CN105316784A - Composite microcapsule additive containing phase change material and sarcandra glabra extract and application of composite microcapsule additive - Google Patents
Composite microcapsule additive containing phase change material and sarcandra glabra extract and application of composite microcapsule additive Download PDFInfo
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- CN105316784A CN105316784A CN201510874156.7A CN201510874156A CN105316784A CN 105316784 A CN105316784 A CN 105316784A CN 201510874156 A CN201510874156 A CN 201510874156A CN 105316784 A CN105316784 A CN 105316784A
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Abstract
The invention belongs to the technical field of functional cellulosic fibers and relates to a composite microcapsule additive containing a phase change material and sarcandra glabra extract. A preparation method comprises the following steps: adding the phase change material, an emulsifying agent, an initiator and distilled water into a heating device, and stirring to form a stable emulsifying solution; slowly dripping methyl methacrylate into the emulsifying solution, and carrying out a polymerization reaction after a pre-polymerization reaction; standing and washing with ethanol and filtering to obtain a solid matter; drying the solid matter to obtain a phase change material microcapsule; mixing the phase change material microcapsule with a sarcandra glabra extract solution, wherein the phase change material microcapsule sufficiently adsorbs the sarcandra glabra extract; drying the mixture to obtain the phase change material microcapsule adsorbing the sarcandra glabra extract on the surface; and adding the phase change material microcapsule into a porous starch ethanol solution to carry out adsorption; adding beta-cyclodextrin and emulsifying at a high speed to obtain composite microcapsule additive containing the phase change material and the sarcandra glabra extract from inside to outside. Sarcandra glabra viscose prepared by using the additive has good temprature adjusting and antibacterial functions.
Description
Technical field
The invention belongs to functional cellulose fibre technology field, specifically, relate to a kind of composite micro-capsule containing phase-change material and Herba Pileae Scriptae extract, for the preparation of Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function and preparation method thereof.
Background technology
Viscose goods have moisture absorption, good permeability and feature comfortable and easy to wear, obtain a wide range of applications.But China's viscose majority is conventional variety, functional fiber, fibre in differentiation kind are little, and therefore Devoting Major Efforts To Developing high-performance, differential viscose new varieties are Main way that field of viscose fiber develops.
Herba Pileae Scriptae extract is the non-volatile granulated brown solids of one extracted from Chloranthus glaber, there is clearing heat and detoxicating, expelling wind and activating blood flow, swelling and pain relieving and anti-inflammation effect, belong to bioactive materials, very easily decompose loss by strong acid, highly basic, Strong oxdiative and temperatures involved.
Chinese patent 201010140457.4 discloses a kind of viscose with antibacterial functions and preparation method thereof, wherein antiseptic is Herba Pileae Scriptae extract, solution is made by soluble in water for Herba Pileae Scriptae extract powder, be added to by the powder solution of Herba Pileae Scriptae extract in rayon spinning stoste, the powder addition of Herba Pileae Scriptae extract is 1% ~ 5% of rayon spinning stock solution quality; Then wet spinning spinning process is shaping routinely, obtains the viscose with Chloranthus glaber antibacterial functions.In the method, the powder solution joining day of Herba Pileae Scriptae extract is too early, Herba Pileae Scriptae extract severe decomposition is made in strong alkali environment, in wet spinning forming process, water-soluble Herba Pileae Scriptae extract additive stream vector is larger simultaneously, affect the functional of fiber, fiber function decay after repeatedly washing is rapid.
Chinese patent 201510176510.9 discloses a kind of preparation method of the viscose containing Herba Pileae Scriptae extract, the method comprises the following steps: the preparation of antimicrobial, add dispersant, add sodium carboxymethylcellulose, and spinning solution is blended, spinning and post processing; The preparation process of antimicrobial is that Herba Pileae Scriptae extract powder to be joined temperature be in the water of 25 ± 1 DEG C, and addition is 100g/1000ml water, is stirred well to powder and dissolves make antimicrobial A completely, adds obtained solution B after dispersant; This technical scheme is dissolved completely by antiseptic Herba Pileae Scriptae extract to make antimicrobial, then adds dispersant and sodium carboxymethylcellulose to improve dispersiveness and solution viscosity; Itself and spinning solution is blended, utilize conventional rayon spinning technique to carry out spinning, therefore also there is the problem run off in effective ingredient breakdown and forming process, the functional of fiber is weakened greatly.
Along with development and the growth in the living standard of science and technology, people are not only satisfied with the general demand to fiber textile, and high-performance, multi-functional fiber textile continue to bring out, and directly impact common market.Therefore, the development of multi-functional fiber is one of important directions of chemical fiber industry development.Phase-change material (PhaseChangeMaterial is called for short PCM) refers to and varies with temperature and change the material that form also can provide latent heat.Organic and inorganic phase-change material two class can be divided into again according to the composition of phase-change material.Phase-change material can undergo phase transition according to the change of ambient temperature, and absorbs or release heat from the external world, the substantially invariable micro climate of formation temperature around textiles, thus realizes temp regulating function.The main purpose of using phase-change material improves the comfortableness of textiles.
Therefore, how to realize the functional compound of phase-change material and Herba Pileae Scriptae extract, reduce decomposition and the loss of active ingredient in spinning process, prepare the Chloranthus glaber viscose having temp regulating function and antibacterial functions concurrently significant.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art existence, seek to design a kind of composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract, use it for the preparation of the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function, and the preparation method of the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function is provided.
