CN104480558A - Preparation method for regenerated cellulose fibers capable of dyeing without salt - Google Patents
Preparation method for regenerated cellulose fibers capable of dyeing without salt Download PDFInfo
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- CN104480558A CN104480558A CN201410718210.4A CN201410718210A CN104480558A CN 104480558 A CN104480558 A CN 104480558A CN 201410718210 A CN201410718210 A CN 201410718210A CN 104480558 A CN104480558 A CN 104480558A
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Abstract
The invention relates to a raw material for the textile industry and a manufacturing method thereof, and particularly relates to a preparation method for regenerated cellulose fibers capable of dyeing without salt. The preparation method comprises the following steps: in the preparation process of the regenerated cellulose fibers, carrying out mixing before spinning or carrying out an injection technology during the spinning, mixing with a spinning solution, and spinning to prepare the regenerated cellulose fiber, and adding a crosslinking agent in the process to enable cationic starch and a cellulose macromolecular chain to generate crosslinking reaction and enable the cationic starch to be fixed on the cellulose macromolecular chain. The prepared regenerated cellulose fibers contain a great amount of cationic groups and have the relatively good absorbing effect for a dye base body with negative charges; in the dyeing process, electrolyte does not need to be added for accelerating dyeing, so that the production cost is reduced, energy is saved and simultaneously the pollution to the environment due to use of excessive inorganic salts is also reduced.
Description
Technical field
The present invention relates to textile industry raw material and manufacture method thereof, particularly a kind of can the preparation method of regenerated celulose fibre of salt-free dyeing.
Background technology
Starch is that the one stored in vegetable kingdom gathers polysaccharose substance, and it is generally that 1-10 micron or larger particulate form exist with diameter, and these particle major sedimentary are in the seed of plant, stem tuber or root.Although starch source spreads all over whole plant world, only have a few crop to be widely used in the production of commodity starch, corn is the main source of producing starch, and other also has wheat, potato, cassava and sweet potato etc.Be a kind of high glycan from structure starch, the basic ring mainly remaining base with glucose is formed by connecting by α-D-(1 → 4) key.
Cationic starch carries out etherification reaction with the various organic amine compound containing halogen or epoxy radicals with the hydroxyl in starch molecule, generation a kind of containing the starch ether derivative with positive charge on amino, nitrogen-atoms.Cationic starch mainly contains tertiary amine salt and quaternary ammonium salt, and as the polymer substance with hydrophilic group, not only raw material sources are wide for it, avirulence, inexpensive, and product fully biodegradable, environmentally safe.Cationic starch is used as detergent additive, has the characteristics such as low to skin irritation, falling property of biology is good, toxicity is low.Cationic starch has many advantages, is therefore widely used in papermaking, weaving, oil field, mining industry, sewage disposal, adhesive, cosmetics (lasting agent) and other industry.Low-substituted Cationic Starch is mainly used in paper industry, and cationic starch with high substitution degree is mainly used in the aspect such as water treatment and anion exchange.
Cation-modified regenerated celulose fibre is a kind of by introducing positively charged group regenerated celulose fibre in regenerated celulose fibre molecular structure, thus make whole fiber surface positively charged, and when dyeing because dyestuff is electronegative, easily having an effect with positively charged fiber and contaminating without the need to salt adding is short.
At present by many for cellulose fiber cationization employings two kinds of approach, one is adopt the mode of post processing directly to carry out graft modification to fiber, and two is carry out graft modification to spinning material in the spinning preparation process of fiber.Former approach is simple, with low cost, but effect is only limitted to surface, and the durability of effect is poor; Latter process is complicated, and technical requirement is high, but treatment effect is thorough, and persistence is good, and the two cuts both ways.
The modifier that existing cellulose fiber cation modification technology mostly adopts is epoxychloropropane aminate and the method for derivative by graft modification thereof and the method for cellulose macromolecule chain combination.The regenerated fiber prepared by the method have modification uniform and complete, the feature that the fiber obtained has level dyeing and thoroughly contaminates.But also there is complex process, severe reaction conditions, the shortcomings such as percent grafting is low.
