CN104131469A - Nano microcapsule material having self-repairing and wear-resisting functions and preparation method thereof - Google Patents
Nano microcapsule material having self-repairing and wear-resisting functions and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a nano microcapsule material and a preparation method thereof. The nano microcapsule material comprises a fabric base body prepared by fibers, and particularly also comprises a wall material cladded outside fiber-forming filaments and having nanoscale thickness; the wall material and the fibers form a nano microcapsule structure with the fiber-forming fine filaments as a 'core' and the wall material as a 'capsule sheath', the capsule sheath has adhesion, after being cladded with the capsule sheath, the fiber fine filaments are in mutual adhesion, so as to block gaps between the fibers; the fabric is used for production of ultra light and thin down jackets, can achieve quite good effect of penetration resistance to feathers, and cannot cause the fabric to become thick and gain weight and affect the wear comfort; and in addition, other properties of the fabric can be modified through introduction of functional auxiliary agents into the capsule sheath, for example, wear resistance of the fabric can effectively be enhanced through introduction of nano silica, or for example, the service life of the material can be effectively prolonged through introduction of self-repairing groups.
Description
Technical field
The present invention relates to a kind of preparation method and application that are particularly suitable for material and this material of making ultra-thin down jackets.
Background technology
Ultra-thin down jackets only have tens to one or two hectogram weights, after folding, can put into a pocket that palm is large, liked by Young vogue personage, as the warming dress ornament of high-grade fashion of new rise, require fabric frivolous, soft, warming, moisture-inhibiting perspire, anti-chiseling down, color is gorgeous, glossiness is high, wear-resistant, water and oil repellant.Ultra-thin feather dress fabric generally adopts 30D, fine denier nylon fabric below 410T.This face liber is thin, and yarn count density is low, especially easily bores suede, and easily tears and wear and tear.The problem of ultra-thin down jackets maximum is bored suede and cracky exactly, and traditional calendering technique is inoperative to superfine fibre, and top finish and RESIN FINISH can reduce again fabric gas permeability, and dress is felt oppressed, and increases fabric weight, is unsuitable for ultra-thin down jackets.
Summary of the invention
Technical problem to be solved by this invention overcome the deficiencies in the prior art, a kind of Nano capsule material that is suitable for making ultra-thin down jackets is provided.
The present invention provides a kind of preparation method who is suitable for the Nano capsule material of making ultra-thin down jackets simultaneously.
For overcoming the above problems, a kind of technical scheme that the present invention takes is as follows:
A kind of capsule of nano material, it comprises the fabric matrix of being made up of fiber, and particularly, described Nano capsule material also comprises and is coated on that fiber is outer, thickness is nano level wall material, wall material and fiber form taking fiber as " core ", the capsule of nano structure taking wall material as " capsule sheath ".
Preferably, described fabric matrix is the Nylon Taffeta of 380 ~ 420T, 10 ~ 30D, 24/48F, the Polyester Taffeta of 380 ~ 420T, 10 ~ 30D, 24/48F, or the spring Asia of 330 ~ 400T, 20 ~ 40D, 24/48/72/96F is spun.
According to the present invention, wall material can be prepared by conventional Micro-Encapsulation Technique, and concrete for example filmogen of material can need to be selected according to the application of material, is not particularly limited.
As the preferred embodiments of the invention: be used to form in the filmogen of wall material and contain ultraviolet excitation selfreparing group.Further preferably, filmogen is the polymer that obtains of modification of chitosan and trithiocarbonate generation cross-linking reaction or the mixture of this polymer and gelatin.
Also preferably, in described wall material, contain abrasion-resistant powder, preferably nano silicon.
Preferably, described capsule of nano material is by carrying out encapsulated arrangement and carry out subsequently satinage obtaining to fabric matrix with microcapsule dressing agent, described microcapsule dressing agent comprises filmogen, auxiliary agent, organic solvent and water, and described auxiliary agent at least comprises emulsifying agent and abrasion-resistant powder.
