CN105381766A - Preparation method and applications of isatis root extract, vitamin and protein composite microcapsule - Google Patents
Preparation method and applications of isatis root extract, vitamin and protein composite microcapsule Download PDFInfo
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- CN105381766A CN105381766A CN201510903008.3A CN201510903008A CN105381766A CN 105381766 A CN105381766 A CN 105381766A CN 201510903008 A CN201510903008 A CN 201510903008A CN 105381766 A CN105381766 A CN 105381766A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
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Abstract
The invention belongs to the technical field of functional cellulose fiber, and relates to an isatis root extract, vitamin and protein composite microcapsule, which is used to prepare isatis root cellulose fiber. The preparation method comprises the following steps: adding isatis root extract and vitamins into a water solution of emulsifier, carrying out shearing emulsification to obtain a mixed emulsified solution; adding the mixed emulsified solution into a gelatin solution, then adding an Arabic gum solution, evenly mixing to form stable oil-in-water emulsion; adjusting the pH value, heating and stirring to carry out complex coacervation to obtain suspension liquid; cooling the suspension liquid, adding a curing agent, adjusting the pH value to carry out crosslinking reactions, after reactions, filtering to obtain isatis root extract, vitamin and protein composite microcapsules; adding the composite microcapsules into viscose stock solution to prepare a blended spinning liquid, and carrying out spinning through an adjusted coagulation bath. Through the micro-encapsulation, crosslinking and solidification, the loss of effective component during the processes of spinning and post treatment is reduced, and the prepared viscose has the antivirus and skincare functions.
Description
Technical field
The invention belongs to functional cellulose fibre technology field, specifically, relate to one with isatis root extract-vitamin for core, gelatin is the isatis root extract vitamin protein composite micro-capsule of wall material, and for the preparation of having the preparation method of Radix Isatidis cellulose fibre of antiviral, functions of skin protection and health care.
Background technology
Healthy is one of society topic of greatest concern with environmental protection.In recent years, textile industry be proposed successively many be conducive to health and environmental protection there is health care, the fiber of medical functions and textile thereof.Through development for many years, health care fibre and textile thereof, technological development or product development all achieve gratifying results, and wherein handlebar vitamin directly incorporates women's shirt; There is the T-shirt etc. containing treatment rheumatism drug microparticles.These have fashion concurrently and piece market that is healthy, health keeping and medical function has a high potential, and reach multi-billion dollar, and become the target of people's pursuit.
Chinese patent ZL201010592931.7 discloses a kind of preparation method with drug fiber in the pearl of functions of skin protection and health care, described fiber is made up of cellulose fibre 90 ~ 95%, pearl 2 ~ 5% and Chinese medicine 2 ~ 5%, and Chinese medicine is the combination of any one or more in pseudo-ginseng, Radix Angelicae Sinensis, the red sage root; This fiber in preparation process, be pearl powder, traditional Chinese medicinal components are mixed with slurry after directly join in spinning slurry, through mixing, filter, spray silk, drawing-off, sizing make drug fiber in pearl; Due in production process of viscose fiber, use the industrial chemicals such as NaOH, carbon disulfide and sulfuric acid, therefore in this fiber production process, pearl powder, Chinese drug-treated group branch are damaged, and have a strong impact on the functional of fiber.
Radix Isatidis is a kind of excellent Chinese medicine, has antibacterial, antiviral, antitumor, to improve immunologic function effect.Chinese patent ZL201310140966.0 discloses a kind of viscose rayon with plant-source antibacterial function and peppermint aromatic odor, during spinning, antimicrobial and peppermint oil microcapsules are joined in viscose the standing vacuum that stirs to arrange and steep, obtain rayon spinning liquid; Gained rayon spinning liquid is introduced spinning moulding in coagulating bath, and strand obtains long filament through draft process; Used isatis root extract in this patent, but isatis root extract does not directly add in viscose glue stoste through overprotection modification, Radix Isatidis be damaged in spinning process and run off serious, have impact on the functional of fiber.
