CN102839440A - Cotton, wood and bamboo composite pulp phase-change microcapsule viscose and preparation method thereof - Google Patents
Cotton, wood and bamboo composite pulp phase-change microcapsule viscose and preparation method thereof Download PDFInfo
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- CN102839440A CN102839440A CN2012103571265A CN201210357126A CN102839440A CN 102839440 A CN102839440 A CN 102839440A CN 2012103571265 A CN2012103571265 A CN 2012103571265A CN 201210357126 A CN201210357126 A CN 201210357126A CN 102839440 A CN102839440 A CN 102839440A
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- viscose
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- change microcapsule
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 96
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- 235000017491 Bambusa tulda Nutrition 0.000 title claims abstract description 95
- 241001330002 Bambuseae Species 0.000 title claims abstract description 95
- 235000015334 Phyllostachys viridis Nutrition 0.000 title claims abstract description 95
- 239000011425 bamboo Substances 0.000 title claims abstract description 95
- 229920000742 Cotton Polymers 0.000 title claims abstract description 64
- 239000002023 wood Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title abstract description 9
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- 238000009987 spinning Methods 0.000 claims description 51
- 230000008569 process Effects 0.000 claims description 50
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 43
- 238000001914 filtration Methods 0.000 claims description 41
- 239000003292 glue Substances 0.000 claims description 38
- 239000000243 solution Substances 0.000 claims description 38
- 239000012782 phase change material Substances 0.000 claims description 28
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 23
- 230000009466 transformation Effects 0.000 claims description 22
- 238000007598 dipping method Methods 0.000 claims description 21
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 21
- 239000000839 emulsion Substances 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 18
- 239000003643 water by type Substances 0.000 claims description 18
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 238000004090 dissolution Methods 0.000 claims description 15
- 230000035800 maturation Effects 0.000 claims description 14
- 229920000609 methyl cellulose Polymers 0.000 claims description 14
- 239000001923 methylcellulose Substances 0.000 claims description 14
- 238000012545 processing Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 12
- 238000004945 emulsification Methods 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- 238000006477 desulfuration reaction Methods 0.000 claims description 8
- 230000023556 desulfurization Effects 0.000 claims description 8
- 229920001971 elastomer Polymers 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 8
- 235000011152 sodium sulphate Nutrition 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 8
- 229960001763 zinc sulfate Drugs 0.000 claims description 8
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- -1 sulphonic acid ester Chemical class 0.000 claims description 7
- 230000008961 swelling Effects 0.000 claims description 7
- 238000010257 thawing Methods 0.000 claims description 7
- 235000002918 Fraxinus excelsior Nutrition 0.000 claims description 6
- 239000002956 ash Substances 0.000 claims description 6
- 239000002585 base Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 230000009257 reactivity Effects 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 7
- 239000008367 deionised water Substances 0.000 abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 2
- 230000003020 moisturizing effect Effects 0.000 abstract 1
- 238000004383 yellowing Methods 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 12
- 238000009825 accumulation Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 6
- 230000006870 function Effects 0.000 description 5
- 238000005406 washing Methods 0.000 description 4
- 229920002488 Hemicellulose Polymers 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- PSYGHMBJXWRQFD-UHFFFAOYSA-N 2-(2-sulfanylacetyl)oxyethyl 2-sulfanylacetate Chemical compound SCC(=O)OCCOC(=O)CS PSYGHMBJXWRQFD-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 235000019394 potassium persulphate Nutrition 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
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- 229920001131 Pulp (paper) Polymers 0.000 description 1
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- 150000004996 alkyl benzenes Chemical class 0.000 description 1
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- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 description 1
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 description 1
- 229940113124 polysorbate 60 Drugs 0.000 description 1
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- 238000009736 wetting Methods 0.000 description 1
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- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to cotton, wood and bamboo composite pulp phase-change microcapsule viscose and a preparation method thereof, belonging to the viscose field. The phase-change microcapsule comprises 80-250 parts of methyl methacrylate, 80-150 parts of phase change paraffin, 2.5-6 parts of an emulsifying agent, 0.5-1.5 parts of azo initiator, and 300-400 parts of deionized water. According to the invention, cotton, wood and bamboo composite pulp is used for preparing spun-viscose for producing the cotton, wood and bamboo composite pulp phase-change microcapsule viscose, and steps such as alkali steeping, aging, yellowing, dissolving and the like during the viscose production process are optimized. The microcapsule disclosed by the invention has a uniform grain size, is suitable for producing composite viscose and capable of remarkably improving the quality of the viscose and the spinnability with small influence; moreover, the prepared viscose not only has a natural moisturizing and ventilating effect of composite bamboo pulp fiber, but also has the function of accumulating heat and adjusting temperature.
Description
Technical field
The present invention relates to a kind of viscose and preparation method thereof, relate in particular to a kind of cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose and preparation method thereof, belong to field of viscose fiber.
Background technology
At present, utilized renewable resource to develop multiple fiber both at home and abroad, what wherein technology was the most ripe, consumption is maximum is regenerated celulose fibre, and wherein the most representative is bamboo fibre.Bamboo fibre is exactly a kind of cellulose fibre that from the bamboo of self-sow, extracts; Bamboo is by 40%～50% cellulose; 30% pentosan and 20%～25% lignin are formed; Wherein most important part is a cellulose, can make corresponding fiber through the processing of bamboo is purified or regenerated.
Functional fiber with heat-accumulation temperature-adjustment function is a developing field of present industry production research and development; Because having the heat-accumulation temperature-adjustment function, fiber will more and more receive popular favor from now on; Market prospects are wide, at present most domestic viscose manufacturer carried out one after another a series of to the heat-accumulation temperature-adjustment fiber research and development and obtained a large amount of achievements.
