Summary of the invention
Its object of the present invention is just to provide a kind of temperature-adjusting viscose production method, its product has bidirectional temp regulation function, dry fracture strength is greater than 1.7 CN/dtex, fiber number is less than 1.35dtex, and dry elongation at break is greater than 18%, and fibers melt heat absorption enthalpy is greater than 5.0J/g, solidify heat release enthalpy and be greater than 5.0J/g, fault is less than 0.1mg/100g, and transition temperature range is 10 DEG C ~ 50 DEG C, also has the feature that fiber number is little, intensity is high, heat enthalpy value is high.
Realize above-mentioned purpose and the technical scheme that adopts, comprise sheet steeping, squeezing, pulverizing, experienced, yellow, rear dissolving, maturation, filtration, phase-change material allotment, phase-change material and viscose glue mix, spinning, two bathe filter, refining processing,
(1) single-steeping quaternization is adopted to generate alkali cellulose,
itspulp floods in the NaOH solution of concentration 220 ~ 250 g/l, dipping temperature 51.0 DEG C ~ 56 DEG C, dip time 10 ~ 20 minutes, slurry congee concentration 4.5% ~ 6.0%, in immersion liquid, half fine content controls at below 45g/l, and add V388 auxiliary agent, within V388 promoter addition 2 kgs/tonne of silks, the alkali cellulose of generation, extrudes unnecessary NaOH solution through squeezing, press ratio is 2 ~ 4, after squeezing, alkali cellulose is pulverized, and degree of grinding controls within 1.0%, the alkali cellulose made, its composition contains first fibre 32% ~ 35%, containing alkali 16% ~ 18%;
(2) the experienced reaction of alkali cellulose, the experienced outlet temperature of alkali cellulose 30.0 DEG C ~ 45.0 DEG C,
Ageing time 4 ~ 7 hours, alkali cellulose viscosity 48 ~ 58 Mpa.s;
(3)yellow reaction and rear dissolving, add sex change auxiliary agent 0.5-0.8 kg/tonne of silk between the yellow stage of reaction. yellow initial temperature 26.0 DEG C ~ 30 DEG C, yellow final temperature 30 DEG C ~ 35 DEG C, CS
2addition (fine to first) 31% ~ 34%, 35 ~ 48 hours yellow time; Rear dissolution process, dissolves alkali concn 11 ± 1 g/l, dissolves alkali temperature 6.0 ~ 10.0 DEG C, dissolve glue containing first fibre 8.85 ± 0.1%, dissolve glue containing alkali 5.1 ± 0.1%, dissolve adhesiveness 38 ~ 55 seconds, dissolve glue degree of ripeness 18 ~ 25 ml, dissolve glue sulfur-bearing 2.2 ± 0.2%, dissolve glue esterification degree 35 ~ 50;
(5) filter, the impurity in removing viscose glue, spins micelle subnumber and is less than 20/gram and spins glue;
(5) maturation of viscose glue, viscose ripening temperature 16.0 DEG C ~ 6.0 DEG C, 13.0 ~ 16.0 hours viscose ripening time, spins glue composition: first fibre 8.8 ± 0.1% after maturation, containing alkali 5.1 ± 0.1%, viscosity 50 ± 3 seconds, degree of ripeness 14 ± 2ml;
(6) phase-change material preparation, phase-change material colloid is after grinding pump grinds 20 minutes, again by phase-change material delivery pump, send into and filter together, circulate at phase-change material storage tank afterwards, send into two road metre filter again, arrive static mixer again to mix with the viscose glue reaching technological requirement through maturation, phase-change material slurry quality requires: pH value controls 8 ~ 10, dispersiveness controls more than 85%, filter pore size at 3 ~ 5um, Microcapsules Size, particle diameter should control between 1 ~ 6 um, slurry concentration 30.0% ~ 50.0%;
(7) phase transformation rayon spinning liquid,
The phase-change microcapsule material paste prepared and spinning glue fully mixed by static mixer, make phase transformation rayon spinning liquid, go spinning machine shaping, microencapsulated phase change material addition is 4-6%;