In view of Radix Isatidis has good functional, vitamin is for treatment scurvy simultaneously, prevention gingival atrophy, hemorrhage, and treatment anaemia, anti-cancer, Cell protection, removing toxic substances, protection liver, the immunity etc. improving human body has good action.Collagen is a kind of biological polymer substance, a kind of white, opaque, unbranched fibroid protein, it can supplement the nutrition needed for skin layers, Collage Activitv in skin is strengthened, there is skin care, delay senility, improve looks, wrinkle-chasing, the effect such as hair care, and the class protein that gelatin is collagenous portion hydrolysis and obtains, has homology with collagen.Therefore, with Radix Isatidis and vitamin prescription as antiviral, health treatment, using its composition as core, using gelatin as wall material, and wall material is carried out crosslinking curing, prepare and there are microcapsules that are antiviral, skin-protection and health-care, thus develop there is textile that is antiviral, functions of skin protection and health care, the healthy tool of China's textile industry and people is of great significance.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art existence, seek the preparation method designing a kind of isatis root extract vitamin protein composite micro-capsule, active princlple-isatis root extract, vitamin and gelatin protein in the fiber number of dropouts in spinning process and last handling process is reduced, be applied to the preparation of Radix Isatidis cellulose fibre, make prepared functional viscose fiber have good antiviral and functions of skin protection and health care.
A kind of preparation method of isatis root extract vitamin protein composite micro-capsule
Step 1: preparation has the mixing and emulsifying solution of isatis root extract and vitamin
Emulsifying agent is joined in distilled water, be stirred well under room temperature and dissolve completely, form emulsifier solution; Isatis root extract and vitamin are joined in emulsifier solution, high speed shear emulsion dispersion 10 ~ 40min under 1000r/min ~ 2000r/min rotating speed, obtain the mixing and emulsifying solution containing isatis root extract and vitamin; Wherein the quality of emulsifying agent is 1.0% ~ 3.0% of isatis root extract and vitamin gross weight, and in mixing and emulsifying solution, the gross mass mark of isatis root extract and vitamin is 15% ~ 40%;
Preferably, described emulsifying agent is one or more in lauryl sodium sulfate (SDS), OP-10, Tween 80 or class 80 of department;
Preferably, the mass ratio of described isatis root extract and vitamin is 1 ~ 5:1;
Step 2: prepare isatis root extract vitamin protein composite micro-capsule
Preparation mass fraction is the gelatin solution of 5.0% ~ 8.0%, and mixing and emulsifying solution step 1 gained being contained isatis root extract and vitamin joins in gelatin solution, and the gross mass of isatis root extract and vitamin and the mass ratio of gelatin are 1:1 ~ 3; Adding mass fraction after stirring is 6.0% ~ 10.0% gumwater, continues stirring and gelatin solution is fully mixed with gumwater, form stable O/w emulsion; Adjust ph is 3.0 ~ 6.5, and heating water bath stirs and carries out complex coacervation, obtains suspension;
Suspension is cooled to 1 ~ 10 DEG C, add curing agent and regulate pH to be 7.5 ~ 9.5, carry out cross-linking reaction 20 ~ 50min, reduce mixing speed, filter after continuing reaction 1.0 ~ 2.0h, namely obtain with isatis root extract-vitamin for core, gelatin is the isatis root extract vitamin protein composite micro-capsule of wall material;
Preferably, in described gumwater, in the content of Arabic gum and gelatin solution, the mass ratio of gelatin is 1:1 ~ 2;
Preferably, described water bath heating temperature is 35 ~ 55 DEG C;
Preferably, described curing agent is the one in TGase, peroxidase, carbodiimide or glutaraldehyde;
Preferably, described with isatis root extract-vitamin for core, gelatin is the Particle size requirements of the microcapsules of wall material is D97≤2.5 μm;
