeroge composite fibre and its preparation method and application |
| CN114605664A (en) * | 2020-12-17 | 2022-06-10 | 赣南师范大学 | Hydrogel and preparation method thereof |
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