(8) spinning moulding, the viscose glue mixed with phase-change material sent here by stoste workshop, measuring pump, the candle filter of spinning machine is entered through pipeline, spray from composite spinning head, in spinning bath, solidify regeneration containing the cellulose strand of phase-change microcapsule material, pool together after the preliminary drawing-off of draw-off godet and guide drawing roller into and enter plasticizing-bath again, after two road drawing-offs, enter cutting machine by fibre bundle, cut into the length of needs, fall into scouring machine and carry out post processing;
Its moulding process comprises
Composition is bathed in acid bath one:
Sulfuric acid concentration 102 ~ 108g/l
Zinc sulfate 11.5 ~ 12.0g/l
Proportion 1.310 ~ 1.325
Acid temperature 46 ~-50 DEG C
Acid bath auxiliary agent 653 0.06 ~ 0.1 kg/tonne of silk
Composition is bathed in acid bath two
Sulfuric acid concentration 40 ~ 50g/l
Temperature 70 ~ 85 DEG C
Pullin performances
Total draft rate 130 ~ 145%
One drawing-off 36 ~ 40%
(9) refining processing
Refining process:
Desulfurization bath temperature 80 DEG C ~ 85 DEG C
Desulfurization bath concentration (NaOH) 1 ~ 3 g/l
Washing temperature 35 DEG C ~ 50 DEG C
Bleaching levels Cl
-g/l 0.40 ~ 0.8
Bleaching liquid PH 8 ~ 10.
Compared with prior art the present invention has the following advantages.
Take native cellulose as raw material, soluble cellulose xanthate acid is made through operations such as alkalization, aging, yellows, be dissolved in sig water again and make viscose glue, auxiliary agent is added in these processes, improve through equipment and process, improve chemical reaction effect and filter effect, reach and improve viscose glue quality object, thus reach the object being conducive to product and regulating fiber number and physical property to improve; In phase transformation capsule material allocation process, carry out grinding and secondary micropore filtration.Before spinning, add phase transformation capsule material, mix with viscose solution; Simultaneously when viscose is still in large molecule noncrystal, during by low diameter spray silk circular hole, select suitable degree of draft and molding technological condition, reach the fiber number object of adjustment fiber.Product has bidirectional temp regulation function, dry fracture strength is greater than 1.7 CN/dtex, fiber number is less than 1.35dtex, dry elongation at break is greater than 18%, fibers melt heat absorption enthalpy is greater than 5.0J/g, and solidify heat release enthalpy and be greater than 5.0J/g, fault is less than 0.1mg/100g, transition temperature range is 10 DEG C ~ 50 DEG C, has the advantages that fiber number is little, intensity is high, heat enthalpy value is high.
Detailed description of the invention
Comprise sheet steeping, squeezing, pulverizing, experienced, yellow, rear dissolving, maturation, filtration, phase-change material allotment, phase-change material and viscose glue mix, spinning, two bathe filter, refining processing,
(1) single-steeping quaternization is adopted to generate alkali cellulose,
itspulp floods in the NaOH solution of concentration 220 ~ 250 g/l, dipping temperature 51.0 DEG C ~ 56 DEG C, dip time 10 ~ 20 minutes, slurry congee concentration 4.5% ~ 6.0%, in immersion liquid, half fine content controls at below 45g/l, and add V388 auxiliary agent, within V388 promoter addition 2 kgs/tonne of silks, the alkali cellulose of generation, extrudes unnecessary NaOH solution through squeezing, press ratio is 2 ~ 4, after squeezing, alkali cellulose is pulverized, and degree of grinding controls within 1.0%, the alkali cellulose made, its composition contains first fibre 32% ~ 35%, containing alkali 16% ~ 18%;
