CN102443869B - Cellulose solution coagulation forming method - Google Patents
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Abstract
The invention discloses a cellulose solution coagulation forming method, which comprises the following steps of: (1) dissolving cellulose pulp into a mixed aqueous solution consisting of urea or thiourea, alkali metal hydroxide and water to obtain a cellulose solution; (2) curing the cellulose solution in the (1) in a non-acid first coagulation bath at the temperature of between 50 and 100 DEG C, wherein the concentrations of the urea/ thiourea and the alkali metal hydroxide are lower than those of the corresponding components in the (1); and (3) obtaining cellulose fibers by subsequent treatment. The product has drawing plasticity, and can create an advantage for improving the strength. The production process and the production equipment of the forming method are simple, the equipment and the plant are not corroded in the production process, and the production costs of urea solvent cellulose fibers, glass paper, films, sponge and related products generated by the cellulose solution are greatly reduced; and the method has high economic benefit and social environment-friendly benefit.
Description
Technical field
The present invention relates to a kind of method of cellulose solution coagulation forming, particularly the manufacturing process of urea solvent method fiber cellulose solution.
Background technology
Cellulose is the abundantest renewable polymer that nature exists, there is good biocompatibility, many good performances such as biological degradability, can be used for preparing several functions cellulose products, wherein, aqueous slkali is current extremely promising cellulose solvent system, such as NaOH/urea etc., cellulose solution moulding in acid coagulating bath afterwards.For example Chinese Patent Application No. 200710021068.8 discloses the commercial run of preparing regenerated cellulose fiber, by cellulose dissolution in solvent, fully stir, make cellulose solution, by cellulose solution through filtration, deaeration, spray silk, coagulating bath solidify, washing, drawing-off, oven dry make regenerated cellulose fiber, wherein coagulating bath is to have sulfuric acid and aqueous sodium persulfate solution.Chinese Patent Application No. 200410013389.X discloses a kind of preparation method of regenerated celulose fibre, by cellulose dissolution in 5-12wt% NaOH and 8-20wt% urea mixed aqueous solution, fully stir, make cellulose concentrated solution, adopt wet spinning process on spinning machine, spray silk and regenerate and solidify in coagulating bath, described coagulating bath is 3-25wt% aqueous sulfuric acid, 3-25wt% sulfuric acid/5-30wt% aqueous sodium persulfate solution, 3-25wt% sulfuric acid/5-30wt% ammonium sulfate solution etc.And in the method for Chinese Patent Application No. 200510018799.8 disclosed preparing regenerative cellulose fiber by two-step coagulating bath process, coagulating bath consist of 5-20wt% sulfuric acid/10-25wt% sodium sulphate mixed aqueous solution.
Above-mentioned cellulose solution all adopts chemical reaction moulding, and its forming speed is fast, but has consumed raw material sulfuric acid and NaOH, and has produced cheap not tractable sodium sulfate byproduct.The hydrogeneous sodium oxide molybdena amount of urea solvent method fiber cellulose solution is larger, if the method that does not adopt physics to be shaped, just must cause a large amount of consumption of raw material such as urea, NaOH, sulfuric acid with said method, produce a large amount of sodium sulfate byproduct, also make the recovery of urea very difficult, cause the product cost of this production technology very high, in addition environment has been affected.Aspect quality, once test is used sulfuric acid reaction to make the fiber of fibre forming have certain fragility and intensity very low, may be to cause that because the alkali of a large amount of acid and cellulose solution plays violent exothermic reaction the structure of fibrous inside and appearance is inhomogeneous, what make that the cellulose solution of the degree of polymerization very high (DP=500～600) obtains be but the fiber that intensity is very low.
Given this, special proposition the present invention.
Summary of the invention
The object of this invention is to provide a kind of method that cellulose fibre solution solidifies is shaped, first coagulating bath of the method is nonacid coagulating bath, the solvent of the first coagulating bath can recycle and reuse, and the consumption of having saved bronsted lowry acids and bases bronsted lowry has also reduced the recovery to sulfate simultaneously; And the fiber obtaining has more pliability.