According to a concrete and preferred aspect, described capsule of nano material makes as follows:
(1) chitin modified: acetic acid solution is added in reactor, under nitrogen protection, add shitosan, be heated to 60 ~ 70 DEG C and be stirred to shitosan and dissolve completely, add ammonium persulfate, N, N '-methylene-bisacrylamide and acrylic acid, at 50 ~ 70 DEG C, react 3 ~ 5 hours, stop reaction, add ethanol, stir 20 ~ 40 minutes, add alkali and regulate pH to 6.8 ~ 7.2, filter, washing, by soaked in absolute ethyl alcohol more than 12 hours, take out, vacuumize, obtain white velvet-like solid, acetic acid in described acetic acid solution, shitosan, ammonium persulfate, N, N '-methylene-bisacrylamide and acrylic acid mass ratio that feeds intake are followed successively by 2 ~ 5:10 ~ 20:1 ~ 2:0.2 ~ 0.5:1 ~ 2,
(2) introduce selfreparing group: velvet-like above-mentioned white solid, trithiocarbonate, ether, azodiisobutyronitrile are added in reactor according to the ratio of mol ratio 2 ~ 5:50 ~ 60:100 ~ 120:1 ~ 2, carry out 2 ~ 4 freeze-thaw-degassed circulations, then at 60 ~ 80 DEG C of nitrogen protection and temperature, insulation reaction 4 ~ 6 hours, obtain cross-linked polymer, after purifying vacuumize, obtain faint yellow solid material;
(3) prepare microcapsule dressing agent: by gelatin, positive nonane, OP-10 emulsifying agent and nano silicon add in distilled water, after mixing, at 60 DEG C ~ 70 DEG C, dissolve, after dissolving, in high-shear emulsion machine, carry out emulsification, obtain emulsion, wherein gelatin, positive nonane, OP-10 emulsifying agent, the mass ratio of nano silicon and distilled water is followed successively by 0.5 ~ 0.6:1 ~ 2:0.2 ~ 0.5:1 ~ 2:100, taking out emulsion joins in reactor, adding volume is the distilled water diluting of 1 ~ 1.5 times of emulsion volume, 40 ~ 50 DEG C of temperature with under stirring, add the faint yellow solid material of step (2) gained, and regulate with the sodium hydroxide solution of 10wt% ~ 15wt% between pH to 5.5 ~ 6.5 of reactant liquor, finally add CALCIUM CHLORIDE DIHYDRATE, isothermal reaction 30 ~ 60min, obtain microcapsule dressing agent, the mass fraction that described faint yellow solid material and CALCIUM CHLORIDE DIHYDRATE account for microcapsule dressing agent is respectively 2% ~ 3% and 0.2% ~ 0.5%,
(4) form wall material: the prepared microcapsule dressing agent of step (3) is joined in impregnation container, fabric is immersed in microcapsule dressing agent, then add glutaraldehyde cross-linking agent, under agitation crosslinking curing 60 ~ 90min, after add again glycerine, after stirring fully, fabric moisture is extruded, dry, enter calender, 180 ~ 190 DEG C of temperature, under pressure 8 ~ 10MP, carry out roll compacting, obtain described capsule of nano material, the quality that feeds intake of described glutaraldehyde cross-linking agent and glycerine accounts for respectively 0.5% ~ 0.6% and 2% ~ 3% of the quality that always feeds intake.
According to the present invention, the thickness of described wall material is preferably 5 ~ 20nm, more preferably 5 ~ 10nm.
