CN105709674A - Temperature-controllable health-care microcapsule and preparation method thereof - Google Patents
Temperature-controllable health-care microcapsule and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a temperature-controllable health-care microcapsule and a preparation method thereof. The preparation method includes the preparation steps of prepolymer preparing, compound core emulsion preparing, film formation by polymerization reaction, washing and drying. The temperature-controllable health-care microcapsule consists of a compound core and a wall material composed of high-molecular polymers, wherein the compound core is formed by blending adsorption of health-care functional powder and temperature-dependent phase change materials, the weight ratio of the composite core to the wall material is 0.3-3 to 1, average grain size of the health-care functional powder is not less than 1.2 micrometers, and average grain size of the microcapsule is not less than 3 micrometers. The temperature-controllable health-care microcapsule has the advantages that owing to the temperature control function of the microcapsule, release rate of trace elements of the functional powder in winter can be increased, human body subcutaneous microcirculation is reinforced, and human bodies' absorption of health-care active ingredients is improved; comfortable temperature between a clothing product and the skin of human bodies can be kept; the problem of dispersibility of the functional powder in blended spinning production can be solved.
Description
Technical field
The invention belongs to Micro-Encapsulation Technique field, relate to a kind of temperature control health care microcapsule suitable in field of textiles and preparation method thereof.
Background technology
Microcapsule technology is a kind of to adopt filmogen that small active particle is overmolding to the new technique with nuclear core-wall shell structure microgranule.By small active material micro encapsulation, it is effectively reduced active substance for periphery system, the reaction including solid, liquid, gas and illumination etc., and effectively controls it for the flowing of external environment, release or extension.At present, microcapsule technology is widely used in the fields such as food, medicine, weaving and engineering material.
Chinese Patent Application No. 200610017695 discloses a kind of fabric nano post-treatment reagent with persistency antibiotic fragrance effect and processing technology thereof, adopt the mixture of antibacterial and aromatic as core, high adhesion material is as wall material, generate antibiotic aromatic type microcapsule solution and be used as fabric nano post-treatment reagent, there is the advantages such as lasting, washable, nontoxic.
Chinese Patent Application No. 201410194001 discloses a kind of clothing energy-saving and temperature-regulating microcapsule phase-change insulation material and preparation method thereof, adopting Organic Alcohol and organic ester mixture is core, chitosan and silica dioxide gel mixture are wall material, prepare energy-saving and temperature-regulating microcapsule, for dress-goods, there is adjustment high insulating effect, temperature retention time is permanent, does not affect the advantages such as clothing snugness of fit.
The application of microcapsule technology, has widened the development approach of new type functional textile.
In textile applications field, consumer is more and more high for the requirement of the functional of textile He comfortableness, and wherein the demand of comfort health-care function class textile increases day by day.Raising along with textile science technical merit, all kinds of health textiles with far-infrared functional, antibacterial functions, magnetic therapy functions, as pearl fiber textile, chitin fiber textile, Chinese medicine blood circulation promoting and blood stasis dispelling fiber textile and anion, magnetic therapy rehabilitation home textile articles for use etc. are come out one after another, largely meet consumer demand.
But, existing health care textile is producing, and takes and still suffers from deficiency with health-care effect aspect, is embodied in:
Aborning, for pearl viscose fiber (Chinese Patent Application No. 200410067962.5), owing to, in this technology, Margarita powder liquid slurry adopts water soluble dispersing agent, and with distilled water for carrier, therefore after adding Margarita powder liquid slurry in spinning process, Margarita powder dispersibility in spinning liquid declines, and when high-volume spinning, Margarita powder blocks the phenomenon of spinneret orifice and happens occasionally after reuniting, spinning terminates, it is seen that Margarita powder body is deposited in the bottom of container；This drawback has had a strong impact on the production efficiency of pearl fiber.Simultaneously as the precipitation of Margarita powder, add raw-material cost.Additionally, in the coagulating bath of rayon spinning, the erosion of sulphuric acid inevitably reduces effect of Margarita powder body.