To achieve these goals, the technical solution used in the present invention is: a kind of composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract, and its preparation method comprises the following steps:
Step 1: prepare phase-change material micro-capsule
Phase-change material, emulsifying agent, initator and distilled water are added in heater, 0.5 ~ 2.0h is stirred at 35 ~ 75 DEG C, make phase-change material form stable emulsion, wherein the mass ratio of phase-change material, emulsifying agent, initator and distilled water is 100:3 ~ 5:0.5 ~ 3:200 ~ 400;
Methyl methacrylate is slowly added drop-wise in above-mentioned emulsion, then at 55 ~ 85 DEG C, prepolymerization reaction is carried out, time is 1.0 ~ 2.5h, then be warming up to 80 ~ 90 DEG C and carry out polymerisation 5.0 ~ 8.0h, after reaction terminates, gained reactant liquor is left standstill, suction filtration, and obtaining solid matter with ethanol washing suction filtration, obtaining after drying with phase-change material is capsule-core, take polymethyl methacrylate as the phase-change material micro-capsule of cyst wall;
Preferably, in step 1, mixing speed is 500 ~ 1000rpm, and baking temperature is 40 ~ 60 DEG C;
Preferably, described phase-change material is the mixture of one or more in atoleine, hexadecane, n-octadecane, nonadecane, n-eicosane, Heneicosane and n-docosane;
Preferably, described emulsifying agent is the mixture of one or more in Tween-80, Span-80, lauryl sodium sulfate (SDS) and OP-10;
Preferably, described initator is benzoyl peroxide or azodiisobutyronitrile;
Preferably, the particle diameter of described phase-change material micro-capsule is D97≤1.6 μm;
Step 2: prepare composite micro-capsule additive
Be dissolved in by Herba Pileae Scriptae extract in distilled water, wherein the mass fraction of Herba Pileae Scriptae extract is 4.0% ~ 9.0%;
Phase-change material micro-capsule prepared by step 1 is mixed with Herba Pileae Scriptae extract dissolution homogeneity, static 1.5 ~ 4.0h, make phase-change material micro-capsule fully adsorb Herba Pileae Scriptae extract, dry at 40 ~ 60 DEG C, namely obtain the phase-change material micro-capsule that adsorption has Herba Pileae Scriptae extract; Wherein in phase-change material micro-capsule, in phase-change material and Herba Pileae Scriptae extract solution, the mass ratio of Herba Pileae Scriptae extract is 1 ~ 3:1 ~ 3;
Being had by adsorption the phase-change material micro-capsule of Herba Pileae Scriptae extract to join mass fraction is adsorb in the porous-starch ethanolic solution of 3.0% ~ 5.0%, the adsorption contained in solution has the mass fraction of the phase-change material micro-capsule of Herba Pileae Scriptae extract to be 20% ~ 30%, absorption duration is 0.5h ~ 2.0h, then beta-schardinger dextrin-is added, in solution, the mass fraction of beta-schardinger dextrin-is 5.0% ~ 8.0%, through 20 ~ 80min, rotating speed is after 5000 ~ 10000r/min emulsify at a high speed, the composite micro-capsule additive from inside to outside containing phase-change material and Herba Pileae Scriptae extract can be obtained,
Preferably, the described particle diameter containing the composite micro-capsule of phase-change material and Herba Pileae Scriptae extract is D97≤2.7 μm.
There is a preparation method for the Chloranthus glaber anti-bacterial fibre cellulose fiber of temp regulating function, comprise the following steps:
Step a: prepare co-blended spinning liquid
Take cellulose pulp as raw material, obtain viscose glue stoste through conventional viscose preparation technology, in viscose glue stoste, content of alphacellulose is 5.6% ~ 9.2%, and in viscose glue stoste, adds polyethylene glycol carry out sex change, obtains modified rayon stoste; Composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract is carried out standing and defoaming, front injection device is spun in utilization, composite micro-capsule additive after deaeration is added in modified rayon stoste, in Herba Pileae Scriptae extract in composite micro-capsule additive and viscose glue stoste, the mass ratio of alpha cellulose is 0.085 ~ 0.2:1, obtains co-blended spinning liquid;
Preferably, the molecular weight of described polyethylene glycol is 1000 ~ 2500, and addition is 0.5% ~ 2.0% of content of alphacellulose in viscose glue stoste;
Step b: spinning and post processing
Described co-blended spinning liquid carries out spinning by the coagulating bath adjusted, and nascent tow obtains shaping tow after drawing-off; Gained tow carries out concise through cutting off, relaxing sulfur removal technology, finish application bath and washing, dries, obtains the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function;
Preferably, in described coagulating bath, sulfuric acid concentration is 75 ~ 95g/L, sodium sulfate concentration is 260 ~ 290g/L, and zinc sulfate concentration is 25 ~ 35g/L.
Preferably, described desulfurization bath: Na
2sO
32.0 ~ 6.0g/L, oil bath: 1.5 ~ 6.0g/L, bake out temperature: 80 ~ 95 DEG C, drying time is 2.5 ~ 4.0h.
There is a Chloranthus glaber anti-bacterial fibre cellulose fiber for temp regulating function, the phase-change material containing 3.0 ~ 12.0wt% in the Chloranthus glaber anti-bacterial fibre cellulose fiber obtained by above-mentioned preparation method, the Herba Pileae Scriptae extract containing 3.0 ~ 10.0wt%.
