CN102839440B - 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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- CN102839440B CN102839440B CN201210357126.5A CN201210357126A CN102839440B CN 102839440 B CN102839440 B CN 102839440B CN 201210357126 A CN201210357126 A CN 201210357126A CN 102839440 B CN102839440 B CN 102839440B
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- 239000000243 solution Substances 0.000 claims description 38
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- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 29
- 239000012782 phase change material Substances 0.000 claims description 28
- 238000012545 processing Methods 0.000 claims description 25
- 238000007598 dipping method Methods 0.000 claims description 22
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- 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
- 239000002994 raw material Substances 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 12
- 239000003643 water by type Substances 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
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- 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
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
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- 235000002918 Fraxinus excelsior Nutrition 0.000 claims description 6
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- 229920001214 Polysorbate 60 Polymers 0.000 claims description 2
- 150000004996 alkyl benzenes Chemical group 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 claims description 2
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 claims description 2
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- 230000006870 function Effects 0.000 description 7
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 6
- 238000009825 accumulation Methods 0.000 description 6
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- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-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
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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, bamboo compound pulp phase-change microcapsule 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 extracting from the bamboo of self-sow, bamboo is by 40%～50% cellulose, 30% pentosan and 20%～25% lignin form, wherein topmost part is cellulose, can be purified or be regenerated by the processing to bamboo to make corresponding fiber.
The functional fiber with heat-accumulation temperature-adjustment function is a developing field of current industry production research and development, because having heat-accumulation temperature-adjustment function, fiber will more and more be subject to popular favor from now on, market prospects are wide, and most domestic viscose manufacturer has carried out one after another a series of research and development for thermo-regulated fiber and obtained a large amount of achievements at present.
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, described intellectual and temperature-adjusting viscose is in 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 in bone dry fiber, phase-change material micro-capsule content is 2-25%; Water content is 7-15%; Oil content is 0.15-0.30%; This fiber is when having inherited viscose good characteristic, there is significant accumulation of heat, heat release bidirectional temp regulation function, it solidifies heat release enthalpy Δ H >=2.5J/g, and melting heat absorption enthalpy Δ H >=2.5J/g, can be widely used in the 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-adaptable bamboo pulp fibers and preparation method thereof ", and this invention provides a kind of temperature-adaptable bamboo pulp fibers.The present invention also provides a kind of preparation method of temperature-adaptable bamboo pulp fibers, comprising: it is 1%～20% phase-change microcapsule colloidal solution that mass concentration is provided; Bamboo cellulose pulp, after dipping, squeezing and pulverization process, is obtained to alkali cellulose; By described alkali cellulose successively after experienced operation, yellow operation, dissolution process, mixed processes, deaeration operation, filter progress, spinning process and postprocessing working procedures, obtain temperature-adaptable bamboo pulp fibers, when carrying out yellow operation, dissolution process, mixed processes or spinning process, in material, add described phase-change microcapsule colloidal solution, yellow operation comprises the following steps: to adding alkali lye to alkalize through in the alkali cellulose of experienced operation, alkalization temperature is 15 ℃～25 ℃; Alkalization finish front 10min～15min by alkali cellulose temperature adjustment to yellow reaction temperature, alkalization finishes to add carbon disulfide to carry out yellow in backward described alkali cellulose.
The phase-change material micro-capsule that above-mentioned patent adopts is that to take the macromolecular compound composite membranes such as urea aldehyde, polyureas, epoxy resin, polyester, polystyrene be wall material, take the microcapsules that phase-change material, heat memory material or plastic crystals material make as core, the Microcapsules Size of preparing and latent heat of phase change differ larger.
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 " a kind of preparation method of phase-change material of microcapsule coated ", this invention relates to a kind of preparation method of phase-change material of microcapsule coated, 1. presses paraffin: 1: 3 feeding of mass ratio of methyl methacrylate; 2. by 0.5% of gross mass in 1, take Ethylene glycol dimethacrylate, 1% methacrylic acid, 1% lauryl sodium sulfate, 1.5% potassium peroxydisulfate, 1% ~ 15% ferrite, 400% deionized water; 3. lauryl sodium sulfate is joined in deionized water, be heated to 50 ℃; 4. the paraffin of ferrite and thawing is added in 3 solution; 5. ultrasonic emulsification, adds methyl methacrylate, Ethylene glycol dimethacrylate and methacrylic acid; 6. emulsification again, moves into the solution obtaining to have in the device of mechanical agitation, condenser pipe, air inlet and charge door; 7. ventilation deoxygenation is 0.5 hour, and heating water bath to 70 ℃, adds potassium peroxydisulfate, is down to room temperature, obtains the phase-change material of microcapsule coated.For fields such as building, heat-accumulation temperature-adjustment weaving and electronic equipments.