Antimicrobial pearl viscose fiber (Chinese Patent Application No. 200710008726) technology adds organic antibacterial agent in Margarita powder mother solution, correspondingly dispersant adopts polyether-type nonionic activating agent, carrier is polyhydric alcohol tween, dispersibility increases to a certain extent, but does not fundamentally solve above-mentioned drawback.
The drawback that the above Margarita powder dispersity is not enough and powder body work in-process is corroded by sulphuric acid has general character in functional powder co-blended spinning is processed.
Take with health-care effect in, owing to Margarita is cold in nature, under taking condition summer, consumer sensation pearl fiber underwear cool and comfortable, be subject to consistent favorable comment；But when taking in the winter time, underwear is taken excessively cooler, have impact on comfortableness to a certain extent.Furthermore, consider that temperature and illumination are energy in arousal function powder body, thus the key factor of effective release of trace elements, therefore, when temperature is on the low side in the winter time, the impact that the trace element burst size of functional powder Margarita microparticle and far infrared normal emittance all can be now shown in.Obviously, maintain the functional powder in textile product and be in the temperature range being conducive to continuing to excite its interior energy, for improving the wearing comfort of textile, strengthen health-care effect significant.
In prior art, the application of microcapsule technology is mainly reflected in the isolation control Technology solving active material with periphery system, to expand the application of active material；For how to realize temperature control health care so that it is active component plays lasting maximum efficiency and still belongs to blank.
Summary of the invention
It is an object of the invention to provide a kind of temperature control health care microcapsule and preparation method thereof, to realize temperature control health care, effect that function powder body is lasting, and solution health care fibrid causes production efficiency to decline in process of production owing to dispersibility is bad, cost of material improves, powder body meets acid degradation and improves the technical problems such as product wearing comfort in winter simultaneously.
The preparation method of a kind of temperature control health care microcapsule of the present invention, is characterized in that step is: prepares performed polymer and prepares heath-function powder body and temperature and cause phase-change material composite core material emulsion polyreaction film forming and wash and dry；
Described performed polymer step of preparing is:
Tripolycyanamide, formalin and distilled water are mixed, regulates pH value to 8～9, be warmed up to 60～80 DEG C, with 200-500r/min low rate mixing to clear viscous shape liquid.
In this stage, macromolecular material used by wall material is pre-formed thick polymer, and the proportioning of this performed polymer determines its viscosity, thus directly affecting the wall material cladding form of microcapsule.
Described heath-function powder body of preparing causes phase-change material composite core material emulsion step with temperature and is:
At 40-50 DEG C of temperature, the temperature of fusing is caused after phase-change material, emulsifying agent and deionized water mix with high speed 6000-10000r/min emulsifying, then it is heated to 90-99 DEG C with oil bath, add heath-function powder body and dispersant, continue with after 400-600r/min rotating speed emulsifying 10～15min, cool to 30-40 DEG C, with weak acid for adjusting pH value to 5～6.
In this stage, functional powder enters, with the form of adsorbent, the emulsion causing phase-change material containing temperature, and its microcellular structure and configuration of surface can receive/adsorb phase transformation particles of material effectively, forms heath-function powder body and causes phase-change material composite core material emulsion with temperature.The concentration of emulsion has material impact for lower road polyreaction film formation process.Concentration is too low, will result in performed polymer molecular weight and molecular weight, and wall material cladding is bad, and compactness is deteriorated, and even can not be effectively formed microcapsule；Excessive concentration, then the homogeneity of microcapsule is deteriorated；Emulsifying rate, the selection of dispersant and the control of technological temperature directly influence functional powder and cause the adsorbed state of phase-change material and the size of microcapsule with temperature.