Cationic starch is as a kind of wide material sources, cheap, the environment friendly and pollution-free raw material of industry, has apply extremely widely in a lot of industry, as papermaking, weaving, mining industry, sewage disposal, washing chemical industry etc.But be used as modifier as spinning additive, but not yet meet pertinent literature and report.
Summary of the invention
Technical problem to be solved by this invention is: the modification carrying out existing in the process of cationization to regenerated celulose fibre is not thorough, be only limitted to surface, the problems such as complex process, propose a kind of can the preparation method of regenerated celulose fibre of salt-free dyeing, cationic starch solution is taked to spin forward slip value or is spun an injection technique and regenerated celulose fibre is prepared in spinning solution blend spinning by the method in the process preparing regenerated celulose fibre, and add crosslinking agent in the process and make, between cationic starch and cellulose macromolecule chain, cross-linking reaction occurs, make it to anchor on fiber macromolecular chain.
Technical scheme:
A kind of can the preparation method of regenerated celulose fibre of salt-free dyeing, comprise the steps: cationic starch by spinning forward slip value or the mode of injection between spinning mixes with regenerated celulose fibre, and add crosslinking agent and make, between ionic starch and cellulose, cross-linking reaction occurs, prepare the regenerated celulose fibre of cationic starch modification.
Described cationic starch adds as a solution; The preferably aqueous solution; Cationic starch content is in the solution 10 ~ 20wt%.
The addition of described cationic starch is 5 ~ 30wt% of the fine content of first of regenerated celulose fibre.
The substitution value of described cationic starch is 0.03 ~ 0.05, and viscosity is 500 ~ 1500mpaS.
Described crosslinking agent is one or both the mixing in glutaraldehyde or glyoxal; Dosage of crosslinking agent is 3 ~ 5wt% of the fine content of first of regenerated celulose fibre.
The dry of regenerated celulose fibre of described cationic starch modification is by force 2.1 ~ 2.4cN/dtex; Wet strong 1.3 ~ 1.7cN/dtex; Dryly stretch 16.0 ~ 20.0%.
Beneficial effect
The modifier used in the preparation process of the cationic-dyeable regenerated celulose fibre in the present invention is cationic starch wide material sources, low price, and it is controlled that each side character is adjustable, has the advantage that reaction condition is gentle and environment friendly and pollution-free simultaneously.Containing a large amount of cation groups on the regenerated celulose fibre prepared, better to the adsorption effect of the dye matrix with negative electrical charge, without the need to adding the short dye of electrolyte in dyeing course, reducing production cost, while economize energy, decrease the pollution of use to environment of too much inorganic salts.
Detailed description of the invention
Below by detailed description of the invention, the present invention is described in further detail.But it will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting scope of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition (such as with reference to " dyeing and finishing technology and principle " that Zhao Tao writes, China Textiles Press, 2009) or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by the conventional products of commercial acquisition.
The numerical value as range limit not only comprising and clearly listing should be interpreted as in a flexible way using the value that range format is expressed, but also comprise and be encompassed in all single numerical value within the scope of this or subinterval, be expressly recited out just as each numerical value and subinterval.Such as, the concentration range of " about 0.1% to about 5% " should be understood to the concentration not only comprising about 0.1% to about 5% clearly listed, also include single concentration in institute's how (as, 1%, 2%, 3% and 4%) and subinterval (such as, 0.1% to 0.5%, 1% to 2.2%, 3.3% to 4.4%).