A preparation method for Radix Isatidis cellulose fibre, comprises 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, the content of alpha cellulose is 7.2% ~ 9.5%; Front injection device is spun in utilization, isatis root extract vitamin protein composite micro-capsule is joined in viscose glue stoste, the gross mass of isatis root extract, vitamin and gelatin is 8.0% ~ 20.0% of alpha cellulose quality, prepares co-blended spinning liquid after mixing through common process;
Step b: spinning and post processing
Co-blended spinning liquid is carried out spinning by the coagulating bath adjusted, and nascent tow obtains shaping tow after drawing-off; Shaping tow is concise through cut-out, mitigation sulfur removal technology, finish application bath and washing, after oven dry, obtains having Radix Isatidis cellulose fibre that is antiviral, functions of skin protection and health care;
Preferably, in described coagulating bath, the concentration of sulfuric acid is 80 ~ 120g/L, the concentration of aluminum sulfate is 2.0 ~ 5.0g/L, sulfuric acid zinc concentration is 5.0 ~ 10.0g/L, the concentration of sodium sulphate is 280 ~ 320g/L;
Preferably, described desulfurization bath: Na
2sO
32.0 ~ 8.0g/L, oil bath: 2.0 ~ 6.0g/L, does not bleach, bake out temperature: 100 ~ 120 DEG C, and drying time is 30 ~ 50min.
A kind of have Radix Isatidis cellulose fibre that is antiviral, functions of skin protection and health care, having prepared by above-mentioned preparation method is antiviral, the Radix Isatidis cellulose fibre of functions of skin protection and health care contains the isatis root extract of 2.0 ~ 10.0wt%, the vitamin of 0.5 ~ 5.0wt% and the protein gelatin of 2.0 ~ 10.0wt%.
Isatis root extract obtains by buying.
The beneficial effect of the invention is: use Radix Isatidis and vitamin prescription as antiviral, health treatment, using its composition as core, using gelatin as wall material, and is solidified by wall material crosslinking, prepares and have microcapsules that are antiviral, skin-protection and health-care, by the crosslinking curing of microencapsulation and wall material gelatin, make the active princlple-isatis root extract in fiber, vitamin and the gelatin protein number of dropouts in spinning process and last handling process reduces, the functional viscose fiber prepared has good antiviral and functions of skin protection and health care, compared with conventional viscose rayon, it is to inactivation ratio >=84.0% of influenza A virus, to inactivation ratio >=82.0% of herpesviral, containing a large amount of vitamin and protein in fiber, containing several amino acids trace element, there is good functions of skin protection and health care, product physical index can reach Grade A requirement, fibre wearability is excellent, textile process performance is good.
Detailed description of the invention
Below by specific embodiment, the invention will be further described:
Embodiment 1
The preparation of the isatis root extract vitamin protein composite micro-capsule of the present embodiment
Step 1: preparation has the mixing and emulsifying solution of isatis root extract and vitamin
Emulsifier sodium lauryl sulfate (SDS) is joined in distilled water, is stirred well under room temperature and dissolves completely, form emulsifier solution; Join in emulsifier solution by isatis root extract and vitamin, the mass ratio of isatis root extract and vitamin is 1:1, and high speed shear emulsion dispersion 40min under 1000r/min rotating speed obtains the mixing and emulsifying solution containing isatis root extract and vitamin; Wherein the quality of emulsifying agent is 1.0% of isatis root extract and vitamin gross weight, and in mixing and emulsifying solution, the gross mass mark of isatis root extract and vitamin is 15%;
Step 2: prepare isatis root extract vitamin protein composite micro-capsule