Beneficial effect of the present invention is:
Adopt the preparation technology of composite micro-capsule, phase-change material is made to be positioned at the innermost layer of microcapsules, Herba Pileae Scriptae extract is outer at phase-change material, and outside also has the protection of cyst wall, not only ensure the stability of phase-change material and Herba Pileae Scriptae extract, utilize two kinds of materials to play one's part to the full simultaneously, obtained Chloranthus glaber viscose has good temperature and regulates and antibacterial functions, compared with conventional viscose, to inhibiting rate >=94.2% of staphylococcus aureus, to colibacillary inhibiting rate >=89.6%, to inhibiting rate >=91.5% of Candida albicans, melting enthalpy >=5.2J/g, crystallization enthalpy >=5.0J/g, textile process performance is good, wearability is excellent, can extensive use clothes, bedding, medical supplies and nonwoven material field.
There is the preparation method of the Chloranthus glaber antibacterial viscose fiber of temp regulating function, rational technology, simple.
Detailed description of the invention
Below by specific embodiment, the invention will be further described:
Embodiment 1
The composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract of the present embodiment, its preparation method comprises the following steps:
Step 1: prepare phase-change material micro-capsule
Phase-change material atoleine, emulsifying agent Tween-80, initator benzoyl peroxide and distilled water are added in heater, 2.0h is stirred with the rotating speed of 1000rpm at 35 DEG C, make phase-change material form stable emulsion, wherein the mass ratio of phase-change material, emulsifying agent, initator and distilled water is 100:3:0.5:200;
Methyl methacrylate is slowly added drop-wise in above-mentioned emulsion, then at 55 DEG C, prepolymerization reaction is carried out, time is 2.5h, then be warming up to 80 DEG C and carry out polymerisation 8.0h, after reaction terminates, gained reactant liquor is left standstill, suction filtration, and obtain solid matter with ethanol washing suction filtration, obtaining with phase-change material after drying under 40 DEG C of conditions is capsule-core, take polymethyl methacrylate as the phase-change material micro-capsule of cyst wall; The particle diameter D97 of phase-change material micro-capsule is 1.562 μm;
Step 2: prepare composite micro-capsule additive
Be dissolved in by Herba Pileae Scriptae extract in distilled water, wherein the mass fraction of Herba Pileae Scriptae extract is 9.0%, and Herba Pileae Scriptae extract obtains by buying;
Phase-change material micro-capsule prepared by step 1 is mixed with Herba Pileae Scriptae extract dissolution homogeneity, static 4.0h, make phase-change material micro-capsule fully adsorb Herba Pileae Scriptae extract, dry at 40 DEG C, namely obtain the phase-change material micro-capsule that adsorption has Herba Pileae Scriptae extract; Wherein in phase-change material micro-capsule, in phase-change material and Herba Pileae Scriptae extract solution, the mass ratio of Herba Pileae Scriptae extract is 1:1;
Being had by adsorption the phase-change material micro-capsule of Herba Pileae Scriptae extract to join mass fraction is adsorb in the porous-starch ethanolic solution of 3.0%, the adsorption contained in solution has the mass fraction of the phase-change material micro-capsule of Herba Pileae Scriptae extract to be 30%, absorption duration is 2.0h, then beta-schardinger dextrin-is added, in solution, the mass fraction of beta-schardinger dextrin-is 8.0%, through 20min, rotating speed is after 10000r/min emulsify at a high speed, can obtain the composite micro-capsule additive from inside to outside containing phase-change material and Herba Pileae Scriptae extract; The particle diameter D97 of the composite micro-capsule containing phase-change material and Herba Pileae Scriptae extract is 2.696 μm.
The preparation method with the Chloranthus glaber anti-bacterial fibre cellulose fiber of temp regulating function of the present embodiment, comprises the following steps:
Step a: prepare co-blended spinning liquid
Take cellulose pulp as raw material, viscose glue stoste is obtained through conventional viscose preparation technology, in viscose glue stoste, content of alphacellulose is 5.6%, and add in viscose glue stoste molecular weight be 1000 polyethylene glycol carry out sex change, addition is 0.5% of content of alphacellulose in viscose glue stoste, obtains modified rayon stoste; Composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract is carried out standing and defoaming, front injection device is spun in utilization, composite micro-capsule additive after deaeration is added in modified rayon stoste, in Herba Pileae Scriptae extract in composite micro-capsule additive and viscose glue stoste, the mass ratio of alpha cellulose is 0.2:1, obtains co-blended spinning liquid;
Step b: spinning and post processing
Co-blended spinning liquid carries out spinning by the coagulating bath adjusted, and in coagulating bath, sulfuric acid concentration is 75g/L, sodium sulfate concentration is 260g/L, and zinc sulfate concentration is 25g/L; Nascent tow obtains shaping tow after drawing-off; Gained tow carries out concise through cutting off, relaxing sulfur removal technology, finish application bath and washing, and dry, desulfurization is bathed: Na
2sO
32.0g/L, oil bath: 1.5g/L, bake out temperature: 80 DEG C, drying time is 4.0h, obtains the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function;
By the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function prepared by embodiment 1, compared with conventional viscose, to the inhibiting rate 97.6% of staphylococcus aureus, to colibacillary inhibiting rate 96.1%, to the inhibiting rate 96.8% of Candida albicans, melting enthalpy is 15.8J/g, crystallization enthalpy 14.3J/g, textile process performance is good, wearability is excellent, can extensive use clothes, bedding, medical supplies and nonwoven material field.
