CN1995497A - Preparation method of thermoregulation cellulose fiber with intelligent thermoregulation function - Google Patents
Preparation method of thermoregulation cellulose fiber with intelligent thermoregulation function Download PDFInfo
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Abstract
The invention relates to a manufacturing method for tempering cellulose fiber with intelligent tempering performance, characterized in that microcapsule grout of phase change energy storage materials with the weight of 10-230% of the fiber is put into the fiber stock solution of cellulose so as to form spinning dope by even mixture, which enters into the dilute caustic soda solution and dilute sulfate in turn to form the fiber; tempering cellulose fiber is formed by dilute acid decoppering, washing and drying. It is provided with simple process, low manufacturing cost and wide applicable range. The tempering cellulose fiber has the base material of cellulose fiber and the functional additive material of microcapsule of phase changer energy storage materials. The phase change energy storage materials are not easy to leak and is provided with good heat stability and tempering effect. When it is applied in down-proof fabric and duvay the phase change energy storage materials can strengthen the tempering performance.
Description
Technical field
The present invention relates to the artificial fibre field, the functional fiber cellulose fiber that particularly has the intelligent thermoregulating performance, temperature adjusting performance specifically of the present invention is excellent and can prevent the cellulose fibre of fibrillation, be in existing cellulose fibre stoste, add phase-changing energy storage material micro-capsule and a spot of emulsifying agent, make described fiber stoste and phase-changing energy storage material micro-capsule evenly be mixed and made into spinning solution with temperature adjusting performance, by having the spinning-nozzle extruding spinning of spinneret orifice, provide the cellulose fiber of the functional fiber with intelligent thermoregulating with described spinning solution.
Background technology
Cellulose strong fiber with viscose process and cuprammonium process regeneration has had more than 100 year history, in viscose process, earlier fiber is immersed production of cellulose in the soda lye, generate cellulose xanthate ester with the carbon disulfide reaction then, thereupon, cellulose xanthate ester is dissolved in rare soda lye, obtains xanthogenate solution (being fiber stoste) after filtration with after the degassing, the regeneration that xanthogenate solution is clamp-oned sulfuric acid, sodium sulphate, zinc sulfate and glucose from spinneret forms continuous filament yarn bathing.This viscose rayon that obtains is widely used in textile industry at present.Cellulose fibre also dissolves in the copper ammon solution, the copper ammon solution of cellulose fibre is entered in rare soda lye or the dilute sulfuric acid through spinneret form fiber.After pickling decopper(ing) and washing, the fiber that obtains has high wet strength.Because the fiber jewelry, expensive clothing and other valuables, gloss is suitable, high-grade silk weaving or the knitted fabric made commonly used.Its wearability is better, and good hygroscopicity has the sense of dangling, and wearability is similar to silk, meets environmental protection dress ornament trend.Copper rayon all is used for textile industry.
The Lyocell fiber of developing recently is that cellulose fibre is dissolved in the oxidation methyl morpholine solution, and fiber stoste through spinneret process air slots, is entered in water or the rare methyl morpholine oxide solution and is frozen into silk.
The heat-accumulation temperature-adjustment fiber develops by fibre manufacturing technology is combined with the phase-change material technology.The heat-accumulation temperature-adjustment fiber is that with the difference of traditional fibre the mechanism that is incubated is different.Traditional insulation fibre is to avoid skin temperature to reduce too much by insulation method, and insulation effect depends primarily on the thickness and the density of fabric.The insulation mechanism of heat-accumulation temperature-adjustment fiber then is to come from phase-changing energy storage material to pass through sense temperature to external world, and undergoes phase transition process, produces heat absorption and heat release.It can absorb heat and be stored in fibrous inside, or emit the heat of storing in the fiber according to the variation of ambient temperature from environment, the substantially invariable micro climate of formation temperature around fiber, thus realize temp regulating function.This heat absorption of heat-accumulation temperature-adjustment fiber and exothermic process are automatic, reversible, repeatedly.
Day disclosure is speciallyyed permit the method that discloses a kind of fiber with temp regulating function with paraffin (fusing point is 52 ℃) and high density polyethylene (HDPE) mixed melting spinning manufacturing among the flat 4-163370, and this fibre wearability is difficult to satisfactory.
Notification number is base material with the fibre-forming polymer for the patent of CN1103385 provides a kind of, and the phase-changing energy storage material micro-capsule is for adding the method with thermoregulator functional fiber of composition by composite molten (its melt spin temperature be 280-320 ℃) spin processes manufacturing.