Preparation mass fraction is the gelatin solution of 5.0%, and mixing and emulsifying solution step 1 gained being contained isatis root extract and vitamin joins in gelatin solution, and the gross mass of isatis root extract and vitamin and the mass ratio of gelatin are 1:1; The gumwater that mass fraction is 6.0% is added after stirring, in gumwater, in the content of Arabic gum and gelatin solution, the mass ratio of gelatin is 1:1, continuing stirring makes gelatin solution fully mix with gumwater, forms stable O/w emulsion; Adjust ph is 3.0, heating water bath 35 DEG C, stirs and carries out complex coacervation, obtain suspension;
Suspension is cooled to 1 DEG C, add curing agent TGase and regulate pH to be 7.5, carry out cross-linking reaction 50min, reduce mixing speed, filter after continuing reaction 1.0h, namely obtain with isatis root extract-vitamin for core, gelatin is the isatis root extract vitamin protein composite micro-capsule of wall material, its particle diameter D97≤2.498 μm;
The preparation method of the Radix Isatidis cellulose fibre of the present embodiment, comprises 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, the content of alpha cellulose is 7.2%; Front injection device is spun in utilization, isatis root extract vitamin protein composite micro-capsule is joined in viscose glue stoste, the gross mass of isatis root extract, vitamin and gelatin is 17.8% of alpha cellulose quality, prepares co-blended spinning liquid after mixing through common process;
Step b: spinning and post processing
Co-blended spinning liquid is carried out spinning by the coagulating bath adjusted, and nascent tow obtains shaping tow after drawing-off; Shaping tow is concise through cut-out, mitigation sulfur removal technology, finish application bath and washing, after oven dry, obtains having Radix Isatidis cellulose fibre that is antiviral, functions of skin protection and health care;
In coagulating bath, the concentration of sulfuric acid is 80g/L, the concentration of aluminum sulfate is 2.0g/L, sulfuric acid zinc concentration is 10.0g/L, the concentration of sodium sulphate is 280g/L; Desulfurization is bathed: Na
2sO
38.0g/L, oil bath: 6.0g/L, does not bleach, bake out temperature: 100 DEG C, and drying time is 50min.
Prepared by the present embodiment having is antiviral, the specification of the Radix Isatidis cellulose fibre of functions of skin protection and health care is 1.33dtex*38mm, through antiviral test and ingredient analysis, compared with conventional viscose rayon, it is 88.2% to the inactivation ratio of influenza A virus, to the inactivation ratio 87.3% of herpesviral, containing the vitamin of 4.45% and the gelatin protein of 8.9% in fiber, containing several amino acids trace element, product physical index can reach the requirement of GB/T14463-2008 " viscose staple fibre " Grade A.
Embodiment 2
The preparation of the isatis root extract vitamin protein composite micro-capsule of the present embodiment
Step 1: preparation has the mixing and emulsifying solution of isatis root extract and vitamin
Emulsifier op-10 is joined in distilled water, be stirred well under room temperature and dissolve completely, form emulsifier solution; Join in emulsifier solution by isatis root extract and vitamin, the mass ratio of isatis root extract and vitamin is 2:1, and high speed shear emulsion dispersion 32min under 1250r/min rotating speed obtains the mixing and emulsifying solution containing isatis root extract and vitamin; Wherein the quality of emulsifying agent is 1.4% of isatis root extract and vitamin gross weight, and in mixing and emulsifying solution, the gross mass mark of isatis root extract and vitamin is 22%;
Step 2: prepare isatis root extract vitamin protein composite micro-capsule
Preparation mass fraction is the gelatin solution of 5.6%, and mixing and emulsifying solution step 1 gained being contained isatis root extract and vitamin joins in gelatin solution, and the gross mass of isatis root extract and vitamin and the mass ratio of gelatin are 1:2; The gumwater that mass fraction is 7.5% is added after stirring, in gumwater, in the content of Arabic gum and gelatin solution, the mass ratio of gelatin is 1:1.2, continuing stirring makes gelatin solution fully mix with gumwater, forms stable O/w emulsion; Adjust ph is 3.6, heating water bath 39 DEG C, stirs and carries out complex coacervation, obtain suspension;