Embodiment 2:
The composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract of the present embodiment, its preparation method comprises the following steps:
Step 1: prepare phase-change material micro-capsule
Phase-change material hexadecane, emulsifying agent Span-80, initator azodiisobutyronitrile and distilled water are added in heater, 1.6h is stirred with the rotating speed of 912rpm at 42 DEG C, make phase-change material form stable emulsion, wherein the mass ratio of phase-change material, emulsifying agent, initator and distilled water is 100:3:0.5:250;
Methyl methacrylate is slowly added drop-wise in above-mentioned emulsion, then at 62 DEG C, prepolymerization reaction is carried out, time is 2.1h, then be warming up to 85 DEG C and carry out polymerisation 7.1h, after reaction terminates, gained reactant liquor is left standstill, suction filtration, and obtain solid matter with ethanol washing suction filtration, obtaining with phase-change material after drying under 46 DEG C of conditions is capsule-core, take polymethyl methacrylate as the phase-change material micro-capsule of cyst wall; The particle diameter D97 of phase-change material micro-capsule is 1.628 μm;
Step 2: prepare composite micro-capsule additive
Be dissolved in by Herba Pileae Scriptae extract in distilled water, wherein the mass fraction of Herba Pileae Scriptae extract is 8.2%;
Phase-change material micro-capsule prepared by step 1 is mixed with Herba Pileae Scriptae extract dissolution homogeneity, static 3.5h, make phase-change material micro-capsule fully adsorb Herba Pileae Scriptae extract, dry at 45 DEG C, namely obtain the phase-change material micro-capsule that adsorption has Herba Pileae Scriptae extract; Wherein in phase-change material micro-capsule, in phase-change material and Herba Pileae Scriptae extract solution, the mass ratio of Herba Pileae Scriptae extract is 3:2;
Being had by adsorption the phase-change material micro-capsule of Herba Pileae Scriptae extract to join mass fraction is adsorb in the porous-starch ethanolic solution of 3.3%, the adsorption contained in solution has the mass fraction of the phase-change material micro-capsule of Herba Pileae Scriptae extract to be 28%, absorption duration is 1.7h, then beta-schardinger dextrin-is added, in solution, the mass fraction of beta-schardinger dextrin-is 7.2%, through 39min, rotating speed is after 9120r/min emulsify at a high speed, can obtain the composite micro-capsule additive from inside to outside containing phase-change material and Herba Pileae Scriptae extract; The particle diameter D97 of the composite micro-capsule containing phase-change material and Herba Pileae Scriptae extract is 2.612 μm.
The preparation method with the Chloranthus glaber anti-bacterial fibre cellulose fiber of temp regulating function of the present embodiment, comprises the following steps:
Step a: prepare co-blended spinning liquid
Take cellulose pulp as raw material, viscose glue stoste is obtained through conventional viscose preparation technology, in viscose glue stoste, content of alphacellulose is 6.3%, and add in viscose glue stoste molecular weight be 1250 polyethylene glycol carry out sex change, addition is 1.0% of content of alphacellulose in viscose glue stoste, obtains modified rayon stoste; Composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract is carried out standing and defoaming, front injection device is spun in utilization, composite micro-capsule additive after deaeration is added in modified rayon stoste, in Herba Pileae Scriptae extract in composite micro-capsule additive and viscose glue stoste, the mass ratio of alpha cellulose is 0.165:1, obtains co-blended spinning liquid;
Step b: spinning and post processing
Co-blended spinning liquid carries out spinning by the coagulating bath adjusted, and in coagulating bath, sulfuric acid concentration is 82g/L, sodium sulfate concentration is 268g/L, and zinc sulfate concentration is 27.6g/L; Nascent tow obtains shaping tow after drawing-off; Gained tow carries out concise through cutting off, relaxing sulfur removal technology, finish application bath and washing, and dry, desulfurization is bathed: Na
2sO
33.2g/L, oil bath: 2.7g/L, bake out temperature: 85 DEG C, drying time is 3.5h, obtains the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function;
By the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function prepared by embodiment 2, compared with conventional viscose, to the inhibiting rate 96.2% of staphylococcus aureus, to colibacillary inhibiting rate 95.1%, to the inhibiting rate 95.6% of Candida albicans, melting enthalpy is 10.8J/g, and crystallization enthalpy is 9.9J/g, textile process performance is good, wearability is excellent, can extensive use clothes, bedding, medical supplies and nonwoven material field.
Embodiment 3:
The composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract of the present embodiment, its preparation method comprises the following steps:
Step 1: prepare phase-change material micro-capsule
Phase-change material n-octadecane, emulsifying agent Span-80, initator azodiisobutyronitrile and distilled water are added in heater, 1.3h is stirred with the rotating speed of 825rpm at 48 DEG C, make phase-change material form stable emulsion, wherein the mass ratio of phase-change material, emulsifying agent, initator and distilled water is 100:3.8:1.1:290;
Methyl methacrylate is slowly added drop-wise in above-mentioned emulsion, then at 71 DEG C, prepolymerization reaction is carried out, time is 1.7h, then be warming up to 88 DEG C and carry out polymerisation 6.3h, after reaction terminates, gained reactant liquor is left standstill, suction filtration, and obtain solid matter with ethanol washing suction filtration, obtaining with phase-change material after drying under 51 DEG C of conditions is capsule-core, take polymethyl methacrylate as the phase-change material micro-capsule of cyst wall; The particle diameter D97 of phase-change material micro-capsule is 1.329 μm;
Step 2: prepare composite micro-capsule additive
Be dissolved in by Herba Pileae Scriptae extract in distilled water, wherein the mass fraction of Herba Pileae Scriptae extract is 7.4%;
Phase-change material micro-capsule prepared by step 1 is mixed with Herba Pileae Scriptae extract dissolution homogeneity, static 2.9h, make phase-change material micro-capsule fully adsorb Herba Pileae Scriptae extract, dry at 51 DEG C, namely obtain the phase-change material micro-capsule that adsorption has Herba Pileae Scriptae extract; Wherein in phase-change material micro-capsule, in phase-change material and Herba Pileae Scriptae extract solution, the mass ratio of Herba Pileae Scriptae extract is 2:3;
Being had by adsorption the phase-change material micro-capsule of Herba Pileae Scriptae extract to join mass fraction is adsorb in the porous-starch ethanolic solution of 3.7%, the adsorption contained in solution has the mass fraction of the phase-change material micro-capsule of Herba Pileae Scriptae extract to be 25%, absorption duration is 1.5h, then beta-schardinger dextrin-is added, in solution, the mass fraction of beta-schardinger dextrin-is 6.4%, through 45min, rotating speed is after 8200r/min emulsify at a high speed, can obtain the composite micro-capsule additive from inside to outside containing phase-change material and Herba Pileae Scriptae extract; The particle diameter D97 of the composite micro-capsule containing phase-change material and Herba Pileae Scriptae extract is 2.963 μm.