It is 200710123411.X that State Intellectual Property Office discloses an application number in 2008.12.24; Name is called the patent of invention of " intellectual and temperature-adjusting viscose and preparation method thereof "; This invention relates to a kind of intellectual and temperature-adjusting viscose and preparation method thereof; Said intellectual and temperature-adjusting viscose is in the common viscose fiber production process, to add phase-change material micro-capsule to make; Wherein fiber weight percentage consists of: bone dry fiber content is 84.7-92.85%, and phase-change material micro-capsule content is 2-25% in the bone dry fiber; Water content is 7-15%; Oil content is 0.15-0.30%; This fiber is when having inherited the viscose good characteristic; Have significant accumulation of heat, heat release bidirectional temp regulation function; It solidifies heat release enthalpy Δ H >=2.5J/g, and fusion heat absorption enthalpy Δ H >=2.5J/g can be widely used in fields such as clothes, underwear, bedding.
It is 201010295055.1 that State Intellectual Property Office discloses an application number in 2011.1.12, and name is called the patent of invention of " a kind of temperature adjustment bamboo viscose and preparation method thereof ", and this invention provides a kind of temperature adjustment bamboo viscose.The present invention also provides a kind of preparation method of temperature adjustment bamboo viscose, comprising: it is 1%～20% phase-change microcapsule colloidal solution that mass concentration is provided; The bamboo cellulose pulp after dipping, squeezing and pulverization process, is obtained alkali cellulose; After the said alkali cellulose experienced operation of process successively, yellow operation, dissolution process, mixed processes, deaeration operation, filtration operation, spinning process and postprocessing working procedures; Obtain temperature adjustment bamboo viscose; When carrying out yellow operation, dissolution process, mixed processes or spinning process; In material, add said phase-change microcapsule colloidal solution, the yellow operation may further comprise the steps: to alkalizing through adding alkali lye in the alkali cellulose of experienced operation, alkalization temperature is 15 ℃～25 ℃; 10min～15min was with alkali cellulose temperature adjustment to yellow reaction temperature before alkalization finished, and alkalization end back adds carbon disulfide and carries out yellow in said alkali cellulose.
The phase-change material micro-capsule that above-mentioned patent adopts is to be the wall material with macromolecular compound composite membranes such as urea aldehyde, polyureas, epoxy resin, polyester, polystyrene; With phase-change material, heat memory material or plastic crystals material is the microcapsules that core is processed, and microcapsules particle diameter and the latent heat of phase change prepared differ bigger.
It is 200910081389.6 that State Intellectual Property Office discloses an application number in 2009.10.7; Name is called the patent of invention of " preparation method of the phase-change material that a kind of microcapsules coat "; This invention relates to a kind of preparation method of phase-change material of microcapsules coating, and 1. by paraffin: the mass ratio of methyl methacrylate is got material at 1: 3; 2. take by weighing GDMA, 1% methacrylic acid, 1% lauryl sodium sulfate, 1.5% potassium peroxydisulfate, 1% ~ 15% ferrite, 400% deionized water by 0.5% of gross mass in 1; 3. lauryl sodium sulfate is joined in the deionized water, be heated to 50 ℃; 4. the paraffin of ferrite and thawing is added in 3 the solution; 5. ultrasonic emulsification adds methyl methacrylate, GDMA and methacrylic acid; 6. emulsification again has the solution immigration that obtains in the device of mechanical agitation, condenser pipe, air inlet and charge door; 7. the ventilation deoxygenation is 0.5 hour, and water-bath is heated to 70 ℃, adds potassium peroxydisulfate, reduces to room temperature, obtains the phase-change material that microcapsules coat.Be used for fields such as building, heat-accumulation temperature-adjustment weaving and electronic equipment.
Phase-change material prescription that microcapsules in the above-mentioned patent coat and preparation method are very complicated, and material is difficult to buy, and preparation time is long; Emulsifying manner is a ultrasonic emulsification, and complicated operation is wayward; Cost and security risk are high; And the microcapsules granularity for preparing is inhomogeneous, is not suitable for the production of compound pulp viscose, and is very big to viscose quality and spinnability influence.
Summary of the invention
It is all very complicated to the objective of the invention is to solve phase-change material prescription and preparation method that microcapsules of the prior art coat, and the microcapsules granularity that obtains is inhomogeneous, is not suitable for the production of composite viscose fiber; To viscose quality and the far-reaching problem of spinnability; A kind of cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose are provided, simplify and optimized the prescription of microcapsules greatly, and the microcapsules epigranular that obtains; Be fit to the production of compound pulp viscose; Can significantly improve viscose quality and spinnability, the viscose that makes not only has compound bamboo pulp fiber natural moisture preserving and ventilative effect, and has the function of heat-accumulation temperature-adjustment.
Another object of the present invention provides the preparation method through optimizing and simplifying of above-mentioned cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose; Make whole technical process be easy to control, cost and security risk and reduce, and solved in the existing production adhering process that the dipping effect of pulp is bad; The alkali cellulose that generates is inhomogeneous; And fall and gather too much, can cause the cellulose sulfonate viscosity of generation low, it is poor to filter; It is powerful low that the finished fiber that generates shows, the problem of spinnability difference.
In order to realize the foregoing invention purpose, concrete technical scheme of the present invention is following:
A kind of cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose is characterized in that: phase-change microcapsule content is 10～30wt.% in described cotton, wood, the compound pulp phase-change microcapsule of the bamboo viscose staple fibre; Described phase-change microcapsule comprises the raw material components of following parts by weight:
80～250 parts of methyl methacrylates
80～150 parts in phase transformation paraffin
2.5～6 parts of emulsifying agents
0.5～1.5 part of azo initiator
300～400 parts of deionized waters.
Phase transformation paraffin of the present invention is preferred, and the employing fusing point is 20～30 ℃ a phase transformation paraffin.
Emulsifying agent of the present invention is the conventional emulsifying agent in this area, preferably: alkyl benzene sulphonate sodium salt, polysorbate60, Tween 80, this class 60 or this class 80.