Described polyreaction film formation step is:
Heath-function powder body and temperature are caused phase-change material composite core material emulsion and is warmed to 50-60 DEG C, maintain pH value 5-6, with the stirring of 200-500r/min rotating speed and drip at a slow speed performed polymer with 10-30ml/min, after arrest reaction 100-150min, cool to 15-25 DEG C, then regulate pH value with sodium hydroxide and terminate reaction to 8-9.
In this stage, the high molecular polymer adsorption precipitation in performed polymer, on composite core material, forms cladding film forming in acid condition around composite core material after polycondensation reaction；The uniformity of film forming depends on mating of mixing speed and drop rate；The arrest reaction time is controlled makes film thickness；In the basic conditions, polyreaction terminates, and cyst wall is formed.
Described washing also dries and is:
Add carbamide and remove residual formaldehyde, with hot ethanol and hot wash after sucking filtration, then carry out vacuum drying, i.e. add carbamide-stirring at low speed-vacuum filtration-interpolation hot ethanol-hot wash-vacuum drying.
This stage, when pH=7-7.5, carbamide and free formaldehyde additive reaction, generate the monomethylolurea and the dimethylol urea that are dissolved in water, stir with 120-200r/min rotating speed, fully after reaction, vacuum filtration implements solid-liquid separation；Add 40-45 DEG C of hot ethanol and remove remaining Organic substance, with the dry 100-120min of 50-60 DEG C of temperature in vacuum drying oven after 40-45 DEG C of hot wash.
The preparation method of a kind of temperature control health care microcapsule as above, the mass ratio of tripolycyanamide, formalin and distilled water is 1: 1～2: 1～2；Wherein the concentration of formalin is 30～50wt%.
The preparation method of a kind of temperature control health care microcapsule as above, it is 1: 0.5～2: 5～10 that temperature causes the mass ratio of phase-change material, emulsifying agent and deionized water；High speed emulsification times is 30～40min；The mass ratio of heath-function powder body and dispersant is 5～10: 1；The mass ratio that heath-function powder body causes phase-change material with temperature is 0.5～2: 1；Described dispersant is propylene glycol block polyether.
The preparation method of a kind of temperature control health care microcapsule as above, it is 0.5～2: 1 that temperature causes the mass ratio of phase-change material and performed polymer.
Present invention also offers a kind of temperature control health care microcapsule prepared by method made above, heath-function powder body cause the blended composite core material formed of phase-change material and the wall material being made up of high molecular polymer is formed with temperature；The mass ratio of described composite core material and wall material is 0.3～3: 1；Described heath-function powder body mean diameter≤1.2 μm；Mean diameter≤3 μm of described microcapsule.
As preferred technical scheme:
Temperature control health care microcapsule as above a kind of, described heath-function powder body is that one or more in Margarita powder body, Chinese crude drug powder body, chitin powder body, antimicrobial powder, bamboo-carbon powder or magnetic material powder mix.
A kind of temperature control health care microcapsule as above, described temperature causes phase-change material and selectes according to the temperature control of product and condition of taking, and mixes for one or more in paraffin, crystalline hydrate salt, eutectic hydrated salt, Polyethylene Glycol or linear paraffin.
A kind of temperature control health care microcapsule as above, the high molecular polymer of described wall material is polyureas, polyester resin, Lauxite, gelatin, poly-polyprotic acid or melamine resin.
A kind of temperature control health care microcapsule as above, it is 0.5～2: 1 that the heath-function powder body in described composite core material and described temperature cause the mass ratio of phase-change material.
The temperature control health care microcapsule of the present invention can be used for spinning functional fibre, including native cellulose class functional fibre and synthetic fibers class functional fibre.
Microcapsule technology is a kind of to adopt filmogen that molecule is overmolding to the new technique with nuclear core-wall shell structure microgranule.The formation basic theory of microcapsule is to make high molecular polymer adsorption precipitation in the periphery of molecule (solid, liquid or gas), then passes through the reaction condition changing polymer, makes high molecular polymer film forming, forms shell.Molecule in microcapsule is called core, and shell is called wall material.The mass ratio of the wall material/core of microcapsule and the rotating speed of modulation molecule emulsion, affect the size of the clad ratio of microcapsule, permeability and particle diameter.