The preparation method with the Chloranthus glaber anti-bacterial fibre cellulose fiber of temp regulating function of the present embodiment, comprises the following steps:
Step a: prepare co-blended spinning liquid
Take cellulose pulp as raw material, viscose glue stoste is obtained through conventional viscose preparation technology, in viscose glue stoste, content of alphacellulose is 7.5%, and add in viscose glue stoste molecular weight be 1500 polyethylene glycol carry out sex change, addition is 1.2% of content of alphacellulose in viscose glue stoste, obtains modified rayon stoste; Composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract is carried out standing and defoaming, front injection device is spun in utilization, composite micro-capsule additive after deaeration is added in modified rayon stoste, in Herba Pileae Scriptae extract in composite micro-capsule additive and viscose glue stoste, the mass ratio of alpha cellulose is 0.152:1, obtains co-blended spinning liquid;
Step b: spinning and post processing
Co-blended spinning liquid carries out spinning by the coagulating bath adjusted, and in coagulating bath, sulfuric acid concentration is 85g/L, sodium sulfate concentration is 275g/L, and zinc sulfate concentration is 29.2g/L; Nascent tow obtains shaping tow after drawing-off; Gained tow carries out concise through cutting off, relaxing sulfur removal technology, finish application bath and washing, and dry, desulfurization is bathed: Na
2sO
34.5g/L, oil bath: 3.9g/L, bake out temperature: 88 DEG C, drying time is 3.2h, obtains the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function;
By the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function prepared by embodiment 3, compared with conventional viscose, be 96.9% to the inhibiting rate of staphylococcus aureus, be 96.1% to colibacillary inhibiting rate, be 95.9% to the inhibiting rate of Candida albicans, melting enthalpy is 9.6J/g, and crystallization enthalpy is 8.6J/g, textile process performance is good, wearability is excellent, can extensive use clothes, bedding, medical supplies and nonwoven material field.
Embodiment 4:
The composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract of the present embodiment, its preparation method comprises the following steps:
Step 1: prepare phase-change material micro-capsule
Phase-change material n-eicosane, emulsifier sodium lauryl sulfate, initator benzoyl peroxide and distilled water are added in heater, 1h is stirred with the rotating speed of 756rpm at 55 DEG C, make phase-change material form stable emulsion, wherein the mass ratio of phase-change material, emulsifying agent, initator and distilled water is 100:4.2:1.7:320;
Methyl methacrylate is slowly added drop-wise in above-mentioned emulsion, then at 75 DEG C, prepolymerization reaction is carried out, time is 2h, then be warming up to 90 DEG C and carry out polymerisation 5h, after reaction terminates, gained reactant liquor is left standstill, suction filtration, and obtain solid matter with ethanol washing suction filtration, obtaining with phase-change material after drying under 56 DEG C of conditions is capsule-core, take polymethyl methacrylate as the phase-change material micro-capsule of cyst wall; The particle diameter D97 of phase-change material micro-capsule is 1.572 μm;
Step 2: prepare composite micro-capsule additive
Be dissolved in by Herba Pileae Scriptae extract in distilled water, wherein the mass fraction of Herba Pileae Scriptae extract is 6.5%;
Phase-change material micro-capsule prepared by step 1 is mixed with Herba Pileae Scriptae extract dissolution homogeneity, static 2h, make phase-change material micro-capsule fully adsorb Herba Pileae Scriptae extract, dry at 55 DEG C, namely obtain the phase-change material micro-capsule that adsorption has Herba Pileae Scriptae extract; Wherein in phase-change material micro-capsule, in phase-change material and Herba Pileae Scriptae extract solution, the mass ratio of Herba Pileae Scriptae extract is 2:1;
Being had by adsorption the phase-change material micro-capsule of Herba Pileae Scriptae extract to join mass fraction is adsorb in the porous-starch ethanolic solution of 3.5%, the adsorption contained in solution has the mass fraction of the phase-change material micro-capsule of Herba Pileae Scriptae extract to be 22%, absorption duration is 1.2h, then beta-schardinger dextrin-is added, in solution, the mass fraction of beta-schardinger dextrin-is 5.9%, through 56min, rotating speed is after 7160r/min emulsify at a high speed, can obtain the composite micro-capsule additive from inside to outside containing phase-change material and Herba Pileae Scriptae extract; The particle diameter D97 of the composite micro-capsule containing phase-change material and Herba Pileae Scriptae extract is 2.682 μm.