The preparation method of a kind of cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose is characterized in that: comprise following processing step:
A, preparation paraffin wax emulsion
With 300～400 parts of deionized waters, the paraffin of 80～150 parts of thawings, 2.5～6 parts of emulsifying agents, 0.5～1.5 part of initator mixes, and at 60～70 ℃, rotating speed is that high speed shear emulsification made paraffin wax emulsion in 15～30 minutes under 1500～2000rpm;
B, preparation contain the phase-change microcapsule of phase-change material
80～250 parts of methyl methacrylates being added dropwise in the paraffin wax emulsion of steps A preparation, is 2000～3000rpm at rotating speed, and temperature is 55～65 ℃ reacted 110～130 minutes down, made the phase-change microcapsule that contains phase-change material;
C, alkali steeping
Select cotton, wood, the compound pulp of bamboo as raw material, carry out alkali steeping and handle, the concentration of dipping alkali is 260～280g/L, and dipping temperature is controlled to be 42～44 ℃, and dip time is 75～85 minutes, obtains cellulose sulfonate;
D, experienced
The cellulose sulfonate that steps A is obtained carries out experienced processing, and experienced temperature is controlled to be 40～43 ℃, and ageing time is 90～100 minutes;
E, yellow
The experienced cellulose sulfonate of process that step B is obtained carries out the yellow dissolution process, obtains viscose solution, wherein CS
2Addition be 35～37% of methylcellulose;
F, dissolving
The yellow cellulose processed sulphonic acid ester that passes through that step C is obtained carries out dissolution process, is specially at 8～12 ℃ of following demineralized waters that add fully to dissolve, and the grinding through common process obtains viscose glue again;
G, deaeration, maturation, filtration
The viscose glue that step D is obtained carries out conventional deaeration, maturation is handled; Carry out filtration treatment according to common process again, obtaining the ɑ content of cellulose is 8.9～9.2%, sodium hydrate content 5.5～6 %; Viscosity 45～55 seconds, degree of ripeness (ammonia value) 4.5～5.5ml spins preceding viscose.
H, preparation viscose glue mixed solution
The phase-change microcapsule that contains phase-change material that makes among the step B is joined spinning in the preceding viscose of obtaining among the step G; Mix the nature dissolving; Stirring and making solid content is 8.5～9.3%, and sodium hydrate content is 5.7～6.3% the preceding viscose glue mixed solution that spins;
I, filtration
The preceding viscose glue mixed solution that spins that step H is made makes spinning solution through the filtering technique of routine;
J, with spinning solution through conventional spinning, desulfurization, wash, oil and stoving process makes the compound bamboo pulp phase-change microcapsule of product viscose.
At the phase-change microcapsule core described in steps A and the B is phase-change material phase transformation paraffin, and the wall material is the free yl polymerizating monomer methyl methacrylate.
Described cotton, wood, the compound pulp of bamboo can be on market, to buy, also can be according to the preparation of existing this area common process, and the compositely proportional of its middle cotton, wood, bamboo can be arbitrary proportion.
The compositely proportional of three kinds of pulps is preferably in above-mentioned cotton, wood, the compound pulp of bamboo:
Bamboo: cotton: wood=55～75:15～20:10～25.It adopts common process to process compound pulp.
In step C; The index of described cotton, wood, the compound pulp of bamboo can be any index of compound pulp standard on the market, and its preferred index is: viscosity is 10～12mpa.s, methylcellulose content for>=93%, content of ashes for≤0.08%, irony content for≤14ppm, inhale that base number is 530～600%, swelling capacity is 170～210%, is 770～830 g/m quantitatively
2, moisture is 10～11.5%, whiteness for>=83%, reactivity worth is 0～250s (9mlCS
2).
In step F; Demineralized water can be by replacing behind the scrap rubber water thin up after filtering, and the index of dissolving, the viscose glue that obtains after grinding is: the ɑ content of cellulose is 8.5～8.8%, and sodium hydrate content is 5～5.5%; Viscosity 60～70 seconds, degree of ripeness (ammonia value) 6.5～7.5ml.
In step G, preferred: the aperture that described filtration is adopted is the stainless steel sintering net of 16～25um.
Be meant that in the spinning described in the step J be 110～130g/l with spinning solution at sulfuric acid content, sodium sulphate content is 328～332g/l, and zinc sulfate content is 10～14g/l, and temperature is a spinning moulding in 48～52 ℃ the acid bath.