The another technical scheme that the present invention takes is: a kind of preparation method of capsule of nano material, and it comprises the following steps:
(1) chitin modified: acetic acid solution is added in reactor, under nitrogen protection, add shitosan, be heated to 60 ~ 70 DEG C and be stirred to shitosan and dissolve completely, add ammonium persulfate, N, N '-methylene-bisacrylamide and acrylic acid, at 50 ~ 70 DEG C, react 3 ~ 5 hours, stop reaction, add ethanol, stir 20 ~ 40 minutes, add alkali and regulate pH to 6.8 ~ 7.2, filter, washing, by soaked in absolute ethyl alcohol more than 12 hours, take out, vacuumize, obtain white velvet-like solid, acetic acid in described acetic acid solution, shitosan, ammonium persulfate, N, N '-methylene-bisacrylamide and acrylic acid mass ratio that feeds intake are followed successively by 2 ~ 5:10 ~ 20:1 ~ 2:0.2 ~ 0.5:1 ~ 2,
(2) introduce selfreparing group: velvet-like above-mentioned white solid, trithiocarbonate, ether, azodiisobutyronitrile are added in reactor according to the ratio of mol ratio 2 ~ 5:50 ~ 60:100 ~ 120:1 ~ 2, carry out 2 ~ 4 freeze-thaw-degassed circulations, then at 60 ~ 80 DEG C of nitrogen protection and temperature, insulation reaction 4 ~ 6 hours, obtain cross-linked polymer, after purifying vacuumize, obtain faint yellow solid material;
(3) prepare microcapsule dressing agent: by gelatin, positive nonane, OP-10 emulsifying agent and nano silicon add in distilled water, after mixing, at 60 DEG C ~ 70 DEG C, dissolve, after dissolving, in high-shear emulsion machine, carry out emulsification, obtain emulsion, wherein gelatin, positive nonane, OP-10 emulsifying agent, the mass ratio of nano silicon and distilled water is followed successively by 0.5 ~ 0.6:1 ~ 2:0.2 ~ 0.5:1 ~ 2:100, taking out emulsion joins in reactor, adding volume is the distilled water diluting of 1 ~ 1.5 times of emulsion volume, 40 ~ 50 DEG C of temperature with under stirring, add the faint yellow solid material of step (2) gained, and regulate with the sodium hydroxide solution of 10wt% ~ 15wt% between pH to 5.5 ~ 6.5 of reactant liquor, finally add CALCIUM CHLORIDE DIHYDRATE, isothermal reaction 30 ~ 60min, obtain microcapsule dressing agent, the mass fraction that described faint yellow solid material and CALCIUM CHLORIDE DIHYDRATE account for microcapsule dressing agent is respectively 2% ~ 3% and 0.2% ~ 0.5%,
(4) form wall material: the prepared microcapsule dressing agent of step (3) is joined in impregnation container, fabric is immersed in microcapsule dressing agent, then add glutaraldehyde cross-linking agent, under agitation crosslinking curing 60 ~ 90min, after add again glycerine, after stirring fully, fabric moisture is extruded, dry, enter calender, 180 ~ 190 DEG C of temperature, under pressure 8 ~ 10MP, carry out roll compacting, obtain described capsule of nano material, the quality that feeds intake of described glutaraldehyde cross-linking agent and glycerine accounts for respectively 0.5% ~ 0.6% and 2% ~ 3% of the quality that always feeds intake.
According to the inventive method preferred aspect, described fiber is superfine fibre, and the dawn, number was between 10 ~ 40D.Described fabric is preferably those that are suitable for making ultra-thin down jackets, include but not limited to the Nylon Taffeta of 380 ~ 420T, 10 ~ 30D, 24/48F, the Polyester Taffeta of 380 ~ 420T, 10 ~ 30D, 24/48F, or the spring Asia of 330 ~ 400T, 20 ~ 40D, 24/48/72/96F is spun.
The present invention is also particularly related to a kind of ultra-thin down jackets, and it adopts the above-mentioned capsule of nano material of the present invention as fabric.These down jackets have extraordinary anti-chiseling down effect, not cracky, and good permeability, lightweight.
Due to the employing of above technical scheme, the present invention compared with prior art has following advantage:
Creative utilization capsule of nano technology of the present invention is carried out modification to fabric and is obtained capsule of nano fabric, this face liber surface is formed with capsule sheath, capsule sheath between the adjacent silk thread of composition fabric can occur to adhere to and space between fill fiber, thereby strengthen the anti-chiseling down performance of fabric, simultaneously, because the thickness of capsule sheath is only an one thousandth of fiber filaments diameter, can not cause the weightening finish of fabric thickening.This fabric is used for making ultra-thin down jackets and both can have reached extraordinary anti-chiseling down effect, can not cause again the weightening finish of fabric thickening and affect sense comfortable and easy to wear; In addition, can also carry out modification to other performances of fabric by introduce functional aid in capsule sheath, for example, introduce the ABRASION RESISTANCE that can effectively strengthen fabric after nano silicon, for example, introduce selfreparing group, can effectively extend the service life of material.