The preparation method with the Chloranthus glaber anti-bacterial fibre cellulose fiber of temp regulating function of the present embodiment, comprises the following steps:
Step a: prepare co-blended spinning liquid
Take cellulose pulp as raw material, viscose glue stoste is obtained through conventional viscose preparation technology, in viscose glue stoste, content of alphacellulose is 8.2%, and add in viscose glue stoste molecular weight be 1700 polyethylene glycol carry out sex change, addition is 1.5% of content of alphacellulose in viscose glue stoste, obtains modified rayon stoste; Composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract is carried out standing and defoaming, front injection device is spun in utilization, composite micro-capsule additive after deaeration is added in modified rayon stoste, in Herba Pileae Scriptae extract in composite micro-capsule additive and viscose glue stoste, the mass ratio of alpha cellulose is 0.136:1, obtains co-blended spinning liquid;
Step b: spinning and post processing
Co-blended spinning liquid carries out spinning by the coagulating bath adjusted, and in coagulating bath, sulfuric acid concentration is 91g/L, sodium sulfate concentration is 281g/L, and zinc sulfate concentration is 31.2g/L; Nascent tow obtains shaping tow after drawing-off; Gained tow carries out concise through cutting off, relaxing sulfur removal technology, finish application bath and washing, and dry, desulfurization is bathed: Na
2sO
35.2g/L, oil bath: 4.2g/L, bake out temperature: 98 DEG C, drying time is 3h, obtains the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function;
By the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function prepared by embodiment 4, compared with conventional viscose, be 95.2% to the inhibiting rate of staphylococcus aureus, be 94.3% to colibacillary inhibiting rate, be 94.7% to the inhibiting rate of Candida albicans, melting enthalpy is 11.9J/g, and crystallization enthalpy is 10.2J/g, textile process performance is good, wearability is excellent, can extensive use clothes, bedding, medical supplies and nonwoven material field.
Embodiment 5:
The composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract of the present embodiment, its preparation method comprises the following steps:
Step 1: prepare phase-change material micro-capsule
Phase-change material Heneicosane, emulsifier op-10, initator benzoyl peroxide and distilled water are added in heater, 0.8h is stirred with the rotating speed of 668rpm at 62 DEG C, make phase-change material form stable emulsion, wherein the mass ratio of phase-change material, emulsifying agent, initator and distilled water is 100:5.0:2.0:350;
Methyl methacrylate is slowly added drop-wise in above-mentioned emulsion, then at 81 DEG C, prepolymerization reaction is carried out, time is 1.2h, then be warming up to 89 DEG C and carry out polymerisation 5.2h, after reaction terminates, gained reactant liquor is left standstill, suction filtration, and obtain solid matter with ethanol washing suction filtration, obtaining with phase-change material after drying under 58 DEG C of conditions is capsule-core, take polymethyl methacrylate as the phase-change material micro-capsule of cyst wall; The particle diameter D97 of phase-change material micro-capsule is 1.459 μm;
Step 2: prepare composite micro-capsule additive
Be dissolved in by Herba Pileae Scriptae extract in distilled water, wherein the mass fraction of Herba Pileae Scriptae extract is 5.1%;
Phase-change material micro-capsule prepared by step 1 is mixed with Herba Pileae Scriptae extract dissolution homogeneity, static 1.6h, make phase-change material micro-capsule fully adsorb Herba Pileae Scriptae extract, dry at 58 DEG C, namely obtain the phase-change material micro-capsule that adsorption has Herba Pileae Scriptae extract; Wherein in phase-change material micro-capsule, in phase-change material and Herba Pileae Scriptae extract solution, the mass ratio of Herba Pileae Scriptae extract is 2:1;
Being had by adsorption the phase-change material micro-capsule of Herba Pileae Scriptae extract to join mass fraction is adsorb in the porous-starch ethanolic solution of 4.1%, the adsorption contained in solution has the mass fraction of the phase-change material micro-capsule of Herba Pileae Scriptae extract to be 20%, absorption duration is 1.0h, then beta-schardinger dextrin-is added, in solution, the mass fraction of beta-schardinger dextrin-is 5.5%, through 65min, rotating speed is after 6580r/min emulsify at a high speed, can obtain the composite micro-capsule additive from inside to outside containing phase-change material and Herba Pileae Scriptae extract; The particle diameter D97 of the composite micro-capsule containing phase-change material and Herba Pileae Scriptae extract is 2.7426 μm.
The preparation method with the Chloranthus glaber anti-bacterial fibre cellulose fiber of temp regulating function of the present embodiment, comprises the following steps:
Step a: prepare co-blended spinning liquid
Take cellulose pulp as raw material, viscose glue stoste is obtained through conventional viscose preparation technology, in viscose glue stoste, content of alphacellulose is 8.9%, and add in viscose glue stoste molecular weight be 2000 polyethylene glycol carry out sex change, addition is 1.7% of content of alphacellulose in viscose glue stoste, obtains modified rayon stoste; Composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract is carried out standing and defoaming, front injection device is spun in utilization, composite micro-capsule additive after deaeration is added in modified rayon stoste, in Herba Pileae Scriptae extract in composite micro-capsule additive and viscose glue stoste, the mass ratio of alpha cellulose is 0.109:1, obtains co-blended spinning liquid;
Step b: spinning and post processing
Co-blended spinning liquid carries out spinning by the coagulating bath adjusted, and in coagulating bath, sulfuric acid concentration is 93g/L, sodium sulfate concentration is 290g/L, and zinc sulfate concentration is 33.6g/L; Nascent tow obtains shaping tow after drawing-off; Gained tow carries out concise through cutting off, relaxing sulfur removal technology, finish application bath and washing, and dry, desulfurization is bathed: Na
2sO
35.8g/L, oil bath: 4.8g/L, bake out temperature: 92 DEG C, drying time is 3.5h, obtains the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function;
By the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function prepared by embodiment 5, compared with conventional viscose, be 96.1% to the inhibiting rate of staphylococcus aureus, be 95.8% to colibacillary inhibiting rate, be 93.9% to the inhibiting rate of Candida albicans, melting enthalpy is 8.8J/g, and crystallization enthalpy is 7.6J/g, textile process performance is good, wearability is excellent, can extensive use clothes, bedding, medical supplies and nonwoven material field.