For realizing goal of the invention of the present invention, a kind of method of cellulose solution coagulation forming, comprises the steps:
(1) cellulose pulp is dissolved in the mixed aqueous solution of urea or thiocarbamide, alkali metal hydroxide and water composition, obtains cellulose solution;
(2) cellulose solution that step (1) obtains solidifies in the first coagulating bath, the composition of the first described coagulating bath comprises the mixed aqueous solution of urea/sulphur urea, alkali metal hydroxide and water composition, temperature is 50～100 ℃, wherein, the concentration of urea/sulphur urea and alkali metal hydroxide all, lower than the corresponding component concentration used of step (1), does not have adding of acidic materials in the first coagulating bath;
(3) the solid-state fiber after final solidifying carries out drawing-off, cut-out, refining, oven dry, packing process and obtains cellulose fibre.
The component that coagulating bath adopts in step (2) is pure water, or NaOH and thiocarbamide/urea, but its concentration will be lower than the concentration of step (1) respective components, due to high concentration material can be freely to the principle of low concentration side's diffusion, solidify water temperature by adjusting, coagulating bath amount, coagulation bath composition, can control in cellulose solution alkali and urea (low concentration aqueous solution is herein with respect to the alkali in cellulose solution and urea concentration) free diffusing speed out in (alkali-free and urea) or low concentration aqueous solution in water, and the stabilising system of urea method cellulose solution is because the diffusive separation of alkali and urea becomes unstable, to reach solidification forming object, and coagulation bath temperature is controlled in the scope of 50～100 ℃, (described solute molecule is containing cellulose macromolecule not for solute molecule in this temperature can improve cellulose solution, it is mainly little molecular diffusion, because little molecular diffusion movement velocity is fast) toward the speed spreading in coagulating bath (speed that causes cellulose solution to be shaped), can be unlikely to again to make urea fast decoupled.In the first coagulating bath, do not have acid to participate in carrying out chemical reaction, can not produce and reclaim complexity and the sodium sulfate byproduct of market cheapness.
In coagulating bath, the mass percent concentration of urea/sulphur urea is 0～1% in step (2), preferably 0.4%.
In coagulating bath, the mass percent concentration of alkali metal hydroxide is 0～1% in step (2), preferably 0.3%.
Preferably, in step (1), the mass percent concentration of alkali metal hydroxide is 5～10%, and the mass percent concentration of urea/sulphur urea is 6～13%.
Preferably, in step (2), the concentration 0～1% of alkali metal hydroxide, the mass percent concentration of urea or thiocarbamide is 0～1%.
In method of the present invention, the component of the first coagulating bath is different from the disclosed coagulating bath of prior art, and the component of the first coagulating bath of the present invention is not containing acid.In fibre forming process, according to actual needs, can only use the present invention's the first coagulating bath, also the present invention's the first coagulating bath can be combined with and prepare required fiber with the coagulating bath of prior art.
The shaping of cellulose solution is very slow with respect to spinning speed, so just must increase the length of bath-fed tube, bath-fed tube length is longer, tow is longer in the coagulating bath time of staying, and the urea and the alkali that diffuse out are more, and fibre forming is finer and close, fibre strength is larger, and forming effect is better.
The coagulating tank of the present invention's the first coagulating bath can be slot type or bobbin formula, and coagulating bath groove depth or coagulating bath bobbin length are 600～1500mm, preferably 1000～1200mm.
In the first coagulating bath in the present invention, coagulating bath flow is to be greater than 20 times of cellulose solution volume flow; Preferably 30-40 doubly.
Preferably, in described method, between step (2), (3), also further comprise the steps:
(a) the solid-state fiber after step (2) is solidified solidifies wherein after drawing-off in the second gelation, the inorganic acid that consists of 1～10wt% concentration of described the second gelation, coagulation bath temperature is 60～100 ℃, and preferably, described inorganic acid is sulfuric acid.