Summary of the invention
The object of the present invention is to provide a kind of is base material with the cellulose fibre, with hydrophily phase-changing energy storage material micro-capsule is the preparation method of the temperature-regulating fiber cellulose fiber with intelligent thermoregulating function of functional adding ingredient, and this temperature-regulating fiber cellulose fiber is a kind of tencel with two-way adjustment effect.It can absorb heat and be stored in fibrous inside, or emit the heat of storing in the fiber according to the variation of ambient temperature from environment, the substantially invariable micro climate of formation temperature around fiber, thus realize temp regulating function.
Preparation method with temperature-regulating fiber cellulose fiber of intelligent thermoregulating function of the present invention is achieved in that the phase-changing energy storage material micro-capsule that adds fibre weight 10～230wt% in cellulose fibre stoste is the phase-changing energy storage material micro-capsule slurries of main component, make fiber stoste and phase-changing energy storage material micro-capsule be uniformly mixed to form spinning solution, above-mentioned spinning solution entered solidifying in rare soda lye and the dilute sulfuric acid by the spinneret order stretch to form fiber, through the pickling decopper(ing), after washing and the drying, obtain the temperature-regulating fiber cellulose fiber, described phase-changing energy storage material micro-capsule slurries are to be solvent with the water or the aqueous solution that contains 0.01～2wt% polyethylene glycol, containing 10～50wt% phase-changing energy storage material micro-capsule and 0.2～2wt% degree of polymerization is the solution of the PVA of 600-8000, fiber in the described fiber stoste adopts cotton fiber, flax fibre, wood pulps or bamboo pulp, described phase-changing energy storage material micro-capsule is different phase transition temperatures, the mixture of one or more in the phase-changing energy storage material micro-capsule of different enthalpy core.
Fiber stoste of the present invention can be viscose stoste or Lyocell fiber stoste, but the most frequently used fiber stoste of the present invention is copper ammonia fibre stoste; And the fiber in the described fiber stoste mainly is cotton fiber, flax fibre, wood pulps or bamboo pulp.
The present invention proposes compound by phase-changing energy storage material and cellulose fibre, providing a kind of is base material with the cellulose fibre, with hydrophily phase-changing energy storage material micro-capsule is the preparation method of the temperature-regulating fiber cellulose fiber with intelligent thermoregulating function of functional adding ingredient, and has solved the method for wherein the most key preparation and selection phase-changing energy storage material micro-capsule.
Among the preparation method of temperature-regulating fiber cellulose fiber of the present invention, described phase-changing energy storage material micro-capsule is to be formed through emulsification, coating by organic phase change material, be with 10 parts of organic phase change materials and 0.5～5 part of emulsifier, add 75～200 parts of aqueous solution that contain 0.2～3wt% nonionic surface active agent class stabilizing agent, 0～2.5 part of alkali metal salt, stir 10～60min down at 40～95 ℃, make phase-change material be uniformly dispersed into emulsion; In above-mentioned emulsion, add 7.5～75 parts of ethyl orthosilicates and 0.15～5 part of acid catalyst, under 20～70 ℃ of water-baths, react 3～12h, the room temperature ageing, filtration, washing get product, above-mentioned organic phase change material is the lipophile organic phase change material, emulsifying agent is the mixture that sorbitol anhydride oleate and Tween-81 were formed by weight 0.4: 0.6～0.6: 0.4, and above umber is weight portion.
Phase-changing energy storage material micro-capsule described in the inventive method because phase-changing energy storage material has been carried out microencapsulation, makes that this material is difficult for leaking, and has improved the specific surface of phase-change material simultaneously, thereby heat endurance and thermoregulation effect are good.
Experiment shows, selects phase transformation paraffin for use, C
14-C
22N-alkane, C
8-18Fatty alcohol or C
8-18Aliphatic acid and ester thereof, as the lipophile organic phase change material of making phase-changing energy storage material micro-capsule among the present invention, make phase-changing energy storage material micro-capsule chemical stability and the Heat stability is good and the applied range of generation, as select for use wherein lightweight paraffin, 25# paraffin, 30# paraffin, 35# paraffin, hexadecane, octadecane, eicosane or n-butyl stearate then to have better effect.
Emulsifying agent of the present invention is a nonionic surface active agent, comparatively commonly used can be the mixture of poly-oxireme lauroyl ether (Brij30) or sorbitol anhydride oleate (Span80) and Tween-81 (Tween80), the mixture of preferably selecting for use Span80: Tween80 (weight) to form in 0.4: 0.6～0.6: 0.4.
