CN110067134A - The preparation method of intelligent thermoregulating microcapsules cyst membrane and its application in textile - Google Patents
The preparation method of intelligent thermoregulating microcapsules cyst membrane and its application in textile Download PDFInfo
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- CN110067134A CN110067134A CN201910435376.8A CN201910435376A CN110067134A CN 110067134 A CN110067134 A CN 110067134A CN 201910435376 A CN201910435376 A CN 201910435376A CN 110067134 A CN110067134 A CN 110067134A
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- cyst membrane
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
- C08J2375/14—Polyurethanes having carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/18—Homopolymers or copolymers of nitriles
- C08J2433/20—Homopolymers or copolymers of acrylonitrile
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
Abstract
The present invention provides the preparation methods of intelligent thermoregulating microcapsules cyst membrane, comprising the following steps: the rabbit hair for taking the wool shredded and shredding is dispersed in constant temperature stirring in carbon amide solution, stands；Phosphoamide crystal is precipitated in filtering, filtrate room temperature, and liquid pours into bag filter mixed protein colloid of dialysing to obtain；Isocyanate prepolymer and paraffin are mixed, microcapsule phase-change liquid is obtained；By sodium sulfocyanate and deionized water mixed dissolution, mixed protein colloid, Soybean Protein Modification eyeball synthetic fibre polymer is added, stirring and dissolving obtains mixed protein modified acrylic fibers spinning solution；It is slowly added to microcapsule phase-change liquid, is uniformly mixed, is stood after continuing stirring；It after knifing, impregnates into the water, natural air drying after taking-up；It is put into boiling water and impregnates, take out and air-dry to obtain the final product.Intelligent thermoregulating microcapsules cyst membrane obtained by this law has good temperature adjusting performance, and transformation temperature is at 30 DEG C or so, and heat enthalpy value is up to 17.4J/g.
Description
Technical field
The present invention relates to the preparation method of intelligent thermoregulating microcapsules cyst membrane and its applications in textile.
Background technique
With the fast development and continuous improvement of people's living standards of social and economic level, requirement of the people to clothes
Constantly changing, is increasingly focusing on aesthetic appearance, conformal performance, hot wet migration energy and the thermal property etc. of fabric.Knitted side
Material has the characteristics such as soft, moisture absorption is ventilative, elasticity and ductility are excellent, and the clothes softness made of it is personal, dress is relaxed
Certain warmth retention property is fitted and had, will be widely welcomed by consumer.One of knitted fabric biggest advantage is exactly the warming of it
Property, especially in winter, human body can be protected well.And simultaneously, with the improvement of living standards, people no longer only meet
In heat-preservation clothing material, also require fabric that can be adjusted according to body temperature, therefore, exploitation has temperature adjustment function material, is applied to face
In material, it can be changed, be had great importance according to body temperature, it may have vast potential for future development.
Summary of the invention
Technical problems to be solved:
A kind of preparation method of intelligent thermoregulating microcapsules cyst membrane is provided, gained intelligent thermoregulating microcapsules cyst membrane has good
Temperature adjusting performance, transformation temperature is at 30 DEG C or so, and heat enthalpy value is up to 17.4J/g.