The phase-change material formula of the microcapsule coated in above-mentioned patent and preparation method are very complicated, material is difficult to buy, preparation time is long, emulsifying manner is ultrasonic emulsification, and complicated operation is wayward, cost and security risk are high, and the microcapsules granularity preparing is inhomogeneous, is not suitable for the production of compound pulp viscose, very large on viscose quality and spinnability impact.
Summary of the invention
The phase-change material formula and the preparation method that the object of the invention is to solve microcapsule coated of the prior art are very complicated, the microcapsules granularity obtaining is inhomogeneous, be not suitable for the production of composite viscose fiber, to viscose quality and the far-reaching problem of spinnability, a kind of cotton is provided, wood, bamboo compound pulp phase-change microcapsule viscose, greatly simplify and optimized the formula of microcapsules, and the microcapsules epigranular obtaining, be applicable to the production of compound pulp viscose, can significantly improve viscose quality and spinnability, the viscose making not only has composite bamboo pulp fibres natural moisture preserving and permeation functions, and there is the function of heat-accumulation temperature-adjustment.
Another object of the present invention is to provide the preparation method through optimizing and simplifying of above-mentioned cotton, wood, bamboo compound pulp phase-change microcapsule viscose, making whole technical process be easy to control, cost and security risk reduces, and solved in existing production adhering process, the dipping effect of pulp is bad, the alkali cellulose generating is inhomogeneous, and fall too much poly-, can cause the cellulose sulfonate viscosity of generation low, it is poor to filter, it is powerful low that the finished fiber generating shows, the problem that spinnability is poor.
In order to realize foregoing invention object, concrete technical scheme of the present invention is as follows:
Cotton, wood, a bamboo compound pulp phase-change microcapsule viscose, is characterized in that: in described cotton, wood, bamboo compound pulp phase-change microcapsule viscose staple fibre, phase-change microcapsule content is 10～30wt.%; Described phase-change microcapsule comprises the raw material components of following parts by weight:
80～250 parts of methyl methacrylates
80～150 parts of phase change paraffins
2.5～6 parts of emulsifying agents
0.5～1.5 part of azo initiator
300～400 parts of deionized waters.
Phase change paraffin of the present invention is preferred, and employing fusing point is the phase change paraffin of 20～30 ℃.
Emulsifying agent of the present invention is the emulsifying agent of this area routine, preferably: alkyl benzene sulphonate sodium salt, polysorbate60, Tween 80, this class 60 or this class 80.
A preparation method for cotton, wood, bamboo compound pulp phase-change microcapsule viscose, is characterized in that: comprise following processing step:
A, prepare paraffin wax emulsion
By 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 under 1500～2000rpm, high speed shear emulsification makes paraffin wax emulsion for 15～30 minutes;
The phase-change microcapsule that B, preparation contain phase-change material
80～250 parts of methyl methacrylates are added dropwise in paraffin wax emulsion prepared by steps A, are 2000～3000rpm at rotating speed, and temperature is at 55～65 ℃, to react 110～130 minutes, makes the phase-change microcapsule that contains phase-change material;
C, alkali steeping
Select cotton, wood, bamboo compound pulp as raw material, carry out alkali steeping processing, the concentration of dipping alkali is 260～280g/L, and it is 42～44 ℃ that dipping temperature is controlled, 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 it is 40～43 ℃ that experienced temperature is controlled, and ageing time is 90～100 minutes;
E, yellow
The experienced cellulose sulfonate of process that step B is obtained carries out yellow dissolution process, obtains viscose solution, wherein CS
2addition be methylcellulose 35～37%;
F, dissolving
The cellulose sulfonate of processing through yellow that step C is obtained carries out dissolution process, is specially at 8～12 ℃ and adds demineralized water fully to dissolve, then obtain viscose glue by the grinding of common process;
G, deaeration, maturation, filtration
The viscose glue that step D is obtained carries out conventional deaeration, maturation is processed, according to common process, carry out filtration treatment again, obtaining 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 front viscose.