The useful technique effect that the present invention brings:
1, the present invention simplifies and optimizes on the basis of the phase-change microcapsule prescription of existing compound bamboo pulp phase-change microcapsule viscose; The microcapsules epigranular that obtains; Be fit to the production of composite viscose fiber, little to viscose quality and spinnability influence, can significantly improve viscose quality and spinnability; The viscose that makes not only has compound bamboo pulp fiber natural moisture preserving and ventilative effect, and has the function of heat-accumulation temperature-adjustment;
2, the present invention optimizes on the basis of the compound bamboo pulp phase-change microcapsule of existing preparation viscose technology and improves, and mainly contains following advantage:
1) in alkali steeping; Dipping alkali concn, dipping temperature and dip time that the present invention selects cooperatively interact, and help cellulosic swelling, improve dipping effect; Guarantee that cotton, wood pulps after adding bamboo pulp, are 50～60% through the esterification degree that floods the cellulose sulfonate that obtains; The crosslinking time of compound bamboo pulp bamboo pulp and NaOH in minutes just can be accomplished; But pulp progressively reaches uniform degree to fibrous inside infiltration to alkali lye and needs certain hour from wetting; The plain stripping of hemicellulose then needs more time; Dip time is long more, and the hemicellulose stripping is more abundant, and its dissolution rate descends along with the increase of hemicellulose concentration in the solution; Reach dynamic equilibrium at last, adopt alkali steeping parameter of the present invention can make whole cotton, wood, the compound pulp system of bamboo reach dynamic equilibrium; And its dipping temperature can make follow-up yellow reaction more even;
2) in experienced, in cotton, wood, the compound pulp of bamboo, its degree of polymerization separately is different; In process of production alkali cellulose when experienced, fall gather less, adopt experienced temperature of the present invention and ageing time control, can obtain the narrower cellulose of molecular weight distribution; Make that the viscose riscosity that makes is higher, has good uniformity in the subsequent production process; Improve the degree of polymerization greatly, thereby in spinning process, can improve the tensile property of as-spun fibre, ready for improving the plasticizing drawing-off;
3) in yellow, the selection of the addition of carbon disulfide can prevent fully yellow of alkali cellulose, makes that the filter process of dissolving and viscose glue of cellulose sulfonate is more smooth, can not cause milky white fiber simultaneously, has reduced unit consumption and pollution;
4) compositely proportional of three kinds of pulps is in cotton of the present invention, wood, the compound pulp of bamboo: bamboo: cotton: wood=55～75:15～20:10～25; Improved the stability of pulp; Can not influence the processing parameter of subsequent handling; And can better bring into play the natural antibacterial property of bamboo pulp, can better evade definite that bamboo pulp is difficult to react again;
5) dissolving water demineralized water of the present invention can be used the solution behind the scrap rubber thin up after the filtration, has so both guaranteed the dissolving of cellulose sulfonate, has avoided the exhaust emission environment of scrap rubber again;
6) the filtration of the present invention aperture of preferably adopting is the stainless steel sintering net of 16～25um, has been controlled at the filter area an of the best, can reduce the loss of viscose glue, reduces cost, and is beneficial to environmental protection;
7) process of the present invention and parameters Optimization are an indivisible and integral body independently, and each parameters Optimization cooperatively interacts, and make that the dipping effect of compound pulp is better; The alkali cellulose that generates is even; Avoid falling and gather too much, can cause the cellulose sulfonate viscosity of generation low, it is poor to filter; The assembled watch that generates is powerful low now, the problem of spinnability difference.
The specific embodiment
Embodiment 1
A kind of cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose, phase-change microcapsule content is 10wt.% in described cotton, wood, the compound pulp phase-change microcapsule of the bamboo viscose staple fibre; Described phase-change microcapsule comprises the raw material components of following parts by weight:
80 parts of methyl methacrylates
80 parts in phase transformation paraffin
2.5 parts of emulsifying agents
0.5 part of azo initiator
300 parts of deionized waters.
Preferably, described phase transformation paraffin employing fusing point is 20 ℃ a phase transformation paraffin.
Embodiment 2
A kind of cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose, phase-change microcapsule content is 30wt.% in described cotton, wood, the compound pulp phase-change microcapsule of the bamboo viscose staple fibre; Described phase-change microcapsule comprises the raw material components of following parts by weight:
250 parts of methyl methacrylates
150 parts in phase transformation paraffin
6 parts of emulsifying agents
1.5 parts of azo initiators
400 parts of deionized waters.
Preferably, described phase transformation paraffin employing fusing point is 30 ℃ a phase transformation paraffin.
Embodiment 3
A kind of cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose, phase-change microcapsule content is 20wt.% in described cotton, wood, the compound pulp phase-change microcapsule of the bamboo viscose staple fibre; Described phase-change microcapsule comprises the raw material components of following parts by weight:
165 parts of methyl methacrylates
115 parts in phase transformation paraffin
4.25 parts of emulsifying agents
1 part of azo initiator
350 parts of deionized waters.
Preferably, described phase transformation paraffin employing fusing point is 25 ℃ a phase transformation paraffin.
Embodiment 4
A kind of cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose, phase-change microcapsule content is 17wt.% in described cotton, wood, the compound pulp phase-change microcapsule of the bamboo viscose staple fibre; Described phase-change microcapsule comprises the raw material components of following parts by weight:
200 parts of methyl methacrylates
99 parts in phase transformation paraffin
5.1 parts of emulsifying agents
0.88 part of azo initiator
395 parts of deionized waters.
Preferably, described phase transformation paraffin employing fusing point is 28 ℃ a phase transformation paraffin.
Embodiment 5
The preparation method of a kind of cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose comprises following processing step:
A, preparation paraffin wax emulsion
With 300～400 parts of deionized waters, the paraffin of 80～150 parts of thawings, 2.5～6 parts of emulsifying agents, 0.5～1.5 part of initator mixes, and at 60 ℃, rotating speed is that high speed shear emulsification made paraffin wax emulsion in 15 minutes under the 1500rpm;
B, preparation contain the phase-change microcapsule of phase-change material
80～250 parts of methyl methacrylates being added dropwise in the paraffin wax emulsion of steps A preparation, is 2000rpm at rotating speed, and temperature is 55 ℃ reacted 110 minutes down, made the phase-change microcapsule that contains phase-change material;
C, alkali steeping
Select cotton, wood, the compound pulp of bamboo as raw material, carry out alkali steeping and handle, the concentration of dipping alkali is 260g/L, and dipping temperature is controlled to be 42 ℃, and dip time is 75 minutes, obtains cellulose sulfonate;
D, experienced
The cellulose sulfonate that steps A is obtained carries out experienced processing, and experienced temperature is controlled to be 40 ℃, and ageing time is 90 minutes;
E, yellow
The experienced cellulose sulfonate of process that step B is obtained carries out the yellow dissolution process, obtains viscose solution, wherein CS
2Addition be 35% of methylcellulose;
F, dissolving
The yellow cellulose processed sulphonic acid ester that passes through that step C is obtained carries out dissolution process, is specially at 8 ℃ of following demineralized waters that add fully to dissolve, and the grinding through common process obtains viscose glue again;
G, deaeration, maturation, filtration
The viscose glue that step D is obtained carries out conventional deaeration, maturation is handled, and carries out filtration treatment according to common process again, and obtaining the ɑ content of cellulose is 8.9%, sodium hydrate content 5.5%, and viscosity 45 seconds, degree of ripeness (ammonia value) 4.5ml spins preceding viscose.