The present invention adopts the method directly adding cationic starch, regenerated celulose fibre is carried out to the modification of cationization, and do not adopt the method for amination reagent modified cellulose, reason is adding to avoid and utilizing amination reagent direct modification spinning solution to be that the required condition such as temperature, pH is on the impact of spinning solution character of cationic starch, in addition cationic starch and cellulose all belong to glucose system derivative, and compatibility is good.Similar to cellulosic structure as the cationic starch taking glucose as most elementary cell, character is close, has good intersolubility, itself just can combine by hydrogen bond therebetween, the introducing of crosslinking agent makes combination therebetween more firm, and modification efficiency is higher, better effects if.The introducing of cationic starch can be mix with regenerated celulose fibre before carrying out spinning, also can be to be mixed with regenerated celulose fibre by the mode of injection during spinning process.Cationic starch is preferably through adding as a solution, such as, be the aqueous solution, and cationic starch content is in the solution 10 ~ 20wt%.The addition of cationic starch is 5 ~ 30wt% of the fine content of first of regenerated celulose fibre, is more preferably 10 ~ 20wt%.The substitution value of described cationic starch is 0.03 ~ 0.05, and the viscosity of cationic starch solution is 500 ~ 1500mpaS.
The preferred glutaraldehyde of crosslinking agent of the present invention and glyoxal are hydroxyl crosslinking agent, but the hydroxyl in cationic starch and cellulose macromolecule structure reacts, thus make the two combine more firm, and utilization ratio is higher; Dosage of crosslinking agent is 1 ~ 8wt% of the fine content of first of regenerated celulose fibre, more preferably 3 ~ 5wt%.
The dry of modification regeneration cellulose fibre obtained through said method is by force 2.1 ~ 2.4cN/dtex; Wet strong 1.3 ~ 1.7cN/dtex; Dryly stretch 16.0 ~ 20.0%.
The regenerated celulose fibre adopted in following examples can be prepared by conventional mode, and a conventional steps flow chart is: dipping, squeezing, pulverize, experienced, yellow, continuous-dissolution, filtration, deaeration.After obtained rayon spinning liquid, measure its viscosity by falling ball method, falling ball method refers to the time that 2mm steel ball falls needed for 20cm from described viscose solution.
After having prepared regenerated celulose fibre, by measuring its dyeability, below in an example, adopt R-04 dyestuff to stock-dye, measure dye uptake %.Dye dosage is 2% (o.w.f), bath raio 50:1,60 DEG C, 30min.
Embodiment 1
The preparation of rayon spinning liquid:
Raw material to be the degree of polymerization be 500 ~ 600 Cotton Pulp, the fine content of its first is greater than 90%, and according to following process route glue: dipping, squeezing, pulverize, experienced, yellow, continuous-dissolution, filtration, deaeration.According to above-mentioned manufacture technics, to form the fine content of rayon spinning liquid first be 8.9%, NaOH mass fraction is 6.0, and viscosity is (falling ball method) 59s, and ripe degree is (10%NH
4cl) 8.8ml.
The preparation of cationic starch solution:
In reactor, be the cationic starch solution of 10% with distilled water preparation mass fraction, fully stir and can obtain comparatively uniform cationic starch solution.Adopt sheet frame filter to filter through double-deck fine cloth, pressure, at below 0.2Mpa, obtains uniform cationic starch solution.
Viscose glue stoste mixes with cationic starch solution:
Cationic starch solution adds in above-mentioned stand-by viscose solution by adoption rate pump quantitatively, and mixes, as mixture.Cationic starch solution adopts syringe pump with the speed injection of 6 liters/min in dynamic mixer, in blender, add the glutaraldehyde accounting for the fine quality 3% of first simultaneously, make it mix with spinning solution, the flow of viscose solution is 50 liters/min, leaves standstill 1h under normal temperature.Wherein, the quality of cationic starch is 0%, 5%, 8%, 15%, 20%, 30% of the fine weight of first.Wherein the addition of 0% refers to and in the process of spinning, does not add cationic starch, is reference examples.
Wet spinning:
The mixed solution of cationic starch solution and viscose glue is fully reacted rear feeding wet spinning operation and carries out spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 55m/min, and coagulation bath temperature is 52 DEG C, and plasticizing-bath temperature is 95 DEG C.Coagulation bath composition is: sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
The leading indicator of the fiber prepared through above-mentioned steps is as follows.
| Cationic starch addition | 0％ | 5％ | 8％ | 15％ | 20％ | 30％ |
| Fiber number dtex | 1.68 | 1.68 | 1.69 | 1.69 | 1.69 | 1.68 |
| Dry strong cN/dtex | 1.98 | 1.96 | 2.01 | 2.31 | 2.10 | 1.92 |
| Wet strong cN/dtex | 1.32 | 1.36 | 1.49 | 1.58 | 1.38 | 1.39 |
| Dryly stretch % | 16.1 | 15.9 | 16.7 | 17.9 | 17.1 | 15.9 |
| Dye uptake % | 65.2 | 75.5 | 88.3 | 92.4 | 94.5 | 91.1 |
As can be seen from the table, by introduce cationic starch in regenerated celulose fibre after, rate of dyeing can be improved significantly, and modified fibre have better elasticity and strength character.