(3) the experienced reaction of alkali cellulose, the experienced outlet temperature of alkali cellulose 30.0 DEG C ~ 45.0 DEG C,
Ageing time 4 ~ 7 hours, alkali cellulose viscosity 48 ~ 58 Mpa.s;
(3)yellow reaction and rear dissolving, add sex change auxiliary agent 0.5 ~ 0.8 kg/tonne of silk between the yellow stage of reaction. yellow initial temperature 26.0 DEG C ~ 30 DEG C, yellow final temperature 30 DEG C ~ 35 DEG C, CS
2addition (fine to first) 31% ~ 34%, 35 ~ 48 hours yellow time; Rear dissolution process, dissolves alkali concn 11 ± 1 g/l, dissolves alkali temperature 6.0 ~ 10.0 DEG C, dissolve glue containing first fibre 8.85 ± 0.1%, dissolve glue containing alkali 5.1 ± 0.1%, dissolve adhesiveness 38 ~ 55 seconds, dissolve glue degree of ripeness 18 ~ 25 ml, dissolve glue sulfur-bearing 2.2 ± 0.2%, dissolve glue esterification degree 35 ~ 50;
(6) filter, the impurity in removing viscose glue, spins micelle subnumber and is less than 20/gram and spins glue;
(5) maturation of viscose glue, viscose ripening temperature 16.0 DEG C ~ 6.0 DEG C, 13.0 ~ 16.0 hours viscose ripening time, spins glue composition: first fibre 8.8 ± 0.1% after maturation, containing alkali 5.1 ± 0.1%, viscosity 50 ± 3 seconds, degree of ripeness 14 ± 2ml;
(6) phase-change material preparation, phase-change material colloid is after grinding pump grinds 20 minutes, again by phase-change material delivery pump, send into and filter together, circulate at phase-change material storage tank afterwards, send into two road metre filter again, arrive static mixer again to mix with the viscose glue reaching technological requirement through maturation, phase-change material slurry quality requires: pH value controls 8 ~ 10, dispersiveness controls more than 85%, filter pore size at 3 ~ 5um, Microcapsules Size, particle diameter should control between 1 ~ 6 um, slurry concentration 30.0% ~ 50.0%;
(7) phase transformation rayon spinning liquid,
The phase-change microcapsule material paste prepared and spinning glue fully mixed by static mixer, make phase transformation rayon spinning liquid, go spinning machine shaping, microencapsulated phase change material addition is 4-6%;
(8) spinning moulding, the viscose glue mixed with phase-change material sent here by stoste workshop, measuring pump, the candle filter of spinning machine is entered through pipeline, spray from composite spinning head, in spinning bath, solidify regeneration containing the cellulose strand of phase-change microcapsule material, pool together after the preliminary drawing-off of draw-off godet and guide drawing roller into and enter plasticizing-bath again, after two road drawing-offs, enter cutting machine by fibre bundle, cut into the length of needs, fall into scouring machine and carry out post processing;
Its moulding process comprises
Composition is bathed in acid bath one:
Sulfuric acid concentration 102 ~ 108g/l
Zinc sulfate 11.5 ~ 12.0g/l
Proportion 1.310 ~ 1.325
Acid temperature 46 ~-50 DEG C
Acid bath auxiliary agent 653 0.06 ~ 0.1 kg/tonne of silk
Composition is bathed in acid bath two
Sulfuric acid concentration 40 ~ 50g/l
Temperature 70 ~ 85 DEG C
Pullin performances
Total draft rate 130 ~ 145%
One drawing-off 36 ~ 40%
(9) refining processing
Refining process:
Desulfurization bath temperature 80 DEG C ~ 85 DEG C
Desulfurization bath concentration (NaOH) 1 ~ 3 g/l
Washing temperature 35 DEG C ~ 50 DEG C
Bleaching levels Cl
-g/l 0.40 ~ 0.8
Bleaching liquid PH 8 ~ 10.
Select circular combined spinning head in described spinning technique, circular combined spinning head panel distributes 45 spinning heads, and spinning head specification is Φ 16 mm, spray orifice footpath Φ 0.05 mm.
Describedly be filtered into KK filter secondary filter, KK filter filter screen selects 15--25 μm of stainless steel metal fibre sintering felt.