Phase-change material refers under the change of ambient temperature, and " solid-solid ", " solid-liquid ", " Gu-vapour " or " liquid-vapour " change reversible material occur its structure mutually.In recent years, owing to phase-change material has the characteristic absorbing or discharging big calorimetric potential in phase transition process, this material obtains very big development in the application of heat accumulation engineering field.Phase-change material kind is a lot, including paraffin class, crystalline hydrate salt, eutectic hydrated salt, Polyethylene Glycol and linear paraffin etc..Wherein paraffin is the mixture comprising linear paraffin, isoparaffin, cycloalkane, and due to it, to have enthalpy change in phase transformation relatively big, good reversibility, temperature-controllable and low cost and other advantages, is subject to the growing interest of researcher.
The temperature control health care microcapsule that technical solution of the present invention prepares, its composite core material is formed by functional powder and the blended adsorption combined of phase-change material, under the effect of auxiliary agent, the microcellular structure of functional powder and configuration of surface can receive/adsorb phase-change material effectively, and the size of the clad ratio of microcapsule, permeability and particle diameter is easily controllable；Temperature control health care uniform microcapsule ground is implanted in main material, product can be made to be not affected by waiting the impact of change, can ensure that the wearing comfort of product and health-care effect.Its mechanism of action is as follows: when ambient temperature raises, and is embedded in the phase-change material in temperature control health care microcapsule and can produce " solid-liquid " phase transformation, in the process, phase-change material heat absorption heat accumulation, make main material surface temperature reduce, user can experience pleasantly cool sense；When ambient temperature reduces, phase-change material can produce " liquid-solid " phase transformation, and in the process, heat released by phase-change material, makes main material surface temperature raise, even if in the winter time, user crosses discomfort that is cool and that produce without experiencing main material；Simultaneously, owing to the temperature of the functional powder in main material raises, the release rate and the far infrared normal emittance that make its trace element in the winter time are improved significantly, and strengthen the subcutaneous microcirculation of user's human body, improve the human body absorption to functional powder effective ingredient.
Use microcapsule technology that composite core material can be made to avoid after product impaired in road processing under the parcel of wall material or dissolve, functional incompatible core composition can be made to be uniformly dispersed being blended in main material, and microcapsule core rate of release in the application can be controlled.Therefore, temperature control health care microcapsule technology applies to, in the production of health care regenerated celulose fibre, to efficiently solve the deficiencies in the prior art.
Beneficial effect:
Compared with prior art, the having the beneficial effect that of temperature control microcapsule technology of the present invention:
(1) the temperature control health care microcapsule of technical solution of the present invention processing gained can strengthen the far infrared normal emittance of functional powder when product is taken winter, improves trace element burst size, strengthens its health-care effect；Can effectively keep the suitable temperature between main material and human body, reach cool in summer and warm in winter to take effect.
(2) technical solution of the present invention can make functional powder be dispersed in uniformly and stably in spinning liquid in the spinning processing in later stage, eliminates functional powder blocking spinneret orifice phenomenon, hence it is evident that improve production efficiency；The valuable significant loss simultaneously avoiding the precipitation of functional powder and cause, thus being greatly lowered production cost.
(3) the temperature control health care microcapsule prepared by technical solution of the present invention is both high temperature resistant, acid and alkali-resistance again, is avoided that functional powder directly contacts with acid solution in spinning coagulation bath and causes the degraded of functional powder, it is ensured that the effective ingredient of powder body.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, the present invention can be made various changes or modifications by those skilled in the art, and these equivalent form of values fall within the model that the application appended claims limits equally. enclose.
A kind of temperature control health care microcapsule of the present invention, described temperature control health care microcapsule is by heath-function powder body and temperature causes the blended composite core material formed of phase-change material and the wall material being made up of high molecular polymer is formed；The mass ratio of described composite core material and wall material is 0.3～3: 1；Described heath-function powder body mean diameter≤1.2 μm；Mean diameter≤3 μm of described microcapsule.