Technical solution:
The present invention provides the preparation methods of intelligent thermoregulating microcapsules cyst membrane, and ingredient is by weight, comprising the following steps:
(1) 20-30 parts of carbamides and 10-15 parts of distilled water are mixed, heating stirring dissolution；
(2) the 2-3 parts of wools shredded and the 1-2 parts of rabbit hairs shredded are taken to be dispersed in carbon amide solution, in 120 DEG C of perseverances
Temperature is lower to stir 20-30min, and 10-15 parts of distilled water are added after standing 60min, continue constant temperature 30min；(3) it filters, filtrate room temperature
12h to be placed, phosphoamide crystal is precipitated, is recycled, liquid pours into bag filter, and bag filter is put into deionized water and is impregnated,
Every 3h changes a deionized water, takes out after 48h, flows out to obtain mixed protein colloid to water；
(4) isocyanates and end hydroxy butadiene hybrid reaction are obtained into isocyanate prepolymer in draught cupboard；
(5) 5-10 parts of isocyanate prepolymers and 10-20 parts of paraffin are mixed, in 60 DEG C of waters bath with thermostatic control, revolving speed 1000-
100-150min is stirred under 1200rpm, obtains microcapsule phase-change liquid；
(6) 30-40 parts of sodium sulfocyanates and 40-45 parts of deionized waters are mixed, be placed in 60 DEG C of water bath with thermostatic control stir it is molten
Solution, be added 1.5-2 part mixed protein colloids, 4-5 parts of Soybean Protein Modification eyeball synthetic fibre polymer, stir to dissolve mixed protein changes
Property acrylic spinning liquid；
(7) 1.8-2.5 parts of microcapsule phase-change liquid are slowly added to, are uniformly mixed, static placement 12h after stirring 30min is continued；
(8) after knifing, 40-60min, natural air drying after taking-up are impregnated into the water；
(9) it is put into boiling water and impregnates 10-15min, take out and air-dry up to intelligent thermoregulating microcapsules cyst membrane.
Further, the wool and the rabbit hair are cut into 1-2mm.
Further, the Soybean Protein Modification eyeball synthetic fibre polymer the preparation method comprises the following steps:
Step 1: it is 70 DEG C that 10 parts of eyeball synthetic fibres, which are added to temperature, and in the NaOH solution that 100 parts of mass fractions are 10%, water
Solution is taken out and cleans drying；
It is accounted in the thionyl chloride closed gas atmosphere that fiber quality score is 10% step 2: being added to, it is anti-at 110 DEG C
Answer 30min；
Step 3: being put into content after taking out is to react 5min under temperature 70 C in 6% soybean protein aqueous solution to obtain the final product.
Further, the mass ratio of isocyanates and end hydroxy butadiene is 0.175 in the step (4).
Intelligent thermoregulating microcapsules cyst membrane answering in textile prepared by the preparation method of intelligent thermoregulating microcapsules cyst membrane
With
Application of the preparation method of intelligent thermoregulating microcapsules cyst membrane in textile.
The utility model has the advantages that
Microcapsules and egg mix white glue compatibility prepared by 1. are good, and thermoregulation effect is good.
2. there is good skin-friendly and water penetration using Soybean Protein Modification eyeball synthetic fibre polymer, very comfortably.
After 3. first film is air-dried, the shell of microcapsules aggregated completion, then when being impregnated through boiling water, extra isocyanates with
Water reaction, the further shell material for reinforcing microcapsules, paraffin are wrapped attached more complete, and heat enthalpy value is more significantly.
4. the intelligent thermoregulating microcapsules cyst membrane through the method for the present invention preparation has good temperature adjusting performance, transformation temperature is 30
DEG C or so, heat enthalpy value is up to 17.4J/g.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit this in any way
Invention.
Embodiment 1
The preparation method of intelligent thermoregulating microcapsules cyst membrane, ingredient is by weight, comprising the following steps:
(1) 20 parts of carbamides and 10 parts of distilled water are mixed, heating stirring dissolution；
(2) 2 parts of wools shredded and 1 part of rabbit hair shredded are taken to be dispersed in carbon amide solution, under 120 DEG C of constant temperature
20min is stirred, 10 parts of distilled water are added after standing 60min, continue constant temperature 30min；
(3) it filters, filtrate room temperature 12h, phosphoamide crystal is precipitated, is recycled, liquid pours into bag filter, will be saturating
Analysis bag, which is put into deionized water, to be impregnated, and every 3h changes a deionized water, takes out after 48h, flows out to obtain mixed protein colloid to water；
(4) isocyanates and end hydroxy butadiene hybrid reaction are obtained into isocyanate prepolymer in draught cupboard；
(5) 5 parts of isocyanate prepolymers and 10 parts of paraffin are mixed, is stirred at 60 DEG C of waters bath with thermostatic control, revolving speed 1000rpm
100min obtains microcapsule phase-change liquid；
(6) 30 parts of sodium sulfocyanates and 40 parts of deionized waters are mixed, is placed in stirring and dissolving in 60 DEG C of water bath with thermostatic control, be added
1.5 parts of mixed protein colloids, 4 parts of Soybean Protein Modification eyeball synthetic fibre polymer, stirring is to dissolving to obtain mixed protein modified acrylic fibers spinning
Liquid；
(7) 1.8 parts of microcapsule phase-change liquid are slowly added to, are uniformly mixed, static placement 12h after stirring 30min is continued；
(8) after knifing, 40min, natural air drying after taking-up are impregnated into the water；
(9) it is put into boiling water and impregnates 10min, take out and air-dry up to intelligent thermoregulating microcapsules cyst membrane.