Embodiment 6:
The composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract of the present embodiment, its preparation method comprises the following steps:
Step 1: prepare phase-change material micro-capsule
Phase-change material Heneicosane and n-docosane, emulsifying agent Span-80, initator azodiisobutyronitrile and distilled water are added in heater, 0.5h is stirred with the rotating speed of 500rpm at 75 DEG C, make phase-change material form stable emulsion, wherein the mass ratio of phase-change material, emulsifying agent, initator and distilled water is 100:5.0:3.0:400;
Methyl methacrylate is slowly added drop-wise in above-mentioned emulsion, then at 85 DEG C, prepolymerization reaction is carried out, time is 1h, then be warming up to 90 DEG C and carry out polymerisation 5h, after reaction terminates, gained reactant liquor is left standstill, suction filtration, and obtain solid matter with ethanol washing suction filtration, obtaining with phase-change material after drying under 60 DEG C of conditions is capsule-core, take polymethyl methacrylate as the phase-change material micro-capsule of cyst wall; The particle diameter D97 of phase-change material micro-capsule is 1.358 μm;
Step 2: prepare composite micro-capsule additive
Be dissolved in by Herba Pileae Scriptae extract in distilled water, wherein the mass fraction of Herba Pileae Scriptae extract is 4.0%;
Phase-change material micro-capsule prepared by step 1 is mixed with Herba Pileae Scriptae extract dissolution homogeneity, static 1.5h, make phase-change material micro-capsule fully adsorb Herba Pileae Scriptae extract, dry at 60 DEG C, namely obtain the phase-change material micro-capsule that adsorption has Herba Pileae Scriptae extract; Wherein in phase-change material micro-capsule, in phase-change material and Herba Pileae Scriptae extract solution, the mass ratio of Herba Pileae Scriptae extract is 3:2;
Being had by adsorption the phase-change material micro-capsule of Herba Pileae Scriptae extract to join mass fraction is adsorb in the porous-starch ethanolic solution of 5.0%, the adsorption contained in solution has the mass fraction of the phase-change material micro-capsule of Herba Pileae Scriptae extract to be 30%, absorption duration is 0.5h, then beta-schardinger dextrin-is added, in solution, the mass fraction of beta-schardinger dextrin-is 5.0%, through 80min, rotating speed is after 5000r/min emulsify at a high speed, can obtain the composite micro-capsule additive from inside to outside containing phase-change material and Herba Pileae Scriptae extract; The particle diameter D97 of the composite micro-capsule containing phase-change material and Herba Pileae Scriptae extract is 2.628 μm.
The preparation method with the Chloranthus glaber anti-bacterial fibre cellulose fiber of temp regulating function of the present embodiment, comprises the following steps:
Step a: prepare co-blended spinning liquid
Take cellulose pulp as raw material, viscose glue stoste is obtained through conventional viscose preparation technology, in viscose glue stoste, content of alphacellulose is 9.2%, and add in viscose glue stoste molecular weight be 2500 polyethylene glycol carry out sex change, addition is 2.0% of content of alphacellulose in viscose glue stoste, obtains modified rayon stoste; Composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract is carried out standing and defoaming, front injection device is spun in utilization, composite micro-capsule additive after deaeration is added in modified rayon stoste, in Herba Pileae Scriptae extract in composite micro-capsule additive and viscose glue stoste, the mass ratio of alpha cellulose is 0.085:1, obtains co-blended spinning liquid;
Step b: spinning and post processing
Co-blended spinning liquid carries out spinning by the coagulating bath adjusted, and in coagulating bath, sulfuric acid concentration is 95g/L, sodium sulfate concentration is 290g/L, and zinc sulfate concentration is 35g/L; Nascent tow obtains shaping tow after drawing-off; Gained tow carries out concise through cutting off, relaxing sulfur removal technology, finish application bath and washing, and dry, desulfurization is bathed: Na
2sO
36g/L, oil bath: 6g/L, bake out temperature: 95 DEG C, drying time is 2.5h, obtains the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function;
By the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function prepared by embodiment 6, compared with conventional viscose, to the inhibiting rate 94.8% of staphylococcus aureus, to colibacillary inhibiting rate 91.2%, to the inhibiting rate 92.6% of Candida albicans, melting enthalpy is 6.2J/g, and crystallization enthalpy is 5.8J/g, textile process performance is good, wearability is excellent, can extensive use clothes, bedding, medical supplies and nonwoven material field.