Wherein, described heath-function powder body be in Margarita powder body, Chinese crude drug powder body, chitin powder body, antimicrobial powder, bamboo-carbon powder or magnetic material powder one or more mix.
Wherein, described temperature cause phase-change material be in paraffin, crystalline hydrate salt, eutectic hydrated salt, Polyethylene Glycol or linear paraffin one or more mix.
Wherein, the high molecular polymer of described wall material is polyureas, polyester resin, Lauxite, gelatin, poly-polyprotic acid or melamine resin.
Wherein, the mass ratio that the heath-function powder body in described composite core material and temperature cause phase-change material is 0.5～2: 1.
Embodiment 1
The preparation method of a kind of temperature control health care microcapsule, step is: prepares performed polymer and prepares heath-function Margarita powder body and temperature and cause phase-change material paraffin composite core material emulsion polyreaction film forming and wash and dry；
Wherein, preparing performed polymer step is:
By formalin that tripolycyanamide that mass ratio is 1: 2: 2, concentration are the 37wt% common-use size of commercially available prod (37% be) and distilled water mixing, regulate pH value with triethanolamine and be warmed up to 70 DEG C to 9, with the low rate mixing of 200r/min to clear viscous shape liquid；Performed polymer total amount is by the 140% of Quality of Paraffin Waxes；
Prepare heath-function Margarita powder body and temperature to cause phase-change material paraffin composite core material emulsion step and be:
At 40 DEG C of temperature, by styrene-maleic anhydride copolymer sodium salt solution that the 250g30# paraffin of fusing, 130g mass fraction are 18% and the mixing of 2000ml deionized water, with high speed 8000r/min emulsifying 40min；Add 250g Margarita powder body (mean diameter 0.8 μm) and 30g propylene glycol block polyether after being heated to 95 DEG C with oil bath, continue with 400r/min rotating speed emulsifying 10min, cool to and regulate ph value of emulsion to 5 with the acetic acid that mass fraction is 10% after 30 DEG C；
Polyreaction film formation step is:
Margarita powder body and paraffin composite core material emulsion are warmed to 50 DEG C, maintain pH value 5, with the stirring of 200r/min rotating speed and with the performed polymer 350g of dropping at a slow speed of 10ml/min, after arrest reaction 100min, cool to 15 DEG C, then regulate pH value with sodium hydroxide and terminate reaction to 9；
Wash and dry and be:
With Fructus Citri Limoniae acid for adjusting pH value to 7.2, adding 10g carbamide, after stirring 5min with 120r/min rotating speed, vacuum filtration implements solid-liquid separation；Add 40 DEG C of hot ethanol 50ml and remove remaining Organic substance, with the dry 120min of 50 DEG C of temperature in vacuum drying oven after 40 DEG C of hot washes, i.e. prepare a kind of temperature control pearl health-care microcapsule.