Embodiment 2
The preparation method of intelligent thermoregulating microcapsules cyst membrane, ingredient is by weight, comprising the following steps:
(1) 22 parts of carbamides and 11 parts of distilled water are mixed, heating stirring dissolution；
(2) 2.5 parts of wools shredded and 1.2 parts of rabbit hairs shredded are taken to be dispersed in carbon amide solution, in 120 DEG C of perseverances
Temperature is lower to stir 22min, and 11 parts of distilled water are added after standing 60min, continue constant temperature 30min；
(3) it filters, filtrate room temperature 12h, phosphoamide crystal is precipitated, is recycled, liquid pours into bag filter, will be saturating
Analysis bag, which is put into deionized water, to be impregnated, and every 3h changes a deionized water, takes out after 48h, flows out to obtain mixed protein colloid to water；
(4) isocyanates and end hydroxy butadiene hybrid reaction are obtained into isocyanate prepolymer in draught cupboard；
(5) 6 parts of isocyanate prepolymers and 12 parts of paraffin are mixed, is stirred at 60 DEG C of waters bath with thermostatic control, revolving speed 1050rpm
110min obtains microcapsule phase-change liquid；
(6) 32 parts of sodium sulfocyanates and 41 parts of deionized waters are mixed, is placed in stirring and dissolving in 60 DEG C of water bath with thermostatic control, be added
1.6 parts of mixed protein colloids, 4.2 parts of Soybean Protein Modification eyeball synthetic fibre polymer stir to dissolving to obtain the spinning of mixed protein modified acrylic fibers
Silk liquid；
(7) 1.9 parts of microcapsule phase-change liquid are slowly added to, are uniformly mixed, static placement 12h after stirring 30min is continued；
(8) after knifing, 45min, natural air drying after taking-up are impregnated into the water；
(9) it is put into boiling water and impregnates 12min, take out and air-dry up to intelligent thermoregulating microcapsules cyst membrane.
Embodiment 3
The preparation method of intelligent thermoregulating microcapsules cyst membrane, ingredient is by weight, comprising the following steps:
(1) 25 parts of carbamides and 13 parts of distilled water are mixed, heating stirring dissolution；
(2) 2.5 parts of wools shredded and 1.5 parts of rabbit hairs shredded are taken to be dispersed in carbon amide solution, in 120 DEG C of perseverances
Temperature is lower to stir 25min, and 13 parts of distilled water are added after standing 60min, continue constant temperature 30min；
(3) it filters, filtrate room temperature 12h, phosphoamide crystal is precipitated, is recycled, liquid pours into bag filter, will be saturating
Analysis bag, which is put into deionized water, to be impregnated, and every 3h changes a deionized water, takes out after 48h, flows out to obtain mixed protein colloid to water；
(4) isocyanates and end hydroxy butadiene hybrid reaction are obtained into isocyanate prepolymer in draught cupboard；
(5) 8 parts of isocyanate prepolymers and 15 parts of paraffin are mixed, is stirred at 60 DEG C of waters bath with thermostatic control, revolving speed 1100rpm
130min obtains microcapsule phase-change liquid；
(6) 35 parts of sodium sulfocyanates and 43 parts of deionized waters are mixed, is placed in stirring and dissolving in 60 DEG C of water bath with thermostatic control, be added
1.7 parts of mixed protein colloids, 4.5 parts of Soybean Protein Modification eyeball synthetic fibre polymer stir to dissolving to obtain the spinning of mixed protein modified acrylic fibers
Silk liquid；
(7) 2 parts of microcapsule phase-change liquid are slowly added to, are uniformly mixed, static placement 12h after stirring 30min is continued；(8) it scrapes
After film, 50min, natural air drying after taking-up are impregnated into the water；
(9) it is put into boiling water and impregnates 13min, take out and air-dry up to intelligent thermoregulating microcapsules cyst membrane.