Described viscose glue course of dissolution adopts three grades of grindings.
Described yellow adopts horizontal single ribbon flight chuck xanthating machine.
The pH value of described microencapsulated phase change material slurry is 8-10, and before phase-change material micro-capsule particulate slurry injects viscose glue mixing, carry out grinding and secondary micropore filtration, pore size filter is at 3-5um, and Microcapsules Size controls between 1 ~ 6 um.
Described spinning adopts a bath deep bathing type and two baths to combine shaping, a bath tow length of immersion 700mm, and is placed in by two baths above the godet roller in spinning machine.
Described microencapsulated phase change material slurry and spinning glue are evenly mixed by static mixer.
Embodiment
Take native cellulose as raw material, soluble cellulose xanthate acid is made through operations such as alkalization, aging, yellows, be dissolved in sig water again and make viscose glue, auxiliary agent is added in these processes, improve through equipment and process, improve chemical reaction effect and filter effect, reach and improve viscose glue quality object, thus reach the object being conducive to product and regulating fiber number and physical property to improve; In phase transformation capsule material allocation process, carry out grinding and secondary micropore filtration.Before spinning, add phase transformation capsule material, mix with viscose solution, make it that there is bidirectional temp regulation function; Simultaneously when viscose is still in large molecule noncrystal, during by low diameter spray silk circular hole, select suitable degree of draft and molding technological condition, reach the fiber number object of adjustment fiber.
In order to realize fiber number little (about reaching 1.35 dtexs), also carry out improving improving to viscose preparation technology, spinning technique and refining process and relevant device.
(1), product main performance
1, there is the advantage of common viscose fiber
Temperature-adjusting viscose is a kind of novel viscose functional product, it has all traditional performances of viscose, stronger moisture absorption ventilating capability, ventilative, resistance to daylight, anti-insect, antistatic, easy weaving, its chemical composition are similar to cotton, more alkaline-resisting and not acidproof.In addition its thermal property is also similar to cotton.
2, latent heat formula is inhaled and is put bidirectional temp regulation function
The temperature-sensitive phase-change material of encapsulation is implanted in fiber; the skin temperature of approximating anatomy to be attracted deposit (or release) a large amount of heat with the form of " latent heat "; there is environmental protection and energy saving characteristic and bidirectional temp regulation function; the physiology avoiding Yin Wendu sharply to change causing is not suitable with; there is the performance such as outstanding regulate body temperature function and protection human body, effectively prevent air conditioner disease.
3, superior physical performance index
Its fiber number is tiny, can be used for the silk-like fabric made, and has both had the advantage of soft comfortable, the luxurious elegance of real silk fabric, and has also had glossiness good, the advantage silk-like fabrics such as product color is bright-coloured in outward appearance and serviceability more and more close to silk broadcloth.Also can be used for high density fabric, although density is very high, quality is slim and graceful, drapability is good, soft and plentiful, structure is fine and closely woven, is a kind of textile product of high added value.Also can with all kinds of fiber blends such as hair, silk, fiber crops, have knitting also can tatting.