Have excellent perspire moisture-inhibiting, anti-suede, the function such as antibacterial, wear-resisting according to the prepared capsule of nano material of the preparation method of capsule of nano material of the present invention, and obviously do not increase with common fabric phase weight/power ratio, wearing comfort does not reduce.
Ultra-thin down jackets of the present invention, owing to adopting capsule of nano material as fabric, not only have extraordinary anti-chiseling down effect, and not cracky is lightweight, and perspire poisture-penetrability is good, comfortable and easy to wear.
Detailed description of the invention
Microcapsules technology starts to be applied to industrial production in the 1950's, so-called microcapsules are exactly by some macromolecular compound or inorganic compound for certain material, adopt machinery or chemical method to be coated, granulation diameter is at 1 ~ 500 μ m, be wrapped by thing and be called " core ", coating is called " wall material " or " cyst wall ", and microcapsules are stable solid particle under normal conditions, and original character of this material is not suffered a loss, can discharge again under proper condition.Microcapsules technology is widely used in finishing functions of textile fabrics processing, can obtain the effect that conventional arrangement cannot obtain, comprise fire-retardant, wrinkle resistant, shrinkproof, refuse water, refuse oil, antistatic, soft, antibacterial, desinsection, fragrance texts.
Along with the development of nanometer technology, microcapsules research and development also enter nanoscale, particle diameter arrives between hundreds of nanometer tens, wall thickness only has several nanometers, cyst wall synthetic material is generally biodegradable polymer, as paracyanogen base propenyl Arrcostab, PLA and polycaprolactone, gelatin, Arabic gum and shitosan etc., human body is had no side effect, can be used for the industries such as food weaving.Wherein shitosan, as natural material, has no side effect to human body, is applied to spinning post-finishing industry and can produces the effects such as wrinkle resistant, antibacterial, antistatic, lubricated, moisture-inhibiting.
The production of chemical fibre is to synthesize mass of fibers by tens spinneret orifices ejection filaments, and the F number of fiber is spinneret orifice number, is generally 12,24,36,48,96 etc., and the diameter of a filament is probably 10 microns of left and right.If the core using a filament as microcapsules, adopt capsule of nano technology, in filament outside, coated a layer thickness is nanoscale the wall material with specific function, form the functional capsule sheath of one deck in fiber filaments outside, will solve the indeterminable problem of a lot of ordinary skills, but yet there are no the report of this aspect.
Ultraviolet excitation self-repair technology is a kind of technology of rising recent years, adopts the structure of reversible covalent bonds control material, can prepare reversible self-repair material.Can repeatedly there is cross-linking reaction at fracture position in this class material; thereby possesses repeatedly repair function; the base materials employed trithiocarbonate polymeric material that is generally; its repair mechanisms are as follows: under UV-irradiation; a C-S key homolysis in polymer in trithiocarbonic acid ester group, generates two free radicals, and this free radical is very active; be easy to react and form new C-S key with other trithiocarbonate, break other molecular links and produce again new free radical simultaneously.This chain reaction meeting is carried out always, until after illumination stops, free radical is combined into trithiocarbonic acid ester group again, gets back to resting state.Therefore this class material has under ultraviolet light the function of selfreparing repeatedly, and such material is introduced to capsule of nano material, is applied to after-finishing of textile products industry, can extend the service life of textiles, but has no at present the report of related fields.
If capsule of nano technology is applied to the rear arrangement finishing technique of thin denier fabric, in cyst material, introduce simultaneously can self-regeneration group, and wear-resisting composition, add the effects such as moisture-inhibiting that microencapsulation material itself has, antibacterial, soft, adhesiveness, through the processing of certain technique, face liber filament surfaces forms Functional capsule sheath, cyst wall between adjacent filament will adhere to, space between fill fiber, strengthen the anti-suede performance of fabric, make fabric there is perspire moisture-inhibiting, anti-suede, the function such as antibacterial, wear-resisting simultaneously.In addition, the thickness of cyst wall only has an one thousandth of fiber filaments diameter, can not cause the weightening finish of cloth thickening, affects the use of fabric in ultra-thin down jackets industry.