Embodiment 4
The preparation method of intelligent thermoregulating microcapsules cyst membrane, ingredient is by weight, comprising the following steps:
(1) 28 parts of carbamides and 14 parts of distilled water are mixed, heating stirring dissolution；
(2) 2.8 parts of wools shredded and 1.8 parts of rabbit hairs shredded are taken to be dispersed in carbon amide solution, in 120 DEG C of perseverances
Temperature is lower to stir 25min, and 14 parts of distilled water are added after standing 60min, continue constant temperature 30min；
(3) it filters, filtrate room temperature 12h, phosphoamide crystal is precipitated, is recycled, liquid pours into bag filter, will be saturating
Analysis bag, which is put into deionized water, to be impregnated, and every 3h changes a deionized water, takes out after 48h, flows out to obtain mixed protein colloid to water；
(4) isocyanates and end hydroxy butadiene hybrid reaction are obtained into isocyanate prepolymer in draught cupboard；
(5) 9 parts of isocyanate prepolymers and 18 parts of paraffin are mixed, is stirred at 60 DEG C of waters bath with thermostatic control, revolving speed 1050rpm
140min obtains microcapsule phase-change liquid；
(6) 38 parts of sodium sulfocyanates and 44 parts of deionized waters are mixed, is placed in stirring and dissolving in 60 DEG C of water bath with thermostatic control, be added
1.8 parts of mixed protein colloids, 4.7 parts of Soybean Protein Modification eyeball synthetic fibre polymer stir to dissolving to obtain the spinning of mixed protein modified acrylic fibers
Silk liquid；
(7) 2.2 parts of microcapsule phase-change liquid are slowly added to, are uniformly mixed, static placement 12h after stirring 30min is continued；
(8) after knifing, 55min, natural air drying after taking-up are impregnated into the water；
(9) it is put into boiling water and impregnates 14min, take out and air-dry up to intelligent thermoregulating microcapsules cyst membrane.
Embodiment 5
The preparation method of intelligent thermoregulating microcapsules cyst membrane, ingredient is by weight, comprising the following steps:
(1) 30 parts of carbamides and 15 parts of distilled water are mixed, heating stirring dissolution；
(2) 3 parts of wools shredded and 2 parts of rabbit hairs shredded are taken to be dispersed in carbon amide solution, under 120 DEG C of constant temperature
30min is stirred, 15 parts of distilled water are added after standing 60min, continue constant temperature 30min；
(3) it filters, filtrate room temperature 12h, phosphoamide crystal is precipitated, is recycled, liquid pours into bag filter, will be saturating
Analysis bag, which is put into deionized water, to be impregnated, and every 3h changes a deionized water, takes out after 48h, flows out to obtain mixed protein colloid to water；
(4) isocyanates and end hydroxy butadiene hybrid reaction are obtained into isocyanate prepolymer in draught cupboard；
(5) 10 parts of isocyanate prepolymers and 20 parts of paraffin are mixed, is stirred at 60 DEG C of waters bath with thermostatic control, revolving speed 1200rpm
150min is mixed, microcapsule phase-change liquid is obtained；
(6) 40 parts of sodium sulfocyanates and 45 parts of deionized waters are mixed, is placed in stirring and dissolving in 60 DEG C of water bath with thermostatic control, be added
2 parts of mixed protein colloids, 5 parts of Soybean Protein Modification eyeball synthetic fibre polymer, stirring is to dissolving to obtain mixed protein modified acrylic fibers spinning solution；
(7) 2.5 parts of microcapsule phase-change liquid are slowly added to, are uniformly mixed, static placement 12h after stirring 30min is continued；
(8) after knifing, 60min, natural air drying after taking-up are impregnated into the water；
(9) it is put into boiling water and impregnates 15min, take out and air-dry up to intelligent thermoregulating microcapsules cyst membrane.