Reference examples 1
Adopt the modification regeneration cellulose fibre that the direct modification spinning solution of amination reagent prepares.Testing result: fiber number 1.69dtex; Dry strong 1.97cN/dtex; Wet strong 1.35cN/dtex; Dryly stretch 17.1%; Dye uptake 68.3%.
Reference examples 2
Post processing mode is adopted to carry out modification to regenerated celulose fibre.Testing result: fiber number 1.68dtex; Dry strong 1.96cN/dtex; Wet strong 1.41cN/dtex; Dryly stretch 15.8%; Dye uptake 72.5%.
Embodiment 2
The preparation of rayon spinning liquid:
Raw material to be the degree of polymerization be 500 ~ 600 hemp dissolving pulp, the fine content of its first is greater than 90%, and according to following process route glue: dipping, squeezing, pulverize, experienced, yellow, continuous-dissolution, filtration, deaeration.According to above-mentioned manufacture technics, to form the fine content of rayon spinning liquid first be 8.8%, NaOH mass fraction is 6.0, and viscosity is (falling ball method) 55s, and ripe degree is (10%NH
4cl) 8.7ml.
The preparation of cationic starch solution:
In reactor, be the cationic starch solution of 15% with distilled water preparation mass fraction, fully stir and can obtain comparatively uniform cationic starch solution.Adopt sheet frame filter to filter through double-deck fine cloth, pressure, at below 0.2Mpa, obtains uniform cationic starch solution.
Viscose glue stoste mixes with cationic starch solution:
Cationic starch solution adds in above-mentioned stand-by viscose solution by adoption rate pump quantitatively, and mixes.Cationic starch solution adopts syringe pump with the speed injection of 6 liters/min in dynamic mixer, in blender, add the glutaraldehyde of the fine quality 1%, 3%, 4%, 5%, 8% of the first accounting for regenerated celulose fibre respectively simultaneously, it is made to mix with spinning solution, the flow of viscose solution is 50 liters/min, leaves standstill 1h under normal temperature.Wherein, the quality of cationic starch is 15% of the fine weight of first of regenerated celulose fibre.
Wet spinning: the mixed solution of cationic starch solution and viscose glue is fully reacted rear feeding wet spinning operation and carries out spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 55m/min, and coagulation bath temperature is 52 DEG C, and plasticizing-bath temperature is 95 DEG C.Coagulation bath composition is: sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
The leading indicator of the fiber prepared through above-mentioned steps is as follows.
| Crosslinking agent addition | 1％ | 3％ | 4％ | 5％ | 8％ |
| Fiber number dtex | 1.68 | 1.69 | 1.69 | 1.69 | 1.68 |
| Dry strong cN/dtex | 1.91 | 2.04 | 2.39 | 2.05 | 1.93 |
| Wet strong cN/dtex | 1.36 | 1.49 | 1.62 | 1.38 | 1.39 |
| Dryly stretch % | 15.7 | 15.5 | 18.3 | 16.5 | 16.3 |
| Dye uptake % | 85.6 | 86.4 | 91.5 | 90.5 | 83.5 |
It can be seen from the table, the consumption of crosslinking agent is regulated and controled when preferable range, rate of dyeing can be improved significantly, and modified fibre has better elasticity and strength character.
Embodiment 3
The preparation of rayon spinning liquid:
Raw material to be the degree of polymerization be 500 ~ 600 bamboo pulp, the fine content of its first is greater than 90%, and according to following process route glue:
According to above-mentioned manufacture technics, to form the fine content of rayon spinning liquid first be 9.1%, NaOH mass fraction is 5.9, and viscosity is (falling ball method) 59s, and ripe degree is (10%NH
4cl) 8.9ml.