The present invention is when preparation organic phase change material emulsion, and per 10 parts of organic phase change materials add 1～5 part of emulsifying agent, and add 75～200 parts of water that contain stabilizing agent.When the emulsifying agent relative amount is higher, should add more water; Otherwise, then add less water.
Because emulsion is a non-equilibrium system, be in the steady state that is situated between, the trend that forms stabilising system is arranged, add stabilizing agent in the emulsion and can change the system rheological characteristic, increase system viscosity, the movement velocity of particulate in the reduction system, thus reach the purpose of stabilising system.
Stabilizing agent among the present invention belongs to nonionic surface active agent, selects water soluble polymer usually for use, preferentially selects polyvinyl alcohol or carboxymethyl cellulose or gelatine for use.
Stabilizing agent of the present invention dissolves in the water earlier usually, join in the emulsion with its aqueous solution, its concentration of aqueous solution is generally at 0.2～3wt%, if cross lowly, then do not reach stablizing effect, be difficult to obtain dispersiveness microballoon preferably, if stabilizer concentration is too high, then emulsion viscosity is too big, and the migration velocity of various materials is too slow in the system, causes reaction speed low excessively.Preferred concentration is 1～2wt%.
The present invention also need add an amount of additive basic slaine when the preparation emulsion, preferentially select sodium chloride usually for use.
The present invention is fully emulsified in order to ensure phase-change material, generally needs to stir 10～60min down at 40～95 ℃.Temperature is low excessively, does not then reach emulsifying effectiveness preferably, if temperature is too high, then may cause emulsion inverse, promptly is converted into water-in-oil type by emulsion oil-in-water, causes the emulsion instability; Emulsification times is too short, and then emulsifying effectiveness is poor, and with 60～95 ℃, 20～40min is comparatively commonly used.
Ethyl orthosilicate as phase-changing energy storage material micro-capsule wall material silicon source joins in the above-mentioned emulsion, is catalyst with acid, carries out hydrolysis, the polycondensation reaction of TEOS under 20～70 ℃ of water-baths.The speed of hydrolytie polycondensation is bigger for the formation influence of micro-capsule, as the temperature height, hydrolysis rate is fast, and polycondensation speed is also fast, the cyst wall that then obtains is a loose structure, porosity is bigger, and densification, and hydrolysis rate inadequately and polycondensation speed are fast, the products obtained therefrom productive rate is also low, low as temperature, then the reaction time long, efficient is low.Optimal conditions in the experiment is 50～70 ℃ of reaction temperatures, and its corresponding reaction time is 2～4 hours.It preferentially selects catalyst commonly used for use is hydrochloric acid, nitric acid, sulfuric acid, acetic acid.
The present invention adds 7.5～75 parts of ethyl orthosilicates in the emulsion that whenever contains 10 parts of organic phase change materials, in the presence of catalyst by hydrolysis, polycondensation reaction, corresponding acquisition organic phase change material is that capsule-core, silica dioxide gel are the phase-changing energy storage material micro-capsule of cyst wall, and its corresponding cyst wall and capsule-core weight ratio are between 20: 80～70: 30.
The present invention has successfully realized the compound of phase-changing energy storage material and cellulose fibre, providing a kind of is base material with the cellulose fibre, with hydrophily phase-changing energy storage material micro-capsule is the preparation method of the temperature-regulating fiber cellulose fiber with intelligent thermoregulating function of functional adding ingredient, and technology is simple, and cost is low.Owing in technology, adopt the phase-changing energy storage material of microencapsulation, make that this material is difficult for leaking, improved the specific surface of phase-change material simultaneously, thereby heat endurance and thermoregulation effect are good; Especially the present invention adds certain amount of stabilizer and makes the phase-changing energy storage material emulsion have enough stability in the emulsion process of organic phase change material, thereby prepared phase-changing energy storage material micro-capsule is spherical in shape, particle diameter is evenly distributed, and has enlarged the scope of application, has also strengthened its thermal property.
The specific embodiment
Embodiment 1.
Get the 5mL phase transition temperature and be 35 ℃ 35# phase transformation paraffin, add 1.0 gram sorbitol anhydride oleates (Span80) and press the blended emulsifier that mass ratio is formed at 0.4: 0.6 with Tween-81 (Tween80), under heating, stirring condition, the aqueous solution that 30mL is contained 1% gelatine joins in the above-mentioned oil phase, the sodium chloride that adds 0.5mL 2.5mol/L again, continue heating, stir emulsification 30min.Relatively fully the back adds 0.25ml 1% hydrochloric acid, 4mL density is the ethyl orthosilicate of 0.9 grams per milliliter to treat emulsification, places under 60 ℃ the stirred in water bath to react 3h, and ageing 12h filters, washing, promptly obtains the phase-changing energy storage material micro-capsule.Scanning electron micrograph is shown as nucleocapsid structure.The enthalpy change of micro-capsule in phase transition process is 108J/g, and 35# phase-change wax (its enthalpy is 137J/g) content in micro-capsule is 78.8%.