H, preparation viscose glue mixed solution
The phase-change microcapsule that contains phase-change material that makes among the step B is joined spinning in the preceding viscose of obtaining among the step G, mix the nature dissolving, stirring and making solid content is 8.5%, and sodium hydrate content is 5.7% the preceding viscose glue mixed solution that spins;
I, filtration
The preceding viscose glue mixed solution that spins that step H is made makes spinning solution through the filtering technique of routine;
J, with spinning solution through conventional spinning, desulfurization, wash, oil and stoving process makes the compound bamboo pulp phase-change microcapsule of product viscose.
Embodiment 6
The preparation method of a kind of cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose comprises following processing step:
A, preparation paraffin wax emulsion
With 300～400 parts of deionized waters, the paraffin of 80～150 parts of thawings, 2.5～6 parts of emulsifying agents, 0.5～1.5 part of initator mixes, and at 70 ℃, rotating speed is that high speed shear emulsification made paraffin wax emulsion in 30 minutes under the 2000rpm;
B, preparation contain the phase-change microcapsule of phase-change material
80～250 parts of methyl methacrylates being added dropwise in the paraffin wax emulsion of steps A preparation, is 3000rpm at rotating speed, and temperature is 65 ℃ reacted 130 minutes down, made the phase-change microcapsule that contains phase-change material;
C, alkali steeping
Select cotton, wood, the compound pulp of bamboo as raw material, carry out alkali steeping and handle, the concentration of dipping alkali is 280g/L, and dipping temperature is controlled to be 44 ℃, and dip time is 85 minutes, obtains cellulose sulfonate;
D, experienced
The cellulose sulfonate that steps A is obtained carries out experienced processing, and experienced temperature is controlled to be 43 ℃, and ageing time is 100 minutes;
E, yellow
The experienced cellulose sulfonate of process that step B is obtained carries out the yellow dissolution process, obtains viscose solution, wherein CS
2Addition be 37% of methylcellulose;
F, dissolving
The yellow cellulose processed sulphonic acid ester that passes through that step C is obtained carries out dissolution process, is specially at 12 ℃ of following demineralized waters that add fully to dissolve, and the grinding through common process obtains viscose glue again;
G, deaeration, maturation, filtration
The viscose glue that step D is obtained carries out conventional deaeration, maturation is handled, and carries out filtration treatment according to common process again, and obtaining the ɑ content of cellulose is 9.2%, sodium hydrate content 6%, and viscosity 55 seconds, degree of ripeness (ammonia value) 5.5ml spins preceding viscose.
H, preparation viscose glue mixed solution
The phase-change microcapsule that contains phase-change material that makes among the step B is joined spinning in the preceding viscose of obtaining among the step G, mix the nature dissolving, stirring and making solid content is 9.3%, and sodium hydrate content is 6.3% the preceding viscose glue mixed solution that spins;
I, filtration
The preceding viscose glue mixed solution that spins that step H is made makes spinning solution through the filtering technique of routine;
J, with spinning solution through conventional spinning, desulfurization, wash, oil and stoving process makes the compound bamboo pulp phase-change microcapsule of product viscose.
Embodiment 7
The preparation method of a kind of cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose comprises following processing step:
A, preparation paraffin wax emulsion
With 300～400 parts of deionized waters, the paraffin of 80～150 parts of thawings, 2.5～6 parts of emulsifying agents, 0.5～1.5 part of initator mixes, and at 65 ℃, rotating speed is that high speed shear emulsification made paraffin wax emulsion in 22.5 minutes under the 1750rpm;
B, preparation contain the phase-change microcapsule of phase-change material
80～250 parts of methyl methacrylates being added dropwise in the paraffin wax emulsion of steps A preparation, is 2500rpm at rotating speed, and temperature is 60 ℃ reacted 120 minutes down, made the phase-change microcapsule that contains phase-change material;
C, alkali steeping
Select cotton, wood, the compound pulp of bamboo as raw material, carry out alkali steeping and handle, the concentration of dipping alkali is 270g/L, and dipping temperature is controlled to be 43 ℃, and dip time is 80 minutes, obtains cellulose sulfonate;
D, experienced
The cellulose sulfonate that steps A is obtained carries out experienced processing, and experienced temperature is controlled to be 41.5 ℃, and ageing time is 95 minutes;
E, yellow
The experienced cellulose sulfonate of process that step B is obtained carries out the yellow dissolution process, obtains viscose solution, wherein CS
2Addition be 36% of methylcellulose;
F, dissolving
The yellow cellulose processed sulphonic acid ester that passes through that step C is obtained carries out dissolution process, is specially at 10 ℃ of following demineralized waters that add fully to dissolve, and the grinding through common process obtains viscose glue again;
G, deaeration, maturation, filtration
The viscose glue that step D is obtained carries out conventional deaeration, maturation is handled, and carries out filtration treatment according to common process again, and obtaining the ɑ content of cellulose is 9.05%, sodium hydrate content 5.75%, and viscosity 50 seconds, degree of ripeness (ammonia value) 5ml spins preceding viscose.
H, preparation viscose glue mixed solution
The phase-change microcapsule that contains phase-change material that makes among the step B is joined spinning in the preceding viscose of obtaining among the step G; Mix the nature dissolving; Stirring and making solid content is 8.5～9.3%, and sodium hydrate content is 5.7～6.3% the preceding viscose glue mixed solution that spins;
I, filtration
The preceding viscose glue mixed solution that spins that step H is made makes spinning solution through the filtering technique of routine;
J, with spinning solution through conventional spinning, desulfurization, wash, oil and stoving process makes the compound bamboo pulp phase-change microcapsule of product viscose.