Claims (10)
1. contain a composite micro-capsule additive for phase-change material and Herba Pileae Scriptae extract, it is characterized in that, its preparation method comprises the following steps:
Step 1: prepare phase-change material micro-capsule
Phase-change material, emulsifying agent, initator and distilled water are added in heater, 0.5 ~ 2.0h is stirred at 35 ~ 75 DEG C, make phase-change material form stable emulsion, wherein the mass ratio of phase-change material, emulsifying agent, initator and distilled water is 100:3 ~ 5:0.5 ~ 3:200 ~ 400;
Methyl methacrylate is slowly added drop-wise in above-mentioned emulsion, then at 55 ~ 85 DEG C, prepolymerization reaction is carried out, time is 1.0 ~ 2.5h, then be warming up to 80 ~ 90 DEG C and carry out polymerisation 5.0 ~ 8.0h, after reaction terminates, gained reactant liquor is left standstill, suction filtration, and obtaining solid matter with ethanol washing suction filtration, obtaining after drying with phase-change material is capsule-core, take polymethyl methacrylate as the phase-change material micro-capsule of cyst wall;
Step 2: prepare composite micro-capsule additive
Be dissolved in by Herba Pileae Scriptae extract in distilled water, wherein the mass fraction of Herba Pileae Scriptae extract is 4.0% ~ 9.0%;
Phase-change material micro-capsule prepared by step 1 is mixed with Herba Pileae Scriptae extract dissolution homogeneity, static 1.5 ~ 4.0h, make phase-change material micro-capsule fully adsorb Herba Pileae Scriptae extract, dry at 40 ~ 60 DEG C, namely obtain the phase-change material micro-capsule that adsorption has Herba Pileae Scriptae extract; Wherein in phase-change material micro-capsule, in phase-change material and Herba Pileae Scriptae extract solution, the mass ratio of Herba Pileae Scriptae extract is 1 ~ 3:1 ~ 3;
Being had by adsorption the phase-change material micro-capsule of Herba Pileae Scriptae extract to join mass fraction is adsorb in the porous-starch ethanolic solution of 3.0% ~ 5.0%, the adsorption contained in solution has the mass fraction of the phase-change material micro-capsule of Herba Pileae Scriptae extract to be 20% ~ 30%, absorption duration is 0.5h ~ 2.0h, then beta-schardinger dextrin-is added, in solution, the mass fraction of beta-schardinger dextrin-is 5.0% ~ 8.0%, through 20 ~ 80min, rotating speed is after 5000 ~ 10000r/min emulsify at a high speed, the composite micro-capsule additive from inside to outside containing phase-change material and Herba Pileae Scriptae extract can be obtained.
2. the composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract according to claim 1, it is characterized in that, in described step 1, mixing speed is 500 ~ 1000rpm, and baking temperature is 40 ~ 60 DEG C.
3. the composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract according to claim 1, it is characterized in that, described phase-change material is the mixture of one or more in atoleine, hexadecane, n-octadecane, nonadecane, n-eicosane, Heneicosane and n-docosane.
4. the composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract according to claim 1, it is characterized in that, described emulsifying agent is the mixture of one or more in Tween-80, Span-80, lauryl sodium sulfate and OP-10.
5. the composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract according to claim 1, it is characterized in that, described initator is benzoyl peroxide or azodiisobutyronitrile.
6. the composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract according to claim 1, it is characterized in that, the particle diameter of described phase-change material micro-capsule is less than or equal to 1.6 μm; The described particle diameter containing the composite micro-capsule of phase-change material and Herba Pileae Scriptae extract is less than or equal to 2.7 μm.
7. there is a preparation method for the Chloranthus glaber anti-bacterial fibre cellulose fiber of temp regulating function, it is characterized in that, comprise the following steps:
Step a: prepare co-blended spinning liquid
Take cellulose pulp as raw material, obtain viscose glue stoste through conventional viscose preparation technology, in viscose glue stoste, content of alphacellulose is 5.6% ~ 9.2%, and in viscose glue stoste, adds polyethylene glycol carry out sex change, obtains modified rayon stoste; Composite micro-capsule additive containing phase-change material and Herba Pileae Scriptae extract according to claim 1 is carried out standing and defoaming, front injection device is spun in utilization, composite micro-capsule additive after deaeration is added in modified rayon stoste, in Herba Pileae Scriptae extract in composite micro-capsule additive and viscose glue stoste, the mass ratio of alpha cellulose is 0.085 ~ 0.2:1, obtains co-blended spinning liquid;
Step b: spinning and post processing
Described co-blended spinning liquid carries out spinning by the coagulating bath adjusted, and nascent tow obtains shaping tow after drawing-off; Gained tow carries out concise through cutting off, relaxing sulfur removal technology, finish application bath and washing, dries, obtains the Chloranthus glaber anti-bacterial fibre cellulose fiber with temp regulating function.
8. the preparation method with the Chloranthus glaber anti-bacterial fibre cellulose fiber of temp regulating function according to claim 7, it is characterized in that, the molecular weight of described polyethylene glycol is 1000 ~ 2500, and addition is 0.5% ~ 2.0% of content of alphacellulose in viscose glue stoste.
9. the preparation method with the Chloranthus glaber anti-bacterial fibre cellulose fiber of temp regulating function according to claim 7, it is characterized in that, in described coagulating bath, sulfuric acid concentration is 75 ~ 95g/L, sodium sulfate concentration is 260 ~ 290g/L, and zinc sulfate concentration is 25 ~ 35g/L; Described desulfurization bath: Na
2sO
32.0 ~ 6.0g/L, oil bath: 1.5 ~ 6.0g/L, bake out temperature: 80 ~ 95 DEG C, drying time is 2.5 ~ 4.0h.
10. one kind has the Chloranthus glaber anti-bacterial fibre cellulose fiber of temp regulating function, the phase-change material had containing 3.0 ~ 12.0wt% in the Chloranthus glaber anti-bacterial fibre cellulose fiber obtained by preparation method of the Chloranthus glaber anti-bacterial fibre cellulose fiber of temp regulating function according to claim 7, the Herba Pileae Scriptae extract containing 3.0 ~ 10.0wt%.
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