That is: described method is:
(1) cellulose pulp is dissolved in the mixed aqueous solution of urea or thiocarbamide, alkali metal hydroxide and water composition, obtains cellulose solution;
(2) cellulose solution that step (1) obtains solidifies in the first coagulating bath, the composition of the first described coagulating bath comprises the mixed aqueous solution of urea/sulphur urea, alkali metal hydroxide and water composition, temperature is 50～100 ℃, wherein, the concentration of urea/sulphur urea and alkali metal hydroxide is all lower than the corresponding component concentration used of step (1);
(3) the solid-state fiber after step (2) is solidified solidifies wherein after drawing-off in the second gelation, the inorganic acid that consists of 1～10wt% concentration of described the second gelation, coagulation bath temperature is 60～100 ℃, preferably, described inorganic acid is sulfuric acid
Solid-state fiber after the second gelation solidifies carries out drawing-off, cut-out, refining, oven dry, packing process again and obtains cellulose fibre.
Preferably, in described method, between step (2), (3), also further comprise the steps
(a) the solid-state fiber after step (2) is solidified solidifies after drawing-off in the second gelation, wherein, the inorganic acid that consists of 1～10wt% concentration of described the second gelation, coagulation bath temperature is 60～100 ℃, preferably, described inorganic acid is sulfuric acid;
(b) the solid-state fiber after step (a) is solidified at least needs a drawing-off, solid-state fiber carries out drawing-off in the 3rd coagulating bath, and wherein, the 3rd described coagulating bath is that temperature is water or the water vapour of 60～100 ℃, it is preferred, and temperature is the water of 95 ℃.
That is: described method is:
(1) cellulose pulp is dissolved in the mixed aqueous solution of urea or thiocarbamide, alkali metal hydroxide and water composition, obtains cellulose solution;
(2) cellulose solution that step (1) obtains solidifies in the first coagulating bath, the composition of the first described coagulating bath comprises the mixed aqueous solution of urea/sulphur urea, alkali metal hydroxide and water composition, temperature is 50～100 ℃, wherein, the concentration of urea/sulphur urea and alkali metal hydroxide is all lower than the corresponding component concentration used of step (1);
(3) the solid-state fiber after step (2) is solidified solidifies after drawing-off in the second gelation, wherein, the inorganic acid that consists of 1～10wt% concentration of described the second gelation, coagulation bath temperature is 60～100 ℃, preferably, described inorganic acid is sulfuric acid;
(4) the solid-state fiber after step (3) is solidified at least needs a drawing-off, solid-state fiber carries out drawing-off in the 3rd coagulating bath, and wherein, the 3rd described coagulating bath is that temperature is water or the water vapour of 60～100 ℃, it is preferred, and temperature is the water of 95 ℃;
Fiber after the 3rd coagulating bath is solidified carries out drawing-off, cut-out, refining, oven dry, packing process again and obtains cellulose fibre.
In the first coagulating bath, also further comprise that trace solidifies auxiliary agent, such as AC1815 etc.
In the first coagulating bath, tow traffic direction is consistent with body lotion flow direction.
In second and third coagulating bath, tow traffic direction is consistent with body lotion flow direction.
The above-mentioned method of operation can reduce the frictional force of fiber and coagulating bath, improves fibre forming effect.In bobbin, water is mobile, both can make fibre forming complete, can take fibre bundle out of bobbin again, makes simple to operate.
Spinning bath curring time (the first coagulating bath time of staying) is 0～10s.
Use the 3rd coagulating bath serviceability temperature be the water (also can add a small amount of various auxiliary agent that function is used that improves) of 60-100 ℃ as coagulating agent, make simply smoothly the specific urea cellulose made by soloent process of quality index solution solidifies become various forms of products.