The phase-changing energy storage material micro-capsule that to get above-mentioned 3 parts of 35# phase-change wax be core adds 0.05 part of polyvinyl alcohol, adds 6.90 parts of water and 0.05 part of polyethylene glycol, and it is mixed the formation slurries; Get 3 parts of wood pulps and pulverize the cellulose copper ammon solution that adds formation thickness in the copper ammon solution; With mixing in the above-mentioned slurries adding cellulose copper ammon solution, form spinning solution; At last, spinning solution is entered in rare soda lye and the dilute sulfuric acid by the spinneret order form fiber.After pickling decopper(ing), washing and drying, obtain temperature-regulating fiber.
Embodiment 2.
Get the 5mL phase transition temperature and be 27～29 ℃ octadecane, add 1.5 gram Span80, Tween80 and press 0.5: 0.5 composite emulsifying agent of mass ratio, under heating, stirring condition, slowly add the aqueous solution that 50mL contains 2% hydroxylated cellulose, the sodium chloride that adds 1mL 2.5mol/L again, continue heating, stir 30min simultaneously, carry out fully emulsified mixed liquor.Treat that relatively fully slowly to add 1mL 10% acetic acid and 16mL density be the ethyl orthosilicate of 0.9 grams per milliliter in the back in emulsification, place under 60 ℃ the stirred in water bath and react 3h that ageing 24h filters, washing, promptly obtains the phase-changing energy storage material micro-capsule.The enthalpy of micro-capsule in phase transition process is 119J/g.Octadecane (its enthalpy is 237J/g) content in micro-capsule is 50.2%.
The phase-changing energy storage material micro-capsule that to get 3 parts of above-mentioned octadecanes be core adds 0.02 part of polyvinyl alcohol, adds 6.98 parts of water as solvent, and it is mixed the formation slurries; 6 parts of cotton fibers are added the copper ammon solution that forms thickness in the copper ammon solution; With mixing in the above-mentioned slurries adding cellulose copper ammon solution, form spinning solution; At last, above-mentioned spinning solution is entered in rare soda lye and the dilute sulfuric acid in proper order by subsurface spinneret form fiber.After decopper(ing), washing and drying, obtain temperature-regulating fiber.
Embodiment 3.
Getting 3 parts is the phase-changing energy storage material micro-capsule of core by embodiment 2 method gained octadecanes, adds 0.05 part of polyvinyl alcohol, adds 6.95 parts of aqueous solvent, and it is mixed the formation slurries; 3 parts of wood pulps are pulverized the copper ammon solution that adds formation thickness in the copper ammon solution; With mixing in the above-mentioned slurries adding cellulose copper ammon solution, form spinning solution; At last, spinning solution is entered in rare soda lye and the dilute sulfuric acid by the spinneret order form fiber.After pickling decopper(ing), washing and drying, obtain temperature-regulating fiber.
Embodiment 4.
Get the 5mL phase transition temperature and be 25 ℃ 25# phase transformation paraffin, add 1.5 gram Span80, Tween80 and press 0.4: 0.6 composite emulsifying agent of mass ratio, under heating, stirring condition, add 60mL and contain polyvinyl alcohol 1.5% aqueous solution, and then the sodium chloride of adding 1mL 2.5mol/L, emulsification 30min under heating and stirring condition.Relatively fully the back adds 0.25mL 1% hydrochloric acid, 24mL density is the ethyl orthosilicate of 0.9 grams per milliliter to treat emulsification, places under 60 ℃ the stirred in water bath to react 3h, and ageing 5h filters, washing, promptly obtains the phase-changing energy storage material micro-capsule.The enthalpy of micro-capsule in phase transition process is 58.6J/g, and 25# phase-change wax (its enthalpy is 145.5J/g) content in micro-capsule is 40.3%..
The phase-changing energy storage material micro-capsule that to get 4 parts of above-mentioned 25# phase-change wax be core adds 0.05 part of polyvinyl alcohol, adds 5.95 parts of aqueous solvent, and it is mixed the formation slurries; 3 parts of cotton fibers are added the copper ammon solution that forms thickness in the copper ammon solution; With mixing in the above-mentioned slurries adding cellulose copper ammon solution, form spinning solution; At last, spinning solution is entered in rare soda lye and the dilute sulfuric acid by the spinneret order form fiber.After pickling decopper(ing), washing and drying, obtain temperature-regulating fiber.