(2), product physical property and functional performance Testing index
1, product leading indicator:
(1), dry fracture strength is greater than 1.7 CN/dtex
(2), fiber number is less than 1.35dtex
(3), dry elongation at break is greater than 18% (4), fibers melt heat absorption enthalpy is greater than 5.0J/g; Solidify heat release enthalpy and be greater than 5.0J/g
(5) fault is less than 0.1mg/100g
(6) transition temperature range is 10 DEG C ~ 50 DEG C
(3), production important technological parameters;
1, the viscose glue index of quality: viscosity 60 ± 3 seconds (falling ball method)
Degree of ripeness 14 ± 2ml (10%NH4Cl)
Spin micelle subnumber (particle diameter 20--40 μm) to be less than 25/ gram and to spin glue
Spin glue composition: first fibre 8.8 ± 0.1% is containing alkali 5.1 ± 0.1%
2, alkali cellulose degree of grinding: be less than 1.0%;
3, temperature-sensitive phase-change material: microcapsule diameter is less than 6 μm, wall thickness is less than 0.8 μm,
During spinning, microcapsules addition is 4-6%;
Phase-change material mother liquor density 1.015, concentration 40.0%,
PH value is 8.9
Dispersant addition 1-2%
Decentralization is greater than 85%
4, acid bath composition: ZnSO4 11.5 ± 0.5g/l H2SO4 105 ± 3 g/l
5, Pullin performances
Total draft rate 130-145%
One drawing-off 35---42%
(4) to viscose glue preparation, technological forming, refining processing and phase-change material treatment technology, specifically comprise:
1, the selection of spinning head
Select circular combined spinning head, (acid is entered in circular combined centre to circular combined large spinning head, and panel distributes 45 spinning heads.Spinning head specification: Φ 16 mm, spray orifice footpath Φ 0.05 mm), distribute more equably inside and outside acid bath concentration, be beneficial to shaping in chemical reaction evenly carry out, substantially increase reaction effect.
The pore size precision of spinning head and micropore fineness are improved, micropore Streamline Design is improved, improve spinnerette material, its scratch resistance and non-deformability effectively improve. and surface treatment is carried out to spinning head, comprises micropore inwall on the whole surface of spinning head, generate one deck modified layer equably, at nozzle surface, make the electrode position which form a suitable viscose spinning, make it not easily adsorb colloidal particles shape discarded object, thus plug-hole is significantly reduced.
2, improve viscose filtration, guarantee that viscose glue removes acrobatics effect
Because the product fiber number of producing is less, spinneret orifice footpath also should be relatively little, and injection diameter is less, the easier plug-hole of impurity, and therefore, the impurity content in spinning viscose is the smaller the better.For this reason, employ KK filter and carry out secondary filter, 15--25 μm of stainless steel metal fibre sintering felt is adopted to the choosing of KK filter filter screen, greatly reduces the impurity in viscose glue.
3, improve viscose glue and dissolve grinding effect
Adopt three grades of grindings, high-efficiency grinding mill internal structure is improved, adopt two abrasive disk type, substantially increase the efficiency of viscose glue grinding, fully ensure the quality of dissolving glue.
4, yellow reaction effect is improved
Adopt serriform gear rack 3 roller pulverizer, improve the fine degree of grinding of alkali, increase the specific area of alkali fibre, be conducive to completing of follow-up yellow reaction; Adopt horizontal single ribbon flight, jacketed xanthating machine, stirrer diameter, single-axis bidirectional ribbon flight, stir without dead angle, evenly, yellow reaction effect improves greatly in yellow reaction;
5, the auxiliary agent selected, improves reactivity worth and the strainability of fiber; Improve viscose glue quality.
6, phase-change material micro-capsule particulate slurry, carries out grinding and secondary micropore filters, filter bores
Footpath, at 3-5um, ensures slurry slagging-off effect; Phase-change material micro-capsule particulate slurry is carried out and is spun front injection, and uses static mixer, ensure that mixed effect is even, stable, is conducive to product with stable quality; Carry out dispersing depolymerization and pH value adjustment to phase-change material micro-capsule particulate slurry, the pH value of microencapsulated phase change material slurry is strict controlled in 8-10.
7, in spinning in forming process, adopt a bath (deep bathing type) and two baths to combine shaping, one bathes tow length of immersion 700mm is also placed in above the godet roller in spinning machine by two baths; Be conducive to fiberoptic fiber physical index to improve.
8, fiber-forming process condition is improved, comprise acid bath composition and two bath process, and the adjustment of Pullin performances; Add auxiliary agent in acid bath, reduce the attachment produced near spinneret orifice, be beneficial to spinning moulding, reduce fault.
9, the acid water after a concise washing is focused on, and select Fen Beike filter, choose diatomite FUNDABAC filter drainage medium, ensure to clear out sedimentary effect in two baths.
10, achieving sulfuric acid replaces acetic acid to carry out the technique of pickling, improves production environment, reduces product cost.