The preparation of cationic starch solution:
In reactor, be respectively the cationic starch solution of 5%, 10%, 15%, 20%, 25% with distilled water preparation mass fraction, fully stir and can obtain comparatively uniform cationic starch solution.Adopt sheet frame filter to filter through double-deck fine cloth, pressure, at below 0.2Mpa, obtains uniform cationic starch solution.
Viscose glue stoste mixes with cationic starch solution:
Cationic starch solution adds in above-mentioned stand-by viscose solution by adoption rate pump quantitatively, and mixes.Cationic starch solution adopts syringe pump with the speed injection of 6 liters/min in dynamic mixer, in blender, add the glutaraldehyde accounting for the fine quality 5% of first simultaneously, make it mix with spinning solution, the flow of viscose solution is 50 liters/min, leaves standstill 1h under normal temperature.Wherein, the quality of cationic starch is 20% of the fine weight of first.
Wet spinning:
The mixed solution of cationic starch solution and viscose glue is fully reacted rear feeding wet spinning operation and carries out spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 55m/min, and coagulation bath temperature is 52 DEG C, and plasticizing-bath temperature is 95 DEG C.Coagulation bath composition is: sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
The leading indicator of the fiber prepared through above-mentioned steps is as follows.
| Cationic starch concentration | 5％ | 10％ | 15％ | 20％ | 25％ |
| Fiber number dtex | 1.69 | 1.68 | 1.68 | 1.68 | 1.69 |
| Dry strong cN/dtex | 1.90 | 2.01 | 2.24 | 2.11 | 1.88 |
| Wet strong cN/dtex | 1.32 | 1.45 | 1.60 | 1.35 | 1.32 |
| Dryly stretch % | 14.7 | 15.8 | 18.1 | 16.2 | 16.1 |
| Dye uptake % | 85.6 | 86.4 | 91.5 | 90.5 | 83.5 |
It can be seen from the table, cationic starch concentration is regulated and controled when preferable range, rate of dyeing can be improved significantly, and modified fibre has better elasticity and strength character.
Embodiment 4
The preparation of rayon spinning liquid:
Raw material to be the degree of polymerization be 500 ~ 600 bamboo pulp, the fine content of its first is greater than 90%, and according to following process route glue:
According to above-mentioned manufacture technics, to form the fine content of rayon spinning liquid first be 9.1%, NaOH mass fraction is 5.9, and viscosity is (falling ball method) 59s, and ripe degree is (10%NH
4cl) 8.9ml.
The preparation of cationic starch solution:
First; modification is carried out to cationic starch: be dissolved in by cationic starch in deionized water; mass concentration controls at 10wt%; after about 80 DEG C gelatinization 30min; first adding initator under nitrogen protection makes itself and starch adsorb in advance; add acrylamide monomer (quality is 20% of cationic starch) again; graft copolymerization is carried out 3 hours at 50 DEG C; modified cationic starch precipitates by the ethanol adding 95% again; at 50 DEG C, vacuumize 48h, obtains modified cationic starch.Again in reactor, be the modified cationic starch solution of 15% with distilled water preparation mass fraction, fully stir and can obtain comparatively uniform modified cationic starch solution.Adopt sheet frame filter to filter through double-deck fine cloth, pressure, at below 0.2Mpa, obtains uniform modified cationic starch solution.
Viscose glue stoste mixes with cationic starch solution:
Cationic starch solution adds in above-mentioned stand-by viscose solution by adoption rate pump quantitatively, and mixes.Cationic starch solution adopts syringe pump with the speed injection of 6 liters/min in dynamic mixer, in blender, add the glutaraldehyde accounting for the fine quality 5% of first simultaneously, make it mix with spinning solution, the flow of viscose solution is 50 liters/min, leaves standstill 1h under normal temperature.Wherein, the quality of cationic starch is 20% of the fine weight of first.