Below in conjunction with specific embodiment, the present invention will be further described in detail.Following examples compared with prior art main innovation and advantage have:
(1) form easy moisture-inhibiting on fiber filaments surface first, antibacterial, soft, the good capsule of nano sheath of adhesiveness, this microcapsules sheath forms the coating film of one deck nanometer grade thickness on fiber filaments surface, by separated between filament, mutually be adhered together by the adhesiveness of coating film again, rolling through calender in the situation that adding lubricant, fibrous inside filament spreads out, gap between filament and interfibrous gap are wrapped by film and fill up, so just form good anti-chiseling down, this tunic has good perspire poisture-penetrability simultaneously, can not lower the comfort level of clothes dress.And coating film thickness only has the one thousandth of fiber filaments diameter, can not increase the mass area ratio of cloth, do not affect the frivolous property of clothes
(2) first ultraviolet is activated to self-repair function group and introduce microencapsulation material, and be applied to after-finishing of textile products technique, make fiber after wearing and tearing, there is self-repair function, extended the service life of cloth.
(3) in microcapsule capsule wall material, add nano silicon, strengthened the ABRASION RESISTANCE of material.
Embodiment 1
This example provides a kind of capsule of nano material with self-regeneration and wear-resisting functions, and it prepares as follows:
(1) chitin modified: acetic acid solution is added in reactor, under nitrogen protection, add shitosan, be heated to 65 DEG C and be stirred to shitosan and dissolve completely, add ammonium persulfate, N, N '-methylene-bisacrylamide and acrylic acid, at 65 DEG C, react 4 hours, stop reaction, add ethanol, stir 30 minutes, add alkali and regulate pH to 7, filter, washing, by soaked in absolute ethyl alcohol 24 hours, take out, vacuumize, obtain white velvet-like solid, acetic acid in described acetic acid solution, shitosan, ammonium persulfate, N, N '-methylene-bisacrylamide, the mass ratio that feeds intake of acrylic acid and ethanol is followed successively by 3.5:15:1.5:0.3:1:4,
(2) introduce selfreparing group: velvet-like above-mentioned white solid, trithiocarbonate, ether, azodiisobutyronitrile are added in reactor according to the ratio of mol ratio 3:55:110:1, carry out 3 freeze-thaw-degassed circulations, then under nitrogen protection and temperature 70 C, insulation reaction 5 hours, obtain cross-linked polymer, with apparatus,Soxhlet's purify and vacuumize after, obtain faint yellow solid material;
(3) prepare microcapsule dressing agent: by gelatin, positive nonane, OP-10 emulsifying agent and nano silicon add in distilled water, after mixing, at 60 DEG C ~ 70 DEG C, dissolve, after dissolving, in high-shear emulsion machine, the rotating speed with 4000r/min carries out emulsification, obtain emulsion, wherein gelatin, positive nonane, OP-10 emulsifying agent, the mass ratio of nano silicon and distilled water is followed successively by 0.5:1:0.4:1.5:100, taking out emulsion joins in reactor, adding volume is the distilled water diluting of 1.2 times of emulsion volumes, 40 ~ 50 DEG C of temperature with under stirring, add the faint yellow solid material of step (2) gained, and regulate with the sodium hydroxide solution of 10wt% between pH to 5.5 ~ 6.5 of reactant liquor, finally add CALCIUM CHLORIDE DIHYDRATE, isothermal reaction 30 ~ 60min, obtain microcapsule dressing agent, the mass fraction that described faint yellow solid material and CALCIUM CHLORIDE DIHYDRATE account for microcapsule dressing agent is respectively 2.5% and 0.3%,
(4) form wall material: the prepared microcapsule dressing agent of step (3) is joined in impregnation container, fabric (20D, 380T, 24F Nylon Taffeta) is immersed in microcapsule dressing agent, then add glutaraldehyde cross-linking agent, under agitation crosslinking curing 70min, after add again glycerine, after stirring fully, fabric moisture is extruded, dry, enter calender, 185 DEG C of temperature, under pressure 8MP, carry out roll compacting, obtain described capsule of nano material, the quality that feeds intake of described glutaraldehyde cross-linking agent and glycerine accounts for respectively 0.55% and 2.5% of the quality that always feeds intake.