Heat stability testing is carried out using DSC-6200 type differential scanning calorimeter.
The partial properties index of 1 intelligent thermoregulating microcapsules cyst membrane of table
| Name of product | Transformation temperature (DEG C) | Heat enthalpy value (J/g) |
| Embodiment 1 | 30.03 | 16.9 |
| Embodiment 2 | 30.09 | 17.1 |
| Embodiment 3 | 30.11 | 17.2 |
| Embodiment 4 | 30.16 | 17.4 |
| Embodiment 5 | 30.10 | 17.3 |
Intelligent thermoregulating microcapsules cyst membrane through the method for the present invention preparation has good temperature adjusting performance, and transformation temperature is at 30 DEG C
Left and right, heat enthalpy value is up to 17.4J/g.
Claims (5)
1. the preparation method of intelligent thermoregulating microcapsules cyst membrane, it is characterised in that: ingredient is by weight, comprising the following steps:
(1) 20-30 parts of carbamides and 10-15 parts of distilled water are mixed, heating stirring dissolution；
(2) the 2-3 parts of wools shredded and the 1-2 parts of rabbit hairs shredded are taken to be dispersed in carbon amide solution, under 120 DEG C of constant temperature
20-30min is stirred, 10-15 parts of distilled water are added after standing 60min, continue constant temperature 30min；
(3) it filters, filtrate room temperature 12h, phosphoamide crystal is precipitated, is recycled, liquid pours into bag filter, by bag filter
It is put into deionized water and impregnates, every 3h changes a deionized water, takes out after 48h, flows out to obtain mixed protein colloid to water；
(4) isocyanates and end hydroxy butadiene hybrid reaction are obtained into isocyanate prepolymer in draught cupboard；
(5) 5-10 parts of isocyanate prepolymers and 10-20 parts of paraffin are mixed, in 60 DEG C of waters bath with thermostatic control, revolving speed 1000-
100-150min is stirred under 1200rpm, obtains microcapsule phase-change liquid；
(6) 30-40 parts of sodium sulfocyanates and 40-45 parts of deionized waters are mixed, is placed in stirring and dissolving in 60 DEG C of water bath with thermostatic control, adds
Enter 1.5-2 parts of mixed protein colloids, 4-5 parts of Soybean Protein Modification eyeball synthetic fibre polymer, stirs to dissolving to obtain the modified nitrile of mixed protein
Synthetic fibre spinning solution；
(7) 1.8-2.5 parts of microcapsule phase-change liquid are slowly added to, are uniformly mixed, static placement 12h after stirring 30min is continued；
(8) after knifing, 40-60min, natural air drying after taking-up are impregnated into the water；
(9) it is put into boiling water and impregnates 10-15min, take out and air-dry up to intelligent thermoregulating microcapsules cyst membrane.
2. the preparation method of intelligent thermoregulating microcapsules cyst membrane according to claim 1, it is characterised in that: the wool and rabbit
Hair is cut into 1-2mm.
3. the preparation method of intelligent thermoregulating microcapsules cyst membrane according to claim 1, it is characterised in that: the soybean protein
Modified eyeball synthetic fibre polymer the preparation method comprises the following steps:
Step 1: it is 70 DEG C that 10 parts of eyeball synthetic fibres, which are added to temperature, in the NaOH solution that 100 parts of mass fractions are 10%, hydrolysis is taken
Drying is cleaned out；
It accounts in the thionyl chloride closed gas atmosphere that fiber quality score is 10% step 2: being added to, is reacted at 110 DEG C
30min；
Step 3: being put into content after taking out is to react 5min under temperature 70 C in 6% soybean protein aqueous solution to obtain the final product.
4. the preparation method of intelligent thermoregulating microcapsules cyst membrane according to claim 1, it is characterised in that: the step (4)
The mass ratio of middle isocyanates and end hydroxy butadiene is 0.175.
5. intelligent thermoregulating microcapsules prepared by the preparation method of intelligent thermoregulating microcapsules cyst membrane described in -4 according to claim 1
Application of the cyst membrane in textile.
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