Embodiment 2
The preparation method of a kind of temperature control health care microcapsule, step is: prepares performed polymer and prepares heath-function Chinese medicine Radix Notoginseng powder body and temperature and cause phase-change material paraffin composite core material emulsion polyreaction film forming and wash and dry；
Wherein, preparing performed polymer step is:
By formalin and distilled water mixing that tripolycyanamide that mass ratio is 1: 1.8: 2, concentration are 37wt%, regulate pH value to 9 with triethanolamine, be warmed up to 68 DEG C, with the low rate mixing of 300r/min to clear viscous shape liquid；Performed polymer total amount is by the 160% of Quality of Paraffin Waxes；
Prepare heath-function Chinese medicine Radix Notoginseng powder body and temperature to cause phase-change material paraffin composite core material emulsion step and be:
At 50 DEG C of temperature, after styrene-maleic anhydride copolymer sodium salt solution that the 250g30# paraffin of fusing, 130g mass fraction are 18% and the mixing of 1800ml deionized water, with high speed 9000r/min emulsifying 30min；Then it is heated to 98 DEG C with oil bath, adds 300g Chinese medicine Radix Notoginseng powder body (mean diameter 1 μm) and 35g dispersant propylene glycol block polyether, continue, after 600r/min rotating speed emulsifying 15min, to cool to 35 DEG C, with Fructus Citri Limoniae acid for adjusting pH value to 5.5；
Polyreaction film formation step is:
Chinese medicine Radix Notoginseng powder body and paraffin composite core material emulsion are warmed to 60 DEG C, maintain pH value 5.5, with the stirring of 250r/min rotating speed and with the performed polymer 400g of dropping at a slow speed of 15ml/min, after arrest reaction 150min, cool to 25 DEG C, then regulate pH value with sodium hydroxide and terminate reaction to 9；
Wash and dry and be:
With Fructus Citri Limoniae acid for adjusting pH value to 7.0, adding 12g carbamide, after stirring 8min with 100r/min rotating speed, vacuum filtration implements solid-liquid separation；Add 42 DEG C of hot ethanol 40ml and remove remaining Organic substance, with the dry 100min of 55 DEG C of temperature in vacuum drying oven after 42 DEG C of hot washes, i.e. prepare a kind of temperature control Chinese medicine Radix Notoginseng health care microcapsule.
Embodiment 3
The preparation method of a kind of temperature control health care microcapsule, step is: prepares performed polymer and prepares heath-function antimicrobial powder and temperature and cause phase-change material n-octadecane composite core material emulsion polyreaction film forming and wash and dry；
Wherein, preparing performed polymer step is:
By formalin and distilled water mixing that tripolycyanamide that mass ratio is 1: 1.6: 1.8, concentration are 37wt%, regulate pH value to 8.5 with triethanolamine, be warmed up to 70 DEG C, with the low rate mixing of 250r/min to clear viscous shape liquid；Performed polymer total amount is by the 150% of n-octadecane quality；
Prepare heath-function antimicrobial powder and temperature to cause phase-change material n-octadecane composite core material emulsion step and be:
At 45 DEG C of temperature, after styrene-maleic anhydride copolymer sodium salt solution that 280g n-octadecane, 140g mass fraction are 18% and the mixing of 2000ml deionized water, with high speed 8000r/min emulsifying 30min；Then it is heated to 92 DEG C with oil bath, adds 300g Zinc oxide powder (mean diameter 1 μm) and 30g dispersant propylene glycol block polyether, continue, after 400r/min rotating speed emulsifying 15min, to cool to 30 DEG C, with Fructus Citri Limoniae acid for adjusting pH value to 5；
Polyreaction film formation step is:
Zinc oxide powder and n-octadecane composite core material emulsion are warmed to 58 DEG C, maintain pH value 5, stir with 220r/min rotating speed, and with the performed polymer 420g of dropping at a slow speed of 18ml/min, after arrest reaction 100min, cool to 20 DEG C, then regulate pH value with sodium hydroxide and terminate reaction to 9；
Wash and dry and be:
With Fructus Citri Limoniae acid for adjusting pH value to 7.3, adding 12g carbamide, after stirring 5min with 120r/min rotating speed, vacuum filtration implements solid-liquid separation；Add 40 DEG C of hot ethanol 50ml and remove remaining Organic substance, with the dry 120min of 60 DEG C of temperature in vacuum drying oven after 45 DEG C of hot washes, i.e. prepare a kind of temperature control antibiotic health care microcapsule.