The capsule of nano material of this example preparation after testing wear-resisting number of turns is 126 circles, and after processing, mass area ratio increase ratio is 0.26%: boring suede quantity is 3 ~ 5, and air penetrability is: 1.8mm/s.
Comparative example 1
By fabric (20D, 380T, 24F Nylon Taffeta) to immerse concentration be 5% water repellent finishing agent (He Te global group produce the water repellent finishing agent of HS1100 model) solution, after infiltrating fully, take out, 150 DEG C of oven dry, calendering under 120 DEG C of 10MPa, repeat again after infiltration-oven dry-calendering technique one time, the aqueous polyurethane that is 20% by concentration (waterborne polyurethane resin that the model that the U.S. macromolecular material of Shandong Order Co., Ltd produces is ADM-F209) is coated in the one side of cloth, then in 30 DEG C of oven dry.And then apply-dry once.
The wear-resisting number of turns is 148 circles after testing, and after processing, mass area ratio increase ratio is 11.91%: boring suede quantity is: 3 ~ 6, air penetrability is: 0mm/s.
By embodiment 1 and comparative example 1 are contrasted known, although take common coating process can obtain the anti-wear performance more excellent than the present invention and the anti-chiseling down effect being equal to, but the gas permeability of fabric after treatment obviously reduces, and mass area ratio increases obviously, the comfort level of clothes dress obviously reduces.
Above, the test of the anti-chiseling down of sample is tested according to annex E " fabric anti-chiseling down test method friction test method " in GB GB/T 14272-2011 " down coat ";
Sample Air permenbility is tested according to GB GB/T 5453-1997 " mensuration of textile fabric gas permeability ";
Sample mass area ratio is tested according to GB GB/T 24218.1-2009 " textiles non-weaving cloth test method part 1: the mensuration of mass area ratio ";
Sample ABRASION RESISTANCE is tested according to GB GB/T " mensuration of textiles Martindale fabric abrasion resistance ".
Above the present invention is described in detail; its object is to allow the personage who is familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; the equivalence that all Spirit Essences according to the present invention are done changes or modifies, and all should be encompassed in protection scope of the present invention.
Claims (10)
1. a capsule of nano material, it comprises the fabric matrix of being made up of fiber, it is characterized in that: described Nano capsule material also comprises and is coated on that described fiber is outer, thickness is nano level wall material, described wall material and described fiber form taking fiber as " core ", the capsule of nano structure taking wall material as " capsule sheath ".
2. capsule of nano material according to claim 1, it is characterized in that: described fabric matrix is the Nylon Taffeta of 380 ~ 420T, 10 ~ 30D, 24/48F, the Polyester Taffeta of 380 ~ 420T, 10 ~ 30D, 24/48F, or the spring Asia of 330 ~ 400T, 20 ~ 40D, 24/48/72/96F is spun.
3. capsule of nano material according to claim 1, is characterized in that: be used to form in the filmogen of described wall material and contain ultraviolet excitation selfreparing group.
4. capsule of nano material according to claim 3, is characterized in that: described in be used to form described wall material filmogen be the polymer that obtains of modification of chitosan and trithiocarbonate generation cross-linking reaction or the mixture of this polymer and gelatin.
5. capsule of nano material according to claim 1, is characterized in that: in described wall material, contain nano silicon.
6. capsule of nano material according to claim 1, it is characterized in that: described capsule of nano material is by carrying out encapsulated arrangement and carry out subsequently satinage obtaining to fabric matrix with microcapsule dressing agent, described microcapsule dressing agent comprises filmogen, auxiliary agent, organic solvent and water, and described auxiliary agent at least comprises emulsifying agent and abrasion-resistant powder.