In the method for fiber solution solidification forming of the present invention, coagulating bath is to spinning head and the corrosion-free effect of other assembly, like this filament spinning component material required to reduce, thereby can reduce cost, extends spinning head service life.For making not rupture after fibre forming, from spinning head tow out, carry out-15～0% negative drawing-off; The second gelation drawing-off adopts 5%～30% positive drawing-off; The 3rd coagulating bath drawing-off adopts 5%～30% positive drawing-off.
In the second gelation, use acid solution that fibrous inside alkali is thoroughly neutralized and urea is all decomposed or washes out, thereby reach complete solidification forming object.Through the plasticizing drawing-off of the 3rd coagulating tank, the plasticity of gained fiber improves, and can improve drafting multiple, reduces fiber weakness, and fiber product is dry to be significantly improved by force with wet by force.
The outstanding beneficial effect of the present invention is as follows:
The method of cellulose solution coagulation forming of the present invention, by the double diffusion principle of physics, finds best forming temperature, cellulose solution is shaped rapid, even, stable.And traditional viscose production technology and former urea method cellulose solution shaping are to use the chemical substances such as sulfuric acid as coagulating bath, make cellulose solution generate cellulose fibre by chemical reaction, chemical reaction process has consumed NaOH and sulfuric acid, the cheap accessory substances such as a large amount of sodium sulphate are produced, make solvent be difficult to reclaim, greatly increased the cost of coagulating bath recycling and the complexity of production technology.In traditional viscose production, the consumption of NaOH is 520Kg/ ton fiber, and sulfuric acid is 720Kg/ ton fiber.Especially with the Related product project of urea solvent method fiber cellulose solution, calculate (having the coagulating bath method of sulfuric acid) by the production method that has sulfuric acid neutralization reaction solidification forming, 1.7 tons, product fiber consumption sulfuric acid per ton, 1.4 tons, consumption NaOH, is also having very large difficulty aspect urea solvent recovery.The method that coagulating bath after method solidification forming of the present invention can separate by films such as simple counter-infiltration, sodium filters is carried out purifying, enrichment, is recycled; in its process, solvent does not almost lose; meet the requirement of cleaner production and environmental protection protection; and the plasticity of gained fiber improves; can improve drafting multiple, fiber product is dry to be significantly improved by force with wet by force.
The specific embodiment
Below in conjunction with the specific embodiment to further detailed introduction of technical scheme of the present invention.
Embodiment 1
Cellulose pulp is dissolved in the mixed aqueous solution of urea, NaOH and water composition, obtain cellulose solution, the mass percent concentration of pulp is 4.96%, and the mass percent concentration of urea is 11.45%, and the mass percent concentration of NaOH is 6.61%; The cellulose solution obtaining solidifies in the first coagulating bath, and the first coagulating bath is that temperature is the pure hot water of 95 ℃, and other consists of zero.The first coagulating bath is solidified and is used rear directly discharge cellulose solution, does not recycle; After entering godet roller drawing-off, solid-state fiber after spinning machine spinning head place coagulating tank solidifies for the first time in the second gelation, solidifies again, obtain cellulose fibre through follow-up processing again, wherein, the sulfuric acid that consists of 5wt% concentration of the second gelation, coagulation bath temperature is 90 ℃, then fiber enters the 3rd coagulating bath, and the 3rd coagulating bath is that bath temperature is the high-temperature-hot-water of 62 ℃.The over dry intensity of the cellulose fibre obtaining: 1.62cN/dtex.