Embodiment 4
The preparation method of a kind of temperature control health care microcapsule, step is: the preparation each heath-function chitin powder body of pre-polymerization system causes phase-change material paraffin composite core material emulsion polyreaction film forming with temperature and washs and dry；
Wherein, preparing performed polymer step is:
By formalin and distilled water mixing that tripolycyanamide that mass ratio is 1: 1.6: 2, concentration are 40wt%, regulate pH value to 8 with triethanolamine, be warmed up to 72 DEG C, with the low rate mixing of 350r/min to clear viscous shape liquid；Performed polymer total amount is by the 150% of Quality of Paraffin Waxes；
Prepare heath-function chitin powder body and temperature to cause phase-change material paraffin composite core material emulsion step and be:
At 45 DEG C of temperature, after styrene-maleic anhydride copolymer sodium salt solution that the 250g30# paraffin of fusing, 130g mass fraction are 18% and the mixing of 1800ml deionized water, with high speed 7000r/min emulsifying 35min；Then it is heated to 90 DEG C with oil bath, adds 300g chitin powder body (mean diameter 1 μm) and 30g dispersant propylene glycol block polyether, continue, after 500r/min rotating speed emulsifying 12min, to cool to 30 DEG C, with Fructus Citri Limoniae acid for adjusting pH value to 5；
Polyreaction film formation step is:
Chitin powder body and paraffin composite core material emulsion are warmed to 55 DEG C, maintain pH value 5, stir with 250r/min rotating speed, and with the performed polymer 375g of dropping at a slow speed of 18ml/min, after arrest reaction 120min, cool to 25 DEG C, then regulate pH value with sodium hydroxide and terminate reaction to 8.5；
Wash and dry and be:
With Fructus Citri Limoniae acid for adjusting pH value to 7.0, adding 10g carbamide, after stirring 6min with 110r/min rotating speed, vacuum filtration implements solid-liquid separation；Add 42 DEG C of hot ethanol 45ml and remove remaining Organic substance, with the dry 110min of 55 DEG C of temperature in vacuum drying oven after 45 DEG C of hot washes, i.e. prepare a kind of temperature control chitosan health-care microcapsule.
Embodiment 5
The preparation method of a kind of temperature control health care microcapsule, step is: prepares performed polymer and prepares heath-function antimicrobial pearl powder body and temperature and cause phase-change material n-octadecane composite core material emulsion polyreaction film forming and wash and dry；
Wherein, preparing performed polymer step is:
By formalin and distilled water mixing that tripolycyanamide that mass ratio is 1: 2: 1.8, concentration are 37wt%, regulate pH value to 9 with triethanolamine, be warmed up to 65 DEG C, with the low rate mixing of 200r/min to clear viscous shape liquid；Performed polymer total amount is by the 140% of n-octadecane quality；
Prepare heath-function antimicrobial pearl powder body and temperature to cause phase-change material n-octadecane composite core material emulsion step and be:
At 40 DEG C of temperature, by styrene-maleic anhydride copolymer sodium salt solution that 250g n-octadecane, 130g mass fraction are 18% and the mixing of 2000ml deionized water, with high speed 8000r/min emulsifying 40min；200g Margarita powder body (mean diameter 0.8 μm), 50g Zinc oxide powder (mean diameter 1 μm) and 30g propylene glycol block polyether is added after being heated to 95 DEG C with oil bath, continue with 500r/min rotating speed emulsifying 10min, cool to and regulate ph value of emulsion to 5 with the acetic acid that mass fraction is 10% after 30 DEG C；
Polyreaction film formation step is:
Margarita powder body, Zinc oxide powder and n-octadecane composite core material emulsion are warmed to 50 DEG C, maintain pH value 5, with the stirring of 200r/min rotating speed and with the performed polymer 350g of dropping at a slow speed of 10ml/min, after arrest reaction 150min, cool to 15 DEG C, then regulate pH value with sodium hydroxide and terminate reaction to 9；
Wash and dry and be:
With Fructus Citri Limoniae acid for adjusting pH value to 7.2, adding 12g carbamide, after stirring 7min with 100r/min rotating speed, vacuum filtration implements solid-liquid separation；Add 45 DEG C of hot ethanol 50ml and remove remaining Organic substance, with the dry 110min of 60 DEG C of temperature in vacuum drying oven after 40 DEG C of hot washes, i.e. prepare a kind of temperature control antimicrobial pearl health care microcapsule.