Embodiment 8
The preparation method of a kind of cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose comprises following processing step:
A, preparation paraffin wax emulsion
With 300～400 parts of deionized waters, the paraffin of 80～150 parts of thawings, 2.5～6 parts of emulsifying agents, 0.5～1.5 part of initator mixes, and at 66 ℃, rotating speed is that high speed shear emulsification made paraffin wax emulsion in 28 minutes under the 1600rpm;
B, preparation contain the phase-change microcapsule of phase-change material
80～250 parts of methyl methacrylates being added dropwise in the paraffin wax emulsion of steps A preparation, is 2900rpm at rotating speed, and temperature is 57 ℃ reacted 128 minutes down, made the phase-change microcapsule that contains phase-change material;
C, alkali steeping
Select cotton, wood, the compound pulp of bamboo as raw material, carry out alkali steeping and handle, the concentration of dipping alkali is 262g/L, and dipping temperature is controlled to be 43.6 ℃, and dip time is 79 minutes, obtains cellulose sulfonate;
D, experienced
The cellulose sulfonate that steps A is obtained carries out experienced processing, and experienced temperature is controlled to be 42 ℃, and ageing time is 97 minutes;
E, yellow
The experienced cellulose sulfonate of process that step B is obtained carries out the yellow dissolution process, obtains viscose solution, wherein CS
2Addition be 35.2% of methylcellulose;
F, dissolving
The yellow cellulose processed sulphonic acid ester that passes through that step C is obtained carries out dissolution process, is specially at 9 ℃ of following demineralized waters that add fully to dissolve, and the grinding through common process obtains viscose glue again;
G, deaeration, maturation, filtration
The viscose glue that step D is obtained carries out conventional deaeration, maturation is handled, and carries out filtration treatment according to common process again, and obtaining the ɑ content of cellulose is 9.12%, sodium hydrate content 5.9 %, and viscosity 53 seconds, degree of ripeness (ammonia value) 5.4ml spins preceding viscose.
H, preparation viscose glue mixed solution
The phase-change microcapsule that contains phase-change material that makes among the step B is joined spinning in the preceding viscose of obtaining among the step G, mix the nature dissolving, stirring and making solid content is 9%, and sodium hydrate content is 5.92% the preceding viscose glue mixed solution that spins;
I, filtration
The preceding viscose glue mixed solution that spins that step H is made makes spinning solution through the filtering technique of routine;
J, with spinning solution through conventional spinning, desulfurization, wash, oil and stoving process makes the compound bamboo pulp phase-change microcapsule of product viscose.
Embodiment 9
On the basis of embodiment 5～8, preferred:
The compositely proportional of three kinds of pulps is in described cotton, wood, the compound pulp of bamboo: bamboo: cotton: wood=55:15:10.
In step C, the index of described cotton, wood, the compound pulp of bamboo is: viscosity is that 10mpa.s, methylcellulose content are 93%, content of ashes is 0.01%, irony content is 8ppm, inhale that base number is 530%, swelling capacity is 170%, quantitatively be 770g/m
2, moisture is 10%, whiteness is 83%, reactivity worth is at 9mlCS
2Condition under be 0s.
In step F, demineralized water replaces after by the scrap rubber water thin up after filtering.
In step F, the index of the viscose glue that obtains after described dissolving, the grinding is: the ɑ content of cellulose is 8.5%, and sodium hydrate content is 5%, viscosity 60 seconds, degree of ripeness 6.5ml.
In step G, the aperture that described filtration is adopted is the stainless steel sintering net of 16um.
Be meant that in the spinning described in the step J be 110g/l with spinning solution at sulfuric acid content, sodium sulphate content is 328g/l, and zinc sulfate content is 10g/l, and temperature is a spinning moulding in 48 ℃ the acid bath.
Embodiment 10
On the basis of embodiment 5～8, preferred:
The compositely proportional of three kinds of pulps is in described cotton, wood, the compound pulp of bamboo: bamboo: cotton: wood=75:20:25.
In step C, the index of described cotton, wood, the compound pulp of bamboo is: viscosity is that 12mpa.s, methylcellulose content are 98%, content of ashes is 0.08%, irony content is 14ppm, inhale that base number is 600%, swelling capacity is 210%, is 830 g/m quantitatively
2, moisture is 11.5%, whiteness is 95%, reactivity worth is at 9mlCS
2Condition under be 250s.
In step F, demineralized water replaces after by the scrap rubber water thin up after filtering.
In step F, the index of the viscose glue that obtains after described dissolving, the grinding is: the ɑ content of cellulose is 8.8%, and sodium hydrate content is 5.5%, viscosity 70 seconds, degree of ripeness 7.5ml.
In step G, the aperture that described filtration is adopted is the stainless steel sintering net of 25um.
Be meant that in the spinning described in the step J be 130g/l with spinning solution at sulfuric acid content, sodium sulphate content is 332g/l, and zinc sulfate content is 14g/l, and temperature is a spinning moulding in 52 ℃ the acid bath.
Embodiment 11
On the basis of embodiment 5～8, preferred:
The compositely proportional of three kinds of pulps is in described cotton, wood, the compound pulp of bamboo: bamboo: cotton: wood=65:17.5:17.5.
In step C, the index of described cotton, wood, the compound pulp of bamboo is: viscosity is that 11mpa.s, methylcellulose content are 95.5%, content of ashes is 0.045%, irony content is 11ppm, inhale that base number is 565%, swelling capacity is 190%, quantitatively be 800g/m
2, moisture is 10.75%, whiteness is 89%, reactivity worth is at 9mlCS
2Condition under be 125s.
In step F, demineralized water replaces after by the scrap rubber water thin up after filtering.
In step F, the index of the viscose glue that obtains after described dissolving, the grinding is: the ɑ content of cellulose is 8.65%, and sodium hydrate content is 5.25%, viscosity 65 seconds, degree of ripeness 7ml.
In step G, the aperture that described filtration is adopted is the stainless steel sintering net of 20um.
Be meant that in the spinning described in the step J be 120g/l with spinning solution at sulfuric acid content, sodium sulphate content is 330g/l, and zinc sulfate content is 12g/l, and temperature is a spinning moulding in 50 ℃ the acid bath.