Embodiment 2
Cellulose pulp is dissolved in the mixed aqueous solution of urea, NaOH and water composition, obtain cellulose solution, the mass percent concentration of pulp is 4.87%, and the mass percent concentration of urea is 11.69%, and the mass percent concentration of NaOH is 6.90%; The cellulose solution obtaining solidifies in the first coagulating bath, the temperature of the first coagulating bath is 90 ℃, it is 900mm that tube length degree (the dipping bath degree of depth) is bathed in the first coagulating bath, coagulating bath flow is 35 times of cellulose solution volume flow, the mass percent concentration of urea is wherein 0.3%, and the mass percent concentration of NaOH is 0.1%; After entering godet roller drawing-off, solid-state fiber after spinning machine spinning head place coagulating tank solidifies for the first time in the second gelation, solidifies again, obtain cellulose fibre through follow-up processing again, wherein, the sulfuric acid that consists of 2wt% concentration of the second gelation, coagulation bath temperature is 98 ℃, then fiber enters the 3rd coagulating bath, and the 3rd coagulating bath is that bath temperature is the hot water of 80 ℃.The over dry intensity of the cellulose fibre obtaining: 1.65cN/dtex.
Embodiment 3
Cellulose pulp is dissolved in the mixed aqueous solution of urea, NaOH and water composition, obtain cellulose solution, the mass percent concentration of pulp is 5.03%, and the mass percent concentration of urea is 11.90%, and the mass percent concentration of NaOH is 7.10%; The cellulose solution obtaining solidifies in the first coagulating bath, the temperature of the first coagulating bath is 65 ℃, it is 700mm that tube length degree (the dipping bath degree of depth) is bathed in the first coagulating bath, coagulating bath flow is 40 times of cellulose solution volume flow, in coagulation bath composition, the mass percent concentration of urea is 0.2%, and the mass percent concentration of NaOH is 0.1%; After entering godet roller drawing-off, solid-state fiber after spinning machine spinning head place coagulating tank solidifies for the first time in the second gelation, solidifies again, obtain cellulose fibre through follow-up processing again, wherein, the sulfuric acid that consists of 10wt% concentration of the second gelation, coagulation bath temperature is 63 ℃, then fiber enters the 3rd coagulating bath, and the 3rd coagulating bath is that bath temperature is the hot water of 61 ℃.The over dry intensity of the cellulose fibre obtaining: 1.65cN/dtex.
Embodiment 4
Cellulose pulp is dissolved in the mixed aqueous solution of urea, NaOH and water composition, obtain cellulose solution, the mass percent concentration of pulp is 4.86%, and the mass percent concentration of urea is 11.93%, and the mass percent concentration of NaOH is 7.23%; The cellulose solution obtaining solidifies in the first coagulating bath.The temperature of the first coagulating bath is 95 ℃, and in coagulating bath, the mass percent concentration of urea is 0.9%, and the mass percent concentration of NaOH is 0.4%; After entering godet roller drawing-off, solid-state fiber after spinning machine spinning head place coagulating tank solidifies for the first time in the second gelation, solidifies again, obtain cellulose fibre through follow-up processing again, wherein, the sulfuric acid that consists of 3wt% concentration of the second gelation, coagulation bath temperature is 90 ℃.Then fiber enters the 3rd coagulating bath, and the 3rd coagulating bath is that bath temperature is the hot water of 90 ℃, the over dry intensity of the cellulose fibre obtaining: 1.61cN/dtex.
Embodiment 5
Cellulose pulp is dissolved in the mixed aqueous solution of urea, NaOH and water composition, obtain cellulose solution, the mass percent concentration of pulp is 4.92%, and the mass percent concentration of urea is 11.65%, and the mass percent concentration of NaOH is 7.20%; The cellulose solution obtaining solidifies in the first coagulating bath, the temperature of the first coagulating bath is 97 ℃, it is 900mm that tube length degree (the dipping bath degree of depth) is bathed in the first coagulating bath, coagulating bath flow is 30 times of cellulose solution volume flow, wherein, the mass percent concentration of urea is 0.4%, and the mass percent concentration of NaOH is 0.2%; After entering godet roller drawing-off, solid-state fiber after spinning machine spinning head place coagulating tank solidifies for the first time in the second gelation, solidifies again, obtain cellulose fibre through follow-up processing again, wherein, the sulfuric acid that consists of 6wt% concentration of the second gelation, coagulation bath temperature is 96 ℃.Then fiber enters the 3rd coagulating bath, and the 3rd coagulating bath is that bath temperature is the hot water of 65 ℃, the over dry intensity of the cellulose fibre obtaining: 1.69cN/dtex.