Wet spinning:
The mixed solution of cationic starch solution and viscose glue is fully reacted rear feeding wet spinning operation and carries out spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 55m/min, and coagulation bath temperature is 52 DEG C, and plasticizing-bath temperature is 95 DEG C.Coagulation bath composition is: sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.Testing result: fiber number 1.68dtex; Dry strong 2.38cN/dtex; Wet strong 1.79cN/dtex; Dryly stretch 19.7%; Dye uptake 93.6%.As can be seen from embodiment 4, after modification is carried out to cationic starch, fibrous elasticity and intensity and rate of dyeing can be improved further.
Claims (8)
1. one kind can the preparation method of regenerated celulose fibre of salt-free dyeing, it is characterized in that, comprise the steps: cationic starch by spinning forward slip value or the mode of injection between spinning mixes with regenerated celulose fibre, and add crosslinking agent and make, between ionic starch and cellulose, cross-linking reaction occurs, prepare the regenerated celulose fibre of cationic starch modification.
2. according to claim 1 can the preparation method of regenerated celulose fibre of salt-free dyeing, it is characterized in that: described cationic starch adds as a solution.
3. according to claim 2 can the preparation method of regenerated celulose fibre of salt-free dyeing, it is characterized in that: described solution is the aqueous solution.
4. according to claim 2 can the preparation method of regenerated celulose fibre of salt-free dyeing, it is characterized in that: cationic starch content is in the solution 10 ~ 20wt%.
5. according to claim 1 can the preparation method of regenerated celulose fibre of salt-free dyeing, it is characterized in that: the addition of described cationic starch is 5 ~ 30wt% of the fine content of first of regenerated celulose fibre.
6. according to claim 1 can the preparation method of regenerated celulose fibre of salt-free dyeing, it is characterized in that: the substitution value of described cationic starch is 0.03 ~ 0.05, and viscosity is 500 ~ 1500mpaS.
7. according to claim 1 can the preparation method of regenerated celulose fibre of salt-free dyeing, it is characterized in that: described crosslinking agent is one or both the mixing in glutaraldehyde or glyoxal; Dosage of crosslinking agent is 3 ~ 5wt% of the fine content of first of regenerated celulose fibre.
8. according to claim 1 can the preparation method of regenerated celulose fibre of salt-free dyeing, it is characterized in that: the dry of regenerated celulose fibre of described cationic starch modification is by force 2.1 ~ 2.4cN/ dtex; Wet strong 1.3 ~ 1.7cN/ dtex; Dryly stretch 16.0 ~ 20.0%.
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Cited By (3)
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| CN106521693A (en) * | 2016-10-26 | 2017-03-22 | 丹阳正联知识产权运营管理有限公司 | Technological method for producing salt-free dyed-cotton fiber adopting starch base |
| CN111394818A (en) * | 2020-04-07 | 2020-07-10 | 江苏金太阳纺织科技股份有限公司 | Liquorice regenerated cellulose fiber and preparation method thereof |
| CN114134586A (en) * | 2021-11-22 | 2022-03-04 | 唐山三友集团兴达化纤有限公司 | Acid dye dyeable viscose fiber and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521693A (en) * | 2016-10-26 | 2017-03-22 | 丹阳正联知识产权运营管理有限公司 | Technological method for producing salt-free dyed-cotton fiber adopting starch base |
| CN111394818A (en) * | 2020-04-07 | 2020-07-10 | 江苏金太阳纺织科技股份有限公司 | Liquorice regenerated cellulose fiber and preparation method thereof |
| CN111394818B (en) * | 2020-04-07 | 2022-09-30 | 江苏金太阳纺织科技股份有限公司 | Liquorice regenerated cellulose fiber and preparation method thereof |
| CN114134586A (en) * | 2021-11-22 | 2022-03-04 | 唐山三友集团兴达化纤有限公司 | Acid dye dyeable viscose fiber and preparation method thereof |
| CN114134586B (en) * | 2021-11-22 | 2023-10-10 | 唐山三友集团兴达化纤有限公司 | Acid dye-dyeable viscose fiber and preparation method thereof |
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