H, Making viscose mixed solution
The phase-change microcapsule that contains phase-change material making in step B is joined to spinning in front viscose of obtaining in step G, mixing nature dissolves, stirring and making solid content is 8.5～9.3%, and sodium hydrate content is 5.7～6.3% spins front viscose glue mixed solution;
I, filtration
The front viscose glue mixed solution that spins that step H is made makes spinning solution through conventional filtering technique;
J, by 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 B, be phase-change material phase change paraffin, wall material is free yl polymerizating monomer methyl methacrylate.
Described cotton, wood, bamboo compound pulp can be to buy on market, also can be according to the preparation of existing this area common process, and wherein compositely proportional cotton, wooden, bamboo can be arbitrary proportion.
In above-mentioned cotton, wood, bamboo compound pulp, the compositely proportional of three kinds of pulps is preferably:
Bamboo: cotton: wood=55～75:15～20:10～25.It adopts common process to make compound pulp.
In step C, the index of described cotton, wood, bamboo compound pulp can be any index of compound pulp standard on 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 quantitatively 770～830 g/m
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 after the scrap rubber water thin up after filtering, and the index of the viscose glue obtaining after dissolving, grinding is: 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 stainless steel sintered meshwork that the aperture that described filtration adopts is 16～25um.
In the spinning described in step J, refer to that be 110～130g/l by spinning solution at sulfuric acid content, sodium sulphate content is 328～332g/l, and zinc sulfate content is 10～14g/l, and temperature is spinning moulding in the acid bath of 48～52 ℃.
The useful technique effect that the present invention brings:
1, the present invention simplifies and optimizes on the basis of the phase-change microcapsule formula of existing composite bamboo pulp phase-change microcapsule viscose, the microcapsules epigranular obtaining, be applicable to the production of composite viscose fiber, little on viscose quality and spinnability impact, can significantly improve viscose quality and spinnability, the viscose making not only has composite bamboo pulp fibres natural moisture preserving and permeation functions, and has the function of heat-accumulation temperature-adjustment;
2, the present invention is optimized and improves on existing basis of preparing composite bamboo pulp phase-change microcapsule viscose technique, mainly contains following advantage:
1) in alkali steeping, dipping alkali concn, dipping temperature and dip time that the present invention selects cooperatively interact, and are conducive to cellulosic swelling, improve dipping effect, guarantee that cotton, wood pulps are after adding bamboo pulp, the esterification degree of the cellulose sulfonate obtaining through dipping is 50～60%; The crosslinking time of composite bamboo pulp bamboo pulp and NaOH in minutes just can complete, but pulp progressively reaches uniform degree to fibrous inside infiltration and needs certain hour from soaking alkali lye, the stripping of hemicellulose element needs the more time, dip time is longer, hemicellulose stripping is more abundant, its dissolution rate declines along with the increase of hemicellulose concentration in solution, finally reach dynamic equilibrium, adopt alkali steeping parameter of the present invention can make whole cotton, wood, bamboo compound pulp system reach dynamic equilibrium; And its dipping temperature can make follow-up yellow reaction more even;
2) in experienced, in cotton, wood, bamboo compound pulp, its degree of polymerization is separately different, and alkali cellulose falls poly-less when experienced in process of production, adopt experienced temperature of the present invention and ageing time to control, can obtain the narrower cellulose of molecular weight distribution, make in subsequent production process, the viscose riscosity making is higher, have good uniformity, greatly improve the degree of polymerization, thereby in spinning process, can improve the tensile property of as-spun fibre, ready for improving plasticizing drawing-off;
3) in yellow, the selection of the addition of carbon disulfide can prevent fully yellow of alkali cellulose, makes the dissolving of cellulose sulfonate and the filter process of viscose glue more smooth, can not cause milky white fiber simultaneously, has reduced unit consumption and pollution;
4) in cotton of the present invention, wood, bamboo compound pulp, the compositely proportional of three kinds of pulps is: bamboo: cotton: wood=55～75:15～20:10～25, improved the stability of pulp, can not affect the processing parameter of subsequent handling, and can better bring into play the natural antibacterial of bamboo pulp, can better evade again bamboo pulp and be difficult to determining of reaction;
5) dissolved water demineralized water of the present invention can so both guarantee the dissolving of cellulose sulfonate with the solution after the scrap rubber thin up after filtering, and has avoided again the exhaust emission environment of scrap rubber;
6) the stainless steel sintered meshwork that the aperture that filtration of the present invention preferably adopts is 16～25um, has been controlled at a best filter area, can reduce the loss of viscose glue, reduces cost, and is beneficial to environmental protection;
7) optimization of process of the present invention and technological parameter is an indivisible and integral body independently, the optimization of each technological parameter cooperatively interacts, make the dipping effect of compound pulp better, the alkali cellulose generating 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 generating is now powerful low, the problem that spinnability is poor.