7. capsule of nano material according to claim 1, is characterized in that: described capsule of nano material makes as follows:
(1) chitin modified: acetic acid solution is added in reactor, under nitrogen protection, add shitosan, be heated to 60 ~ 70 DEG C and be stirred to shitosan and dissolve completely, add ammonium persulfate, N, N '-methylene-bisacrylamide and acrylic acid, at 50 ~ 70 DEG C, react 3 ~ 5 hours, stop reaction, add ethanol, stir 20 ~ 40 minutes, add alkali and regulate pH to 6.8 ~ 7.2, filter, washing, by soaked in absolute ethyl alcohol more than 12 hours, take out, vacuumize, obtain white velvet-like solid, acetic acid in described acetic acid solution, shitosan, ammonium persulfate, N, N '-methylene-bisacrylamide and acrylic acid mass ratio that feeds intake are followed successively by 2 ~ 5:10 ~ 20:1 ~ 2:0.2 ~ 0.5:1 ~ 2,
(2) introduce selfreparing group: velvet-like above-mentioned white solid, trithiocarbonate, ether, azodiisobutyronitrile are added in reactor according to the ratio of mol ratio 2 ~ 5:50 ~ 60:100 ~ 120:1 ~ 2, carry out 2 ~ 4 freeze-thaw-degassed circulations, then at 60 ~ 80 DEG C of nitrogen protection and temperature, insulation reaction 4 ~ 6 hours, obtain cross-linked polymer, after purifying vacuumize, obtain faint yellow solid material;
(3) prepare microcapsule dressing agent: by gelatin, positive nonane, OP-10 emulsifying agent and nano silicon add in distilled water, after mixing, at 60 DEG C ~ 70 DEG C, dissolve, after dissolving, in high-shear emulsion machine, carry out emulsification, obtain emulsion, wherein gelatin, positive nonane, OP-10 emulsifying agent, the mass ratio of nano silicon and distilled water is followed successively by 0.5 ~ 0.6:1 ~ 2:0.2 ~ 0.5:1 ~ 2:100, taking out emulsion joins in reactor, adding volume is the distilled water diluting of 1 ~ 1.5 times of emulsion volume, 40 ~ 50 DEG C of temperature with under stirring, add the faint yellow solid material of step (2) gained, and regulate with the sodium hydroxide solution of 10wt% ~ 15wt% between pH to 5.5 ~ 6.5 of reactant liquor, finally add CALCIUM CHLORIDE DIHYDRATE, isothermal reaction 30 ~ 60min, obtain microcapsule dressing agent, the mass fraction that described faint yellow solid material and CALCIUM CHLORIDE DIHYDRATE account for microcapsule dressing agent is respectively 2% ~ 3% and 0.2% ~ 0.5%,
(4) form wall material: the prepared microcapsule dressing agent of step (3) is joined in impregnation container, fabric is immersed in microcapsule dressing agent, then add glutaraldehyde cross-linking agent, under agitation crosslinking curing 60 ~ 90min, after add again glycerine, after stirring fully, fabric moisture is extruded, dry, enter calender, 180 ~ 190 DEG C of temperature, under pressure 8 ~ 10MP, carry out roll compacting, obtain described capsule of nano material, the quality that feeds intake of described glutaraldehyde cross-linking agent and glycerine accounts for respectively 0.5% ~ 0.6% and 2% ~ 3% of the quality that always feeds intake.