Suspension is cooled to 3 DEG C, add curing agent TGase and regulate pH to be 8.1, carry out cross-linking reaction 42min, reduce mixing speed, filter after continuing reaction 1.2h, namely obtain with isatis root extract-vitamin for core, gelatin is the isatis root extract vitamin protein composite micro-capsule of wall material, its particle diameter D97≤2.359 μm;
The preparation method of the Radix Isatidis cellulose fibre of the present embodiment, comprises 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, the content of alpha cellulose is 7.7%; Front injection device is spun in utilization, isatis root extract vitamin protein composite micro-capsule is joined in viscose glue stoste, the gross mass of isatis root extract, vitamin and gelatin is 13.2% of alpha cellulose quality, prepares co-blended spinning liquid after mixing through common process;
Step b: spinning and post processing
Co-blended spinning liquid is carried out spinning by the coagulating bath adjusted, and nascent tow obtains shaping tow after drawing-off; Shaping tow is concise through cut-out, mitigation sulfur removal technology, finish application bath and washing, after oven dry, obtains having Radix Isatidis cellulose fibre that is antiviral, functions of skin protection and health care;
In coagulating bath, the concentration of sulfuric acid is 89g/L, the concentration of aluminum sulfate is 3.1g/L, sulfuric acid zinc concentration is 8.8g/L, the concentration of sodium sulphate is 291g/L; Desulfurization is bathed: Na
2sO
37.2g/L, oil bath: 5.3g/L, does not bleach, bake out temperature: 106 DEG C, and drying time is 44min.
Prepared by the present embodiment having is antiviral, the specification of the Radix Isatidis cellulose fibre of functions of skin protection and health care is 1.67dtex*38mm, through antiviral test and ingredient analysis, compared with conventional viscose rayon, it is 86.1% to the inactivation ratio of influenza A virus, to the inactivation ratio 85.3% of herpesviral, containing the vitamin of 1.17% and the gelatin protein of 7.0% in fiber, containing several amino acids trace element, product physical index can reach the requirement of GB/T14463-2008 " viscose staple fibre " Grade A.
Embodiment 3
The preparation of the isatis root extract vitamin protein composite micro-capsule of the present embodiment
Step 1: preparation has the mixing and emulsifying solution of isatis root extract and vitamin
Emulsifier tween 80 is joined in distilled water, is stirred well under room temperature and dissolves completely, form emulsifier solution; Join in emulsifier solution by isatis root extract and vitamin, the mass ratio of isatis root extract and vitamin is 3:1, and high speed shear emulsion dispersion 26min under 1500r/min rotating speed obtains the mixing and emulsifying solution containing isatis root extract and vitamin; Wherein the quality of emulsifying agent is 2.0% of isatis root extract and vitamin gross weight, and in mixing and emulsifying solution, the gross mass mark of isatis root extract and vitamin is 28%;
Step 2: prepare isatis root extract vitamin protein composite micro-capsule
Preparation mass fraction is the gelatin solution of 6.5%, and mixing and emulsifying solution step 1 gained being contained isatis root extract and vitamin joins in gelatin solution, and the gross mass of isatis root extract and vitamin and the mass ratio of gelatin are 1:2; The gumwater that mass fraction is 8.2% is added after stirring, in gumwater, in the content of Arabic gum and gelatin solution, the mass ratio of gelatin is 1:1.5, continuing stirring makes gelatin solution fully mix with gumwater, forms stable O/w emulsion; Adjust ph is 4.2, heating water bath 43 DEG C, stirs and carries out complex coacervation, obtain suspension;
Suspension is cooled to 5 DEG C, add curing agent TGase and regulate pH to be 8.6, carry out cross-linking reaction 39min, reduce mixing speed, filter after continuing reaction 1.4h, namely obtain with isatis root extract-vitamin for core, gelatin is the isatis root extract vitamin protein composite micro-capsule of wall material, its particle diameter D97≤2.427 μm;