The specific embodiment
embodiment 1
Cotton, wood, a bamboo compound pulp phase-change microcapsule viscose, in described cotton, wood, bamboo compound pulp phase-change microcapsule viscose staple fibre, phase-change microcapsule content is 10wt.%; Described phase-change microcapsule comprises the raw material components of following parts by weight:
80 parts of methyl methacrylates
80 parts of phase change paraffins
2.5 parts of emulsifying agents
0.5 part of azo initiator
300 parts of deionized waters.
Preferably, described phase change paraffin employing fusing point is the phase change paraffin of 20 ℃.
embodiment 2
Cotton, wood, a bamboo compound pulp phase-change microcapsule viscose, in described cotton, wood, bamboo compound pulp phase-change microcapsule viscose staple fibre, phase-change microcapsule content is 30wt.%; Described phase-change microcapsule comprises the raw material components of following parts by weight:
250 parts of methyl methacrylates
150 parts of phase change paraffins
6 parts of emulsifying agents
1.5 parts of azo initiators
400 parts of deionized waters.
Preferably, described phase change paraffin employing fusing point is the phase change paraffin of 30 ℃.
embodiment 3
Cotton, wood, a bamboo compound pulp phase-change microcapsule viscose, in described cotton, wood, bamboo compound pulp phase-change microcapsule viscose staple fibre, phase-change microcapsule content is 20wt.%; Described phase-change microcapsule comprises the raw material components of following parts by weight:
165 parts of methyl methacrylates
115 parts of phase change paraffins
4.25 parts of emulsifying agents
1 part of azo initiator
350 parts of deionized waters.
Preferably, described phase change paraffin employing fusing point is the phase change paraffin of 25 ℃.
embodiment 4
Cotton, wood, a bamboo compound pulp phase-change microcapsule viscose, in described cotton, wood, bamboo compound pulp phase-change microcapsule viscose staple fibre, phase-change microcapsule content is 17wt.%; Described phase-change microcapsule comprises the raw material components of following parts by weight:
200 parts of methyl methacrylates
99 parts of phase change paraffins
5.1 parts of emulsifying agents
0.88 part of azo initiator
395 parts of deionized waters.
Preferably, described phase change paraffin employing fusing point is the phase change paraffin of 28 ℃.
embodiment 5
A preparation method for cotton, wood, bamboo compound pulp phase-change microcapsule viscose, comprises following processing step:
A, prepare paraffin wax emulsion
By 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 under 1500rpm, high speed shear emulsification makes paraffin wax emulsion for 15 minutes;
The phase-change microcapsule that B, preparation contain phase-change material
80～250 parts of methyl methacrylates are added dropwise in paraffin wax emulsion prepared by steps A, are 2000rpm at rotating speed, and temperature is at 55 ℃, to react 110 minutes, makes the phase-change microcapsule that contains phase-change material;
C, alkali steeping
Select cotton, wood, bamboo compound pulp as raw material, carry out alkali steeping processing, the concentration of dipping alkali is 260g/L, and it is 42 ℃ that dipping temperature is controlled, and dip time is 75 minutes, obtains cellulose sulfonate;
D, experienced
The cellulose sulfonate that steps A is obtained carries out experienced processing, and it is 40 ℃ that experienced temperature is controlled, and ageing time is 90 minutes;
E, yellow
The experienced cellulose sulfonate of process that step B is obtained carries out yellow dissolution process, obtains viscose solution, wherein CS
2addition be methylcellulose 35%;
F, dissolving
The cellulose sulfonate of processing through yellow that step C is obtained carries out dissolution process, is specially at 8 ℃ and adds demineralized water fully to dissolve, then obtain viscose glue by the grinding of common process;
G, deaeration, maturation, filtration
The viscose glue that step D is obtained carries out conventional deaeration, maturation to be processed, then carries out filtration treatment according to common process, and obtaining ɑ content of cellulose is 8.9%, sodium hydrate content 5.5%, and viscosity 45 seconds, degree of ripeness (ammonia value) 4.5ml spins front viscose.