Embodiment 12
On the basis of embodiment 5～8, preferred:
The compositely proportional of three kinds of pulps is in described cotton, wood, the compound pulp of bamboo: bamboo: cotton: wood=58:17:21.
In step C, the index of described cotton, wood, the compound pulp of bamboo is: viscosity is that 10.8mpa.s, methylcellulose content are 97%, content of ashes is 0.055%, irony content is 12ppm, inhale that base number is 571%, swelling capacity is 174%, quantitatively be 789g/m
2, moisture is 11%, whiteness is 90%, reactivity worth is at 9mlCS
2Condition under be 50s.
In step F, demineralized water replaces after by the scrap rubber water thin up after filtering.
In step F, the index of the viscose glue that obtains after described dissolving, the grinding is: the ɑ content of cellulose is 8.7%, and sodium hydrate content is 5.1%, viscosity 69 seconds, degree of ripeness 7.25ml.
In step G, the aperture that described filtration is adopted is the stainless steel sintering net of 19um.
Be meant that in the spinning described in the step J be 128g/l with spinning solution at sulfuric acid content, sodium sulphate content is 329g/l, and zinc sulfate content is 11.5g/l, and temperature is a spinning moulding in 51 ℃ the acid bath.
Embodiment 13
The compound bamboo pulp phase transformation of preparation 1.67dtex*38mm viscose staple fibre:
Use compound bamboo pulp pulp to be raw material, make the 20kg viscose solution through dipping, squeezing, pulverizing, experienced, yellow, dissolving step, wherein methylcellulose content is 9%.
1.2kg phase-change microcapsule emulsion is joined in the 20kg viscose solution; Dissolve, stirring and making solid content is 9.3%, contains alkali and be 5.7% viscose solution; The preceding viscose that spins through filtration, maturation system; Is 120g/l with this spinning solution at sulfuric acid content, and sodium sulphate content is 330g/l, and zinc sulfate content is 12g/l; Temperature is a spinning moulding in 50 ℃ the acid bath, with institute's spinning bar through cut-out, washing, desulfurization, washing, dewater, oil, baking step handles the compound bamboo pulp phase-change microcapsule viscose staple fibre that obtains 1.67dtex*38mm.
Fiber index: do fracture strength: 1.83cN/dtex; Wet breaking strength: 0.85cN/dtex; Dried elongation at break: 16%; Line density deviation :-1.0%; Whiteness: 85%; Oil content: 0.25%; Regain: 13%; Residual sulphur rate: 15mg/100g; Fiber phase-changing and temperature-regulating scope: 25～35 ℃, fiber phase transformation enthalpy △ H:155J/g;
Embodiment 14
The compound bamboo pulp phase-change microcapsule of preparation 2.22dtex*38mm viscose staple fibre:
Use compound bamboo pulp pulp to be raw material, make the 20kg viscose solution through dipping, squeezing, pulverizing, experienced, yellow, dissolving step, wherein methylcellulose content is 9%.
1.2kg phase-change microcapsule emulsion is joined in the 20kg viscose solution; Dissolve, stirring and making solid content is 9.3%, contains alkali and be 5.7% viscose solution; The preceding viscose that spins through filtration, maturation system; Is 120g/l with this spinning solution at sulfuric acid content, and sodium sulphate content is 330g/l, and zinc sulfate content is 12g/l; Temperature is a spinning moulding in 50 ℃ the acid bath, with institute's spinning bar through cut-out, washing, desulfurization, washing, dewater, oil, baking step handles the compound bamboo pulp phase-change microcapsule viscose staple fibre that obtains 1.67dtex*38mm.
Fiber index: do fracture strength: 1.7cN/dtex; Wet breaking strength: 0.75cN/dtex; Dried elongation at break: 15%; Line density deviation :-1.0%; Whiteness: 80%; Oil content: 0.20%; Regain: 12%; Residual sulphur rate: 13mg/100g; Fiber phase-changing and temperature-regulating scope: 25～35 ℃, fiber phase transformation enthalpy △ H:105J/g;
Claims (9)
1. a cotton, wood, the compound pulp phase-change microcapsule of bamboo viscose, it is characterized in that: phase-change microcapsule content is 10～30wt.% in described cotton, wood, the compound pulp phase-change microcapsule of the bamboo viscose staple fibre; Described phase-change microcapsule comprises the raw material components of following parts by weight:
80～250 parts of methyl methacrylates
80～150 parts in phase transformation paraffin
2.5～6 parts of emulsifying agents
0.5～1.5 part of azo initiator
300～400 parts of deionized waters.
2. a kind of cotton according to claim 1, wood, the compound pulp phase-change microcapsule of bamboo viscose is characterized in that: described phase transformation paraffin employing fusing point is 20～30 ℃ a phase transformation paraffin.