Claims (9)
1. a preparation method for temperature control health care microcapsule, is characterized in that step is: prepares performed polymer and prepares heath-function powder body and temperature and cause phase-change material composite core material emulsion polyreaction film forming and wash and dry；
Described performed polymer step of preparing is:
Tripolycyanamide, formalin and distilled water are mixed, regulates pH value to 8～9, be warmed up to 60～80 DEG C, with 200-500r/min low rate mixing to clear viscous shape liquid；
Described heath-function powder body of preparing causes phase-change material composite core material emulsion step with temperature and is:
At 40-50 DEG C of temperature, the temperature of fusing is caused after phase-change material, emulsifying agent and deionized water mix with high speed 6000-10000r/min emulsifying, then it is heated to 90-99 DEG C with oil bath, add heath-function powder body and dispersant, continue with after 400-600r/min rotating speed emulsifying 10～15min, cool to 30-40 DEG C, with weak acid for adjusting pH value to 5～6；
Described polyreaction film formation step is:
Heath-function powder body and temperature are caused phase-change material composite core material emulsion and is warmed to 50～60 DEG C, maintain pH value 5～6 and with the stirring of 200-500r/min rotating speed and drip at a slow speed performed polymer with 10～30ml/min, after arrest reaction 100～150min, cool to 15～25 DEG C, then regulate pH value with sodium hydroxide and terminate reaction to 8～9；
Described washing also dries and is:
Add carbamide and remove residual formaldehyde, with hot ethanol and hot wash after sucking filtration, then carry out vacuum drying.
2. the preparation method of a kind of temperature control health care microcapsule according to claim 1, it is characterised in that the mass ratio of tripolycyanamide, formalin and distilled water is 1: 1～2: 1～2；Wherein the concentration of formalin is 30～50wt%.
3. the preparation method of a kind of temperature control health care microcapsule according to claim 1, it is characterised in that it is 1: 0.5～2: 5～10 that temperature causes the mass ratio of phase-change material, emulsifying agent and deionized water；High speed emulsification times is 30～40min；The mass ratio of heath-function powder body and dispersant is 5～10: 1；The mass ratio that heath-function powder body causes phase-change material with temperature is 0.5～2: 1；Described dispersant is propylene glycol block polyether.
4. the preparation method of a kind of temperature control health care microcapsule according to claim 1, it is characterised in that it is 0.5～2: 1 that temperature causes the mass ratio of phase-change material and performed polymer.
5. a kind of temperature control health care microcapsule that prepared by the preparation method according to any one of above claim 1-4, is characterized in that: described temperature control health care microcapsule is by heath-function powder body and temperature causes the blended composite core material formed of phase-change material and the wall material being made up of high molecular polymer is formed；The mass ratio of described composite core material and wall material is 0.3～3: 1；Described heath-function powder body mean diameter≤1.2 μm；Mean diameter≤3 μm of described microcapsule.
6. a kind of temperature control health care microcapsule according to claim 5, it is characterised in that described heath-function powder body is that one or more in Margarita powder body, Chinese crude drug powder body, chitin powder body, antimicrobial powder, bamboo-carbon powder or magnetic material powder mix.
7. a kind of temperature control health care microcapsule according to claim 5, it is characterised in that it is that one or more in paraffin, crystalline hydrate salt, eutectic hydrated salt, Polyethylene Glycol or linear paraffin mix that described temperature causes phase-change material.
8. a kind of temperature control health care microcapsule according to claim 5, it is characterised in that the high molecular polymer of described wall material is polyureas, polyester resin, Lauxite, gelatin, poly-polyprotic acid or melamine resin.
9. a kind of temperature control health care microcapsule according to claim 5, it is characterised in that it is 0.5～2: 1 that the heath-function powder body in described composite core material and described temperature cause the mass ratio of phase-change material.
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