H, Making viscose mixed solution
The phase-change microcapsule that contains phase-change material making in step B is joined to spinning in front viscose of obtaining in step G, mix nature and dissolve, stirring and making solid content is 8.5%, and sodium hydrate content is 5.7% spins front viscose glue mixed solution;
I, filtration
The front viscose glue mixed solution that spins that step H is made makes spinning solution through conventional filtering technique;
J, by spinning solution through conventional spinning, desulfurization, wash, oil and stoving process makes the compound bamboo pulp phase-change microcapsule of product viscose.
embodiment 6
A preparation method for cotton, wood, bamboo compound pulp phase-change microcapsule viscose, comprises following processing step:
A, prepare paraffin wax emulsion
By 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 under 2000rpm, high speed shear emulsification makes paraffin wax emulsion for 30 minutes;
The phase-change microcapsule that B, preparation contain phase-change material
80～250 parts of methyl methacrylates are added dropwise in paraffin wax emulsion prepared by steps A, are 3000rpm at rotating speed, and temperature is at 65 ℃, to react 130 minutes, makes the phase-change microcapsule that contains phase-change material;
C, alkali steeping
Select cotton, wood, bamboo compound pulp as raw material, carry out alkali steeping processing, the concentration of dipping alkali is 280g/L, and it is 44 ℃ that dipping temperature is controlled, and dip time is 85 minutes, obtains cellulose sulfonate;
D, experienced
The cellulose sulfonate that steps A is obtained carries out experienced processing, and it is 43 ℃ that experienced temperature is controlled, and ageing time is 100 minutes;
E, yellow
The experienced cellulose sulfonate of process that step B is obtained carries out yellow dissolution process, obtains viscose solution, wherein CS
2addition be methylcellulose 37%;
F, dissolving
The cellulose sulfonate of processing through yellow that step C is obtained carries out dissolution process, is specially at 12 ℃ and adds demineralized water fully to dissolve, then obtain viscose glue by the grinding of common process;
G, deaeration, maturation, filtration
The viscose glue that step D is obtained carries out conventional deaeration, maturation to be processed, then carries out filtration treatment according to common process, and obtaining ɑ content of cellulose is 9.2%, sodium hydrate content 6%, and viscosity 55 seconds, degree of ripeness (ammonia value) 5.5ml spins front viscose.
H, Making viscose mixed solution
The phase-change microcapsule that contains phase-change material making in step B is joined to spinning in front viscose of obtaining in step G, mix nature and dissolve, stirring and making solid content is 9.3%, and sodium hydrate content is 6.3% spins front viscose glue mixed solution;
I, filtration
The front viscose glue mixed solution that spins that step H is made makes spinning solution through conventional filtering technique;
J, by spinning solution through conventional spinning, desulfurization, wash, oil and stoving process makes the compound bamboo pulp phase-change microcapsule of product viscose.
embodiment 7
A preparation method for cotton, wood, bamboo compound pulp phase-change microcapsule viscose, comprises following processing step:
A, prepare paraffin wax emulsion
By 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 under 1750rpm, high speed shear emulsification makes paraffin wax emulsion for 22.5 minutes;
The phase-change microcapsule that B, preparation contain phase-change material
80～250 parts of methyl methacrylates are added dropwise in paraffin wax emulsion prepared by steps A, are 2500rpm at rotating speed, and temperature is at 60 ℃, to react 120 minutes, makes the phase-change microcapsule that contains phase-change material;
C, alkali steeping
Select cotton, wood, bamboo compound pulp as raw material, carry out alkali steeping processing, the concentration of dipping alkali is 270g/L, and it is 43 ℃ that dipping temperature is controlled, and dip time is 80 minutes, obtains cellulose sulfonate;
D, experienced
The cellulose sulfonate that steps A is obtained carries out experienced processing, and it is 41.5 ℃ that experienced temperature is controlled, and ageing time is 95 minutes;
E, yellow
The experienced cellulose sulfonate of process that step B is obtained carries out yellow dissolution process, obtains viscose solution, wherein CS
2addition be methylcellulose 36%;
F, dissolving
The cellulose sulfonate of processing through yellow that step C is obtained carries out dissolution process, is specially at 10 ℃ and adds demineralized water fully to dissolve, then obtain viscose glue by the grinding of common process;
G, deaeration, maturation, filtration
The viscose glue that step D is obtained carries out conventional deaeration, maturation to be processed, then carries out filtration treatment according to common process, and obtaining ɑ content of cellulose is 9.05%, sodium hydrate content 5.75%, and viscosity 50 seconds, degree of ripeness (ammonia value) 5ml spins front viscose.