Embodiment 6
Cellulose pulp is dissolved in the mixed aqueous solution of urea, NaOH and water composition, obtain cellulose solution, the mass percent concentration of pulp is 4.72%, and the mass percent concentration of urea is 6.22%, and the mass percent concentration of NaOH is 10.00%; The cellulose solution obtaining solidifies in the first coagulating bath, and the coagulation bath temperature of the first coagulating bath is 50 ℃, and wherein, the mass percent concentration of urea is 0.3%, and the mass percent concentration of NaOH is 1.0%; After entering godet roller drawing-off, solid-state fiber after spinning machine spinning head place coagulating tank solidifies for the first time in the second gelation, solidifies again, obtain cellulose fibre through follow-up processing again, wherein, the sulfuric acid that consists of 6wt% concentration of the second gelation, coagulation bath temperature is 96 ℃.The over dry intensity of the cellulose fibre obtaining: 1.57cN/dtex.
Embodiment 7
Cellulose pulp is dissolved in the mixed aqueous solution of urea, NaOH and water composition, obtain cellulose solution, the mass percent concentration of pulp is 5.22%, and the mass percent concentration of urea is 13.0%, and the mass percent concentration of NaOH is 6.0%; The cellulose solution obtaining solidifies in the first coagulating bath, the coagulation bath temperature of the first coagulating bath is 80 ℃, and wherein, the mass percent concentration of urea is 0.3%, the mass percent concentration of NaOH is 1.0%, then enters drawing-off, cut-out, refining, oven dry, packing and obtain cellulose fibre.The over dry intensity of the cellulose fibre obtaining: 1.52cN/dtex.
Embodiment 8
Cellulose pulp is dissolved in the mixed aqueous solution of urea, NaOH and water composition, obtain cellulose solution, the mass percent concentration of pulp is 4.90%, and the mass percent concentration of urea is 11.50%, and the mass percent concentration of NaOH is 6.62%; The cellulose solution obtaining solidifies in the first coagulating bath, and it is 1200mm that tube length degree (the dipping bath degree of depth) is bathed in the first coagulating bath, and temperature is the pure hot water of 95 ℃, and other consists of zero, and coagulating bath flow is 40 times of cellulose solution volume flow.The first coagulating bath is solidified and is used rear directly discharge cellulose solution, does not recycle; After entering godet roller drawing-off, solid-state fiber after spinning machine spinning head place coagulating tank solidifies for the first time in the second gelation, solidifies again, obtain cellulose fibre through follow-up processing again, wherein, the sulfuric acid that consists of 5wt% concentration of the second gelation, coagulation bath temperature is 90 ℃, then fiber enters the 3rd coagulating bath, and the 3rd coagulating bath is that bath temperature is the high-temperature-hot-water of 62 ℃.The over dry intensity of the cellulose fibre obtaining: 1.70cN/dtex.
Embodiment 9
Cellulose pulp is dissolved in the mixed aqueous solution of urea, NaOH and water composition, obtain cellulose solution, the mass percent concentration of pulp is 4.70%, and the mass percent concentration of urea is 6.81%, and the mass percent concentration of NaOH is 9.80%; The cellulose solution obtaining solidifies in the first coagulating bath, it is 600mm that tube length degree (the dipping bath degree of depth) is bathed in the first coagulating bath, the coagulation bath temperature of the first coagulating bath is 50 ℃, wherein, the mass percent concentration of urea is 0.5%, the mass percent concentration of NaOH is 0.9%, and coagulating bath flow is 25 times of cellulose solution volume flow; After entering godet roller drawing-off, solid-state fiber after spinning machine spinning head place coagulating tank solidifies for the first time in the second gelation, solidifies again, obtain cellulose fibre through follow-up processing again, wherein, the sulfuric acid that consists of 6wt% concentration of the second gelation, coagulation bath temperature is 96 ℃.The over dry intensity of the cellulose fibre obtaining: 1.67cN/dtex.