The preparation method of the Radix Isatidis cellulose fibre of the present embodiment, comprises 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, the content of alpha cellulose is 8.2%; Front injection device is spun in utilization, isatis root extract vitamin protein composite micro-capsule is joined in viscose glue stoste, the gross mass of isatis root extract, vitamin and gelatin is 8.0% of alpha cellulose quality, prepares co-blended spinning liquid after mixing through common process;
Step b: spinning and post processing
Co-blended spinning liquid is carried out spinning by the coagulating bath adjusted, and nascent tow obtains shaping tow after drawing-off; Shaping tow is concise through cut-out, mitigation sulfur removal technology, finish application bath and washing, after oven dry, obtains having Radix Isatidis cellulose fibre that is antiviral, functions of skin protection and health care;
In coagulating bath, the concentration of sulfuric acid is 95g/L, the concentration of aluminum sulfate is 4.5g/L, sulfuric acid zinc concentration is 8.2g/L, the concentration of sodium sulphate is 298g/L; Desulfurization is bathed: Na
2sO
36.6g/L, oil bath: 4.8g/L, does not bleach, bake out temperature: 110 DEG C, and drying time is 40min.
Prepared by the present embodiment having is antiviral, the specification of the Radix Isatidis cellulose fibre of functions of skin protection and health care is 1.56dtex*41mm, through antiviral test and ingredient analysis, compared with conventional viscose rayon, it is 88.5% to the inactivation ratio of influenza A virus, to the inactivation ratio 87.6% of herpesviral, containing the vitamin of 0.664% and the gelatin protein of 7.0% in fiber, containing several amino acids trace element, product physical index can reach the requirement of GB/T14463-2008 " viscose staple fibre " Grade A.
Embodiment 4
The preparation of the isatis root extract vitamin protein composite micro-capsule of the present embodiment
Step 1: preparation has the mixing and emulsifying solution of isatis root extract and vitamin
Emulsifier tween 80 is joined in distilled water, is stirred well under room temperature and dissolves completely, form emulsifier solution; Join in emulsifier solution by isatis root extract and vitamin, the mass ratio of isatis root extract and vitamin is 4:1, and high speed shear emulsion dispersion 18min under 1750r/min rotating speed obtains the mixing and emulsifying solution containing isatis root extract and vitamin; Wherein the quality of emulsifying agent is 2.6% of isatis root extract and vitamin gross weight, and in mixing and emulsifying solution, the gross mass mark of isatis root extract and vitamin is 34%;
Step 2: prepare isatis root extract vitamin protein composite micro-capsule
Preparation mass fraction is the gelatin solution of 6.5%, and mixing and emulsifying solution step 1 gained being contained isatis root extract and vitamin joins in gelatin solution, and the gross mass of isatis root extract and vitamin and the mass ratio of gelatin are 1:3; The gumwater that mass fraction is 9.1% is added after stirring, in gumwater, in the content of Arabic gum and gelatin solution, the mass ratio of gelatin is 1:1.7, continuing stirring makes gelatin solution fully mix with gumwater, forms stable O/w emulsion; Adjust ph is 5.7, heating water bath 49 DEG C, stirs and carries out complex coacervation, obtain suspension;
Suspension is cooled to 8 DEG C, add curing agent TGase and regulate pH to be 9.1, carry out cross-linking reaction 31min, reduce mixing speed, filter after continuing reaction 1.6h, namely obtain with isatis root extract-vitamin for core, gelatin is the isatis root extract vitamin protein composite micro-capsule of wall material, its particle diameter D97≤2.216 μm;
The preparation method of the Radix Isatidis cellulose fibre of the present embodiment, comprises 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, the content of alpha cellulose is 8.9%; Front injection device is spun in utilization, isatis root extract vitamin protein