Embodiment 5.
Get the 5mL phase transition temperature and be 30 ℃ 30# phase transformation paraffin, add 0.5 gram Span80, Tween80 and press the mixture that mass ratio is formed at 0.45: 0.55, the aqueous solution that 40mL is contained 0.5% polyvinyl alcohol under heating, stirring condition joins in the above-mentioned oil phase, the sodium chloride that adds 1mL 2.5mol/L again, continue heating, stir 30min, carry out fully emulsified mixed liquor.With 0.5mL 10% acetic acid and 8mL density is that the ethyl orthosilicate of 0.9 grams per milliliter joins in the above-mentioned emulsion, places 60 ℃ water-bath, under agitation reacts 3h, and room temperature ageing 5 hours is filtered, washing, promptly obtains the phase-changing energy storage material micro-capsule.Be spherical nucleocapsid, the enthalpy of micro-capsule in phase transition process is 87.1J/g.30# phase-change wax (its enthalpy is 140J/g) content in micro-capsule is 62.2%.
The phase-changing energy storage material micro-capsule that to get above-mentioned 4 parts of 30# phase-change wax be core adds 0.05 part of polyvinyl alcohol, adds 6.95 parts of aqueous solvent, and it is mixed the formation slurries; 2 parts of cotton fibers are added the copper ammon solution that forms thickness in the copper ammon solution; With mixing in the above-mentioned slurries adding cellulose copper ammon solution, form spinning solution; At last, spinning solution is entered in rare soda lye and the dilute sulfuric acid by the spinneret order form fiber.After pickling decopper(ing), washing and drying, obtain temperature-regulating fiber.
Claims (5)
1, a kind of preparation method with temperature-regulating fiber cellulose fiber of intelligent thermoregulating function, the phase-changing energy storage material micro-capsule that it is characterized in that adding fibre weight 10～230% in cellulose fibre stoste is the phase-changing energy storage material micro-capsule slurries of main component, make fiber stoste and phase-changing energy storage material micro-capsule be uniformly mixed to form spinning solution, above-mentioned spinning solution entered solidifying in rare soda lye and the dilute sulfuric acid in proper order stretch to form fiber, after diluted acid decopper(ing), washing and drying, obtain the temperature-regulating fiber cellulose fiber; Described phase-changing energy storage material micro-capsule slurries are to be solvent, to contain 10～50wt% phase-changing energy storage material micro-capsule and 0.2～2wt% degree of polymerization is the PVA solution of 600-8000 with the water or the aqueous solution that contains 0.01～2wt% polyethylene glycol, fiber in the described fiber stoste adopts cotton fiber, flax fibre, wood pulps or bamboo pulp, and described phase-changing energy storage material micro-capsule is one or more the mixture in the phase-changing energy storage material micro-capsule of different phase transition temperatures, different enthalpy core.
2, the preparation method of temperature-regulating fiber cellulose fiber as claimed in claim 1, it is characterized in that described phase-changing energy storage material micro-capsule is to be formed through emulsification, coating by organic phase change material, be with 10 parts of organic phase change materials and 0.5～5 part of emulsifier, add 75～200 parts of aqueous solution that contain 0.2～3wt% nonionic surface active agent class stabilizing agent, 0～2.5 part of alkali metal salt, stir 10～60min down at 40～95 ℃, make phase-change material be uniformly dispersed into emulsion; In above-mentioned emulsion, add 7.5～75 parts of ethyl orthosilicates and 0.15～5 part of acid catalyst, under 20～70 ℃ of water-baths, react 3～12h, the room temperature ageing, filtration, washing get product, above-mentioned organic phase change material is the oleophylic organic phase change material, emulsifying agent is the mixture that sorbitol anhydride oleate and Tween-81 were formed by weight 0.4: 0.6～0.6: 0.4, and above umber is weight portion.
3, the preparation method of temperature-regulating fiber cellulose fiber as claimed in claim 2 is characterized in that the alkali metal salt that is adopted is a sodium chloride, and described acid as catalyst is hydrochloric acid or nitric acid or sulfuric acid or acetic acid.
4. as the preparation method of claim 2 or 3 described temperature-regulating fiber cellulose fibers, it is characterized in that described stabilizing agent is a water soluble polymer.
5. the preparation method of temperature-regulating fiber cellulose fiber as claimed in claim 4 is characterized in that described water soluble polymer class stabilizing agent is polyvinyl alcohol or carboxymethyl cellulose or gelatine.
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| CN100523319C (en) | 2009-08-05 |
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