H, Making viscose mixed solution
The phase-change microcapsule that contains phase-change material making in step B is joined to spinning in front viscose of obtaining in step G, mixing nature dissolves, stirring and making solid content is 8.5～9.3%, and sodium hydrate content is 5.7～6.3% spins front viscose glue mixed solution;
I, filtration
The front viscose glue mixed solution that spins that step H is made makes spinning solution through conventional filtering technique;
J, by spinning solution through conventional spinning, desulfurization, wash, oil and stoving process makes the compound bamboo pulp phase-change microcapsule of product viscose.
embodiment 8
A preparation method for cotton, wood, bamboo compound pulp phase-change microcapsule viscose, comprises following processing step:
A, prepare paraffin wax emulsion
By 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 under 1600rpm, high speed shear emulsification makes paraffin wax emulsion for 28 minutes;
The phase-change microcapsule that B, preparation contain phase-change material
80～250 parts of methyl methacrylates are added dropwise in paraffin wax emulsion prepared by steps A, are 2900rpm at rotating speed, and temperature is at 57 ℃, to react 128 minutes, makes the phase-change microcapsule that contains phase-change material;
C, alkali steeping
Select cotton, wood, bamboo compound pulp as raw material, carry out alkali steeping processing, the concentration of dipping alkali is 262g/L, and it is 43.6 ℃ that dipping temperature is controlled, and dip time is 79 minutes, obtains cellulose sulfonate;
D, experienced
The cellulose sulfonate that steps A is obtained carries out experienced processing, and it is 42 ℃ that experienced temperature is controlled, and ageing time is 97 minutes;
E, yellow
The experienced cellulose sulfonate of process that step B is obtained carries out yellow dissolution process, obtains viscose solution, wherein CS
2addition be methylcellulose 35.2%;
F, dissolving
The cellulose sulfonate of processing through yellow that step C is obtained carries out dissolution process, is specially at 9 ℃ and adds demineralized water fully to dissolve, then obtain viscose glue by the grinding of common process;
G, deaeration, maturation, filtration
The viscose glue that step D is obtained carries out conventional deaeration, maturation to be processed, then carries out filtration treatment according to common process, and obtaining ɑ content of cellulose is 9.12%, sodium hydrate content 5.9 %, and viscosity 53 seconds, degree of ripeness (ammonia value) 5.4ml spins front viscose.
H, Making viscose mixed solution
The phase-change microcapsule that contains phase-change material making in step B is joined to spinning in front viscose of obtaining in step G, mix nature and dissolve, stirring and making solid content is 9%, and sodium hydrate content is 5.92% spins front viscose glue mixed solution;
I, filtration
The front viscose glue mixed solution that spins that step H is made makes spinning solution through conventional filtering technique;
J, by 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:
In described cotton, wood, bamboo compound pulp, the compositely proportional of three kinds of pulps is: bamboo: cotton: wood=55:15:10.
In step C, the index of described cotton, wood, bamboo compound pulp 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%, is quantitatively 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 obtaining after described dissolving, grinding is: 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 stainless steel sintered meshwork that the aperture that described filtration adopts is 16um.
In the spinning described in step J, refer to that be 110g/l by spinning solution at sulfuric acid content, sodium sulphate content is 328g/l, and zinc sulfate content is 10g/l, and temperature is spinning moulding in the acid bath of 48 ℃.
embodiment 10
On the basis of embodiment 5～8, preferred:
In described cotton, wood, bamboo compound pulp, the compositely proportional of three kinds of pulps is: bamboo: cotton: wood=75:20:25.