3. the preparation method of a kind of cotton according to claim 1, wood, the compound pulp phase-change microcapsule of bamboo viscose is characterized in that: comprise following processing step:
A, preparation paraffin wax emulsion
With 300～400 parts of deionized waters, the paraffin of 80～150 parts of thawings, 2.5～6 parts of emulsifying agents, 0.5～1.5 part of initator mixes, and at 60～70 ℃, rotating speed is that high speed shear emulsification made paraffin wax emulsion in 15～30 minutes under 1500～2000rpm;
B, preparation contain the phase-change microcapsule of phase-change material
80～250 parts of methyl methacrylates being added dropwise in the paraffin wax emulsion of steps A preparation, is 2000～3000rpm at rotating speed, and temperature is 55～65 ℃ reacted 110～130 minutes down, made the phase-change microcapsule that contains phase-change material;
C, alkali steeping
Select cotton, wood, the compound pulp of bamboo as raw material, carry out alkali steeping and handle, the concentration of dipping alkali is 260～280g/L, and dipping temperature is controlled to be 42～44 ℃, and dip time is 75～85 minutes, obtains cellulose sulfonate;
D, experienced
The cellulose sulfonate that steps A is obtained carries out experienced processing, and experienced temperature is controlled to be 40～43 ℃, and ageing time is 90～100 minutes;
E, yellow
The experienced cellulose sulfonate of process that step B is obtained carries out the yellow dissolution process, obtains viscose solution, wherein CS
2Addition be 35～37% of methylcellulose;
F, dissolving
The yellow cellulose processed sulphonic acid ester that passes through that step C is obtained carries out dissolution process, is specially at 8～12 ℃ of following demineralized waters that add fully to dissolve, and the grinding through common process obtains viscose glue again;
G, deaeration, maturation, filtration
The viscose glue that step D is obtained carries out deaeration, maturation is handled, and carries out filtration treatment again, and obtaining the ɑ content of cellulose is 8.9～9.2%, sodium hydrate content 5.5～6 %, and viscosity 45～55 seconds, degree of ripeness 4.5～5.5ml spins preceding viscose;
H, preparation viscose glue mixed solution
The phase-change microcapsule that contains phase-change material that makes among the step B is joined spinning in the preceding viscose of obtaining among the step G; Mix the nature dissolving; Stirring and making solid content is 8.5～9.3%, and sodium hydrate content is 5.7～6.3% the preceding viscose glue mixed solution that spins;
I, filtration
The preceding viscose glue mixed solution that spins that step H is made makes spinning solution through the filtering technique of routine;
J, with spinning solution through conventional spinning, desulfurization, wash, oil and stoving process makes the compound bamboo pulp phase-change microcapsule of product viscose.
4. the preparation method of a kind of cotton according to claim 3, wood, the compound pulp phase-change microcapsule of bamboo viscose is characterized in that: the compositely proportional of three kinds of pulps is in described cotton, wood, the compound pulp of bamboo: bamboo: cotton: wood=55～75:15～20:10～25.
5. the preparation method of a kind of cotton according to claim 3, wood, the compound pulp phase-change microcapsule of bamboo viscose; It is characterized in that: in step C; The index of described cotton, wood, the compound pulp of bamboo can be any index of compound pulp standard on the market, and its preferred index is: viscosity is 10～12mpa.s, methylcellulose content for>=93%, content of ashes for≤0.08%, irony content for≤14ppm, inhale that base number is 530～600%, swelling capacity is 170～210%, is 770～830 g/m quantitatively
2, moisture is 10～11.5%, whiteness for>=83%, reactivity worth is at 9mlCS
2Condition under be 0～250s.
6. the preparation method of a kind of cotton according to claim 3, wood, the compound pulp phase-change microcapsule of bamboo viscose is characterized in that: in step F, demineralized water replaces after by the scrap rubber water thin up after filtering.
7. the preparation method of a kind of cotton according to claim 3, wood, the compound pulp phase-change microcapsule of bamboo viscose; It is characterized in that: in step F; The index of the viscose glue that obtains after described dissolving, the grinding is: the ɑ content of cellulose is 8.5～8.8%; Sodium hydrate content is 5～5.5%, viscosity 60～70 seconds, degree of ripeness 6.5～7.5ml.
8. the preparation method of a kind of cotton according to claim 3, wood, the compound pulp phase-change microcapsule of bamboo viscose is characterized in that: in step G, the aperture that described filtration is adopted is the stainless steel sintering net of 16～25um.
9. the preparation method of a kind of cotton according to claim 3, wood, the compound pulp phase-change microcapsule of bamboo viscose; It is characterized in that: be meant that in the spinning described in the step J be 110～130g/l with spinning solution at sulfuric acid content; Sodium sulphate content is 328～332g/l; Zinc sulfate content is 10～14g/l, and temperature is a spinning moulding in 48～52 ℃ the acid bath.
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| CN104389039A (en) * | 2014-11-06 | 2015-03-04 | 龙达（江西）差别化化学纤维有限公司 | Method for producing temperature-regulating viscose fibers |
| CN104947214A (en) * | 2015-07-14 | 2015-09-30 | 爱谱诗（苏州）服装有限公司 | Manufacture process for automatically temperature-adjustable fiber fabric |
| CN105951261B (en) * | 2016-06-12 | 2019-07-02 | 合肥市再德高分子材料有限公司 | A kind of fabric lining with heat-accumulation temperature-adjustment function |
| CN105951261A (en) * | 2016-06-12 | 2016-09-21 | 合肥市再德高分子材料有限公司 | Fiber fabric with heat storage and temperature adjusting functions |
| CN107354527B (en) * | 2017-08-14 | 2019-10-18 | 恒天海龙（潍坊）新材料有限责任公司 | A kind of preparation method of speed heat warm-keeping cellulose fiber |
| CN107354527A (en) * | 2017-08-14 | 2017-11-17 | 恒天海龙（潍坊）新材料有限责任公司 | A kind of preparation method of speed heat warm-keeping cellulose fiber |
| CN111074366A (en) * | 2019-12-25 | 2020-04-28 | 宜宾海丝特纤维有限责任公司 | Phase-change energy-storage viscose fiber and production process thereof |
| CN111455487A (en) * | 2020-04-27 | 2020-07-28 | 宁波市纤维检验所 | Phase-change temperature-regulating fiber and preparation method thereof |
| CN111676536A (en) * | 2020-06-05 | 2020-09-18 | 西安工程大学 | Preparation method of temperature-adjusting microcapsule and graphene compounded viscose fiber |
| CN112251864A (en) * | 2020-09-25 | 2021-01-22 | 江西金源纺织有限公司 | Wear-resistant improved viscose composite yarn and preparation method thereof |
| CN112251864B (en) * | 2020-09-25 | 2022-06-07 | 江西金源纺织有限公司 | Wear-resistant improved viscose composite yarn and preparation method thereof |
| CN113089119A (en) * | 2021-05-19 | 2021-07-09 | 冯杰宝 | Regenerated cellulose fiber containing sea cucumber protein and preparation method thereof |
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