Claims (12)
1. a method for cellulose solution coagulation forming, comprises the steps:
(1) cellulose pulp is dissolved in the mixed aqueous solution of urea or thiocarbamide, alkali metal hydroxide and water composition, obtains cellulose solution;
(2) cellulose solution that step (1) obtains solidifies in the first coagulating bath, the composition of the first described coagulating bath comprises the mixed aqueous solution of urea/sulphur urea, alkali metal hydroxide and water composition, temperature is 50～100 ℃, wherein, the concentration of urea/sulphur urea and alkali metal hydroxide, lower than the corresponding component concentration used of step (1), does not have adding of acidic materials in the first coagulating bath;
(3) the solid-state fiber after final solidifying carries out drawing-off, cut-out, refining, oven dry, packing process and obtains cellulose fibre,
In step (2), in coagulating bath, the mass percent concentration of urea or thiocarbamide is 0～1%, and the mass percent concentration of alkali metal hydroxide is 0～1%;
Between step (2), (3), also comprise the steps:
(a) the solid-state fiber after step (2) is solidified solidifies after drawing-off in the second gelation, wherein, the inorganic acid that consists of 1～10wt% concentration of described the second gelation, coagulation bath temperature is 60～100 ℃.
2. method according to claim 1, is characterized in that, in the middle coagulating bath of step (2), the mass percent concentration of urea or thiocarbamide is 0.4%.
3. method according to claim 1 and 2, is characterized in that, in step (2), in coagulating bath, the mass percent concentration of alkali metal hydroxide is 0.3%.
4. method according to claim 1, is characterized in that, in step (1), the mass percent concentration of alkali metal hydroxide is 5～10%, and the mass percent concentration of urea/sulphur urea is 6～13%.
5. method according to claim 1, is characterized in that, also comprises and comprising the steps: afterwards in step (a)
(b) the solid-state fiber after step (a) is solidified at least needs a drawing-off, solid-state fiber carries out drawing-off in the 3rd coagulating bath, carry out again drawing-off, go cut-out, refining, oven dry, packing process to obtain cellulose fibre, wherein, the 3rd described coagulating bath is that temperature is water or the water vapour of 60～100 ℃.
6. method according to claim 1, is characterized in that, in the first coagulating bath, tow traffic direction is consistent with body lotion flow direction.
7. method according to claim 1, is characterized in that, the pipe range that solidifies of the first coagulating bath is 600～1500mm.
8. according to the method described in claim 1 or 7, it is characterized in that, coagulating bath flow is greater than 20 times of cellulose solution volume flow.
9. method according to claim 1 or 5, is characterized in that, described inorganic acid is sulfuric acid.
10. method according to claim 5, is characterized in that, the 3rd described coagulating bath is that temperature is the water of 95 ℃.
11. methods according to claim 7, is characterized in that, the pipe range that solidifies of the first coagulating bath is 1000～1200mm.
12. methods according to claim 8, is characterized in that, coagulating bath flow is greater than 30-40 times of cellulose solution volume flow.
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| CN110577664A (en) * | 2018-06-08 | 2019-12-17 | 淮安市冰青建设工程管理有限公司 | Preparation method of cellulose foam material |
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| CN1594680A (en) * | 2004-06-29 | 2005-03-16 | 武汉大学 | Preparation method for regenerated cellulose fiber |
| CN1702201A (en) * | 2005-05-30 | 2005-11-30 | 武汉大学 | Method for preparing regenerative cellulose fiber by two-step coagulating bath process |
| CN101429682A (en) * | 2008-11-28 | 2009-05-13 | 东华大学 | Method for producing regenerated cellulose fiber by dual-bath coagulation |
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