In step C, the index of described cotton, wood, bamboo compound pulp 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 quantitatively 830 g/m
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 obtaining after described dissolving, grinding is: 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 stainless steel sintered meshwork that the aperture that described filtration adopts is 25um.
In the spinning described in step J, refer to that be 130g/l by spinning solution at sulfuric acid content, sodium sulphate content is 332g/l, and zinc sulfate content is 14g/l, and temperature is spinning moulding in the acid bath of 52 ℃.
embodiment 11
On the basis of embodiment 5～8, preferred:
In described cotton, wood, bamboo compound pulp, the compositely proportional of three kinds of pulps is: bamboo: cotton: wood=65:17.5:17.5.
In step C, the index of described cotton, wood, bamboo compound pulp 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%, is quantitatively 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 obtaining after described dissolving, grinding is: 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 stainless steel sintered meshwork that the aperture that described filtration adopts is 20um.
In the spinning described in step J, refer to that be 120g/l by spinning solution at sulfuric acid content, sodium sulphate content is 330g/l, and zinc sulfate content is 12g/l, and temperature is spinning moulding in the acid bath of 50 ℃.
embodiment 12
On the basis of embodiment 5～8, preferred:
In described cotton, wood, bamboo compound pulp, the compositely proportional of three kinds of pulps is: bamboo: cotton: wood=58:17:21.
In step C, the index of described cotton, wood, bamboo compound pulp 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%, is quantitatively 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 obtaining after described dissolving, grinding is: 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 stainless steel sintered meshwork that the aperture that described filtration adopts is 19um.
In the spinning described in step J, refer to that be 128g/l by spinning solution at sulfuric acid content, sodium sulphate content is 329g/l, and zinc sulfate content is 11.5g/l, and temperature is spinning moulding in the acid bath of 51 ℃.
embodiment 13
The compound bamboo pulp phase transformation of preparation 1.67dtex*38mm viscose staple fibre:
With compound bamboo pulp pulp, be raw material, by dipping, squeezing, pulverizing, experienced, yellow, dissolving step, make 20kg viscose solution, wherein methylcellulose content is 9%.
1.2kg phase-change microcapsule emulsion is joined in 20kg viscose solution, dissolve, stirring and making solid content is 9.3%, the viscose solution that is 5.7% containing alkali, after filtration, maturation system spins front viscose, by this spinning solution, at sulfuric acid content, be 120g/l, sodium sulphate content is 330g/l, zinc sulfate content is 12g/l, temperature is spinning moulding in the acid bath of 50 ℃, by institute's spinning bar through cut-out, washing, desulfurization, washing, dewater, oil, baking step processes the compound bamboo pulp phase-change microcapsule viscose staple fibre that obtains 1.67dtex*38mm.
Fiber index: dry fracture strength: 1.83cN/dtex; Wet breaking strength: 0.85cN/dtex; Dry 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:
With compound bamboo pulp pulp, be raw material, by dipping, squeezing, pulverizing, experienced, yellow, dissolving step, make 20kg viscose solution, wherein methylcellulose content is 9%.
1.2kg phase-change microcapsule emulsion is joined in 20kg viscose solution, dissolve, stirring and making solid content is 9.3%, the viscose solution that is 5.7% containing alkali, after filtration, maturation system spins front viscose, by this spinning solution, at sulfuric acid content, be 120g/l, sodium sulphate content is 330g/l, zinc sulfate content is 12g/l, temperature is spinning moulding in the acid bath of 50 ℃, by institute's spinning bar through cut-out, washing, desulfurization, washing, dewater, oil, baking step processes the compound bamboo pulp phase-change microcapsule viscose staple fibre that obtains 1.67dtex*38mm.