8. a preparation method for capsule of nano material, is characterized in that: comprise the following steps:
(1) chitin modified: acetic acid solution is added in reactor, under nitrogen protection, add shitosan, be heated to 60 ~ 70 DEG C and be stirred to shitosan and dissolve completely, add ammonium persulfate, N, N '-methylene-bisacrylamide and acrylic acid, at 50 ~ 70 DEG C, react 3 ~ 5 hours, stop reaction, add ethanol, stir 20 ~ 40 minutes, add alkali and regulate pH to 6.8 ~ 7.2, filter, washing, by soaked in absolute ethyl alcohol more than 12 hours, take out, vacuumize, obtain white velvet-like solid, acetic acid in described acetic acid solution, shitosan, ammonium persulfate, N, N '-methylene-bisacrylamide and acrylic acid mass ratio that feeds intake are followed successively by 2 ~ 5:10 ~ 20:1 ~ 2:0.2 ~ 0.5:1 ~ 2,
(2) introduce selfreparing group: velvet-like above-mentioned white solid, trithiocarbonate, ether, azodiisobutyronitrile are added in reactor according to the ratio of mol ratio 2 ~ 5:50 ~ 60:100 ~ 120:1 ~ 2, carry out 2 ~ 4 freeze-thaw-degassed circulations, then at 60 ~ 80 DEG C of nitrogen protection and temperature, insulation reaction 4 ~ 6 hours, obtain cross-linked polymer, after purifying vacuumize, obtain faint yellow solid material;
(3) prepare microcapsule dressing agent: by gelatin, positive nonane, OP-10 emulsifying agent and nano silicon add in distilled water, after mixing, at 60 DEG C ~ 70 DEG C, dissolve, after dissolving, in high-shear emulsion machine, carry out emulsification, obtain emulsion, wherein gelatin, positive nonane, OP-10 emulsifying agent, the mass ratio of nano silicon and distilled water is followed successively by 0.5 ~ 0.6:1 ~ 2:0.2 ~ 0.5:1 ~ 2:100, taking out emulsion joins in reactor, adding volume is the distilled water diluting of 1 ~ 1.5 times of emulsion volume, 40 ~ 50 DEG C of temperature with under stirring, add the faint yellow solid material of step (2) gained, and regulate with the sodium hydroxide solution of 10wt% ~ 15wt% between pH to 5.5 ~ 6.5 of reactant liquor, finally add CALCIUM CHLORIDE DIHYDRATE, isothermal reaction 30 ~ 60min, obtain microcapsule dressing agent, the mass fraction that described faint yellow solid material and CALCIUM CHLORIDE DIHYDRATE account for microcapsule dressing agent is respectively 2% ~ 3% and 0.2% ~ 0.5%,
(4) form wall material: the prepared microcapsule dressing agent of step (3) is joined in impregnation container, fabric is immersed in microcapsule dressing agent, then add glutaraldehyde cross-linking agent, under agitation crosslinking curing 60 ~ 90min, after add again glycerine, after stirring fully, fabric moisture is extruded, dry, enter calender, 180 ~ 190 DEG C of temperature, under pressure 8 ~ 10MP, carry out roll compacting, obtain described capsule of nano material, the quality that feeds intake of described glutaraldehyde cross-linking agent and glycerine accounts for respectively 0.5% ~ 0.6% and 2% ~ 3% of the quality that always feeds intake.
9. the preparation method of capsule of nano material according to claim 8, is characterized in that: described fiber is superfine fibre, and the dawn, number was between 10 ~ 40D.
10. ultra-thin down jackets, is characterized in that: the capsule of nano material in employing claim 1 to 7 described in any one claim is as fabric.
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| CN107384326A (en) * | 2017-07-25 | 2017-11-24 | 延安大学 | Gelatin chitosan nano silicon multinuclear microcapsules of storing energy through phase change preparation method |
| CN109297937A (en) * | 2018-11-13 | 2019-02-01 | 东华大学 | A kind of anti-chiseling down characteristic test evaluation method based on fabric light transmission image |
| CN110368879A (en) * | 2019-07-18 | 2019-10-25 | 太原理工大学 | A kind of self-repairing microcapsule and preparation method thereof, selfreparing basalt fibre and preparation method thereof |
| CN110835404A (en) * | 2019-12-02 | 2020-02-25 | 肇庆市海特复合材料技术研究院 | Preparation method of microcapsule rapid curing agent for epoxy resin |
| CN115142259A (en) * | 2022-07-05 | 2022-10-04 | 杭州鑫马纺织有限公司 | High-density full-silk anti-velvet jacquard fabric |
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