Fiber index: dry fracture strength: 1.7cN/dtex; Wet breaking strength: 0.75cN/dtex; Dry 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 (6)
1. cotton, wood, a bamboo compound pulp phase-change microcapsule viscose, is characterized in that: in described cotton, wood, bamboo compound pulp phase-change microcapsule viscose staple fibre, phase-change microcapsule content is 10～30wt.%; Described phase-change microcapsule comprises the raw material components of following parts by weight:
80～250 parts of methyl methacrylates
80～150 parts of phase change paraffins
2.5～6 parts of emulsifying agents
0.5～1.5 part of azo initiator
300～400 parts of deionized waters;
Described phase change paraffin employing fusing point is the phase change paraffin of 20～30 ℃;
Described emulsifying agent is alkyl benzene sulphonate sodium salt, polysorbate60, Tween 80, this class 60 or this class 80;
Described cotton, wood, bamboo compound pulp phase-change microcapsule viscose are made by following methods:
A, prepare paraffin wax emulsion
By 300～400 parts of deionized waters, the paraffin of 80～150 parts of fusings, 2.5～6 parts of emulsifying agents, 0.5～1.5 part of initator mixes, and at 60～70 ℃, rotating speed is that under 1500～2000rpm, high speed shear emulsification makes paraffin wax emulsion for 15～30 minutes;
The phase-change microcapsule that B, preparation contain phase-change material
80～250 parts of methyl methacrylates are added dropwise in paraffin wax emulsion prepared by steps A, are 2000～3000rpm at rotating speed, and temperature is at 55～65 ℃, to react 110～130 minutes, makes the phase-change microcapsule that contains phase-change material;
C, alkali steeping
Select cotton, wood, bamboo compound pulp as raw material, carry out alkali steeping processing, the concentration of dipping alkali is 260～280g/L, and it is 42～44 ℃ that dipping temperature is controlled, and dip time is 75～85 minutes, obtains cellulose sulfonate; In described cotton, wood, bamboo compound pulp, the compositely proportional of three kinds of pulps is: bamboo: cotton: wood=55～75:15～20:10～25;
D, experienced
The cellulose sulfonate that step C is obtained carries out experienced processing, and it is 40～43 ℃ that experienced temperature is controlled, and ageing time is 90～100 minutes;
E, yellow
The experienced cellulose sulfonate of process that step D is obtained carries out yellow dissolution process, obtains viscose solution, wherein CS
2addition be methylcellulose 35～37%;
F, dissolving
The cellulose sulfonate of processing through yellow that step e is obtained carries out dissolution process, is specially at 8～12 ℃ and adds demineralized water fully to dissolve, then obtain viscose glue by the grinding of common process;
G, deaeration, maturation, filtration
The viscose glue that step F is obtained carries out deaeration, maturation to be processed, then carries out filtration treatment, and obtaining 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 front viscose;
H, Making viscose mixed solution
The phase-change microcapsule that contains phase-change material making in step B is joined to spinning in front viscose of obtaining in step G, mixing nature dissolves, stirring and making solid content is 8.5～9.3%, and sodium hydrate content is 5.7～6.3% spins front viscose glue mixed solution;
I, filtration
The front viscose glue mixed solution that spins that step H is made makes spinning solution through conventional filtering technique;
J, by spinning solution through conventional spinning, desulfurization, wash, oil and stoving process makes the compound bamboo pulp phase-change microcapsule of product viscose.
2. a kind of cotton according to claim 1, wood, bamboo compound pulp phase-change microcapsule viscose, it is characterized in that: in step C, the index of described cotton, wood, bamboo compound pulp 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 quantitatively 770～830 g/m
2, moisture is 10～11.5%, whiteness for>=83%, reactivity worth is at 9mLCS
2condition under be 0～250s.
3. a kind of cotton according to claim 1, wood, bamboo compound pulp phase-change microcapsule viscose, is characterized in that: in step F, demineralized water replaces after by the scrap rubber water thin up after filtering.
4. a kind of cotton according to claim 1, wood, bamboo compound pulp phase-change microcapsule viscose, it is characterized in that: in step F, the index of the viscose glue obtaining after described dissolving, grinding is: 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.
5. a kind of cotton according to claim 1, wood, bamboo compound pulp phase-change microcapsule viscose, is characterized in that: in step G, the aperture that described filtration adopts is the stainless steel sintered meshwork of 16～25 μ m.
6. a kind of cotton according to claim 1, wood, bamboo compound pulp phase-change microcapsule viscose, it is characterized in that: in the spinning described in step J, refer to that be 110～130g/L by spinning solution at sulfuric acid content, sodium sulphate content is 328～332g/L, zinc sulfate content is 10～14g/L, and temperature is spinning moulding in the acid bath of 48～52 ℃.
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| CN103074695B (en) * | 2013-01-28 | 2014-09-24 | 淄博奈琦尔生物科技有限公司 | Preparation method of antibacterial and sterile nano bamboo carbon fiber |
| 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 |
| 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 |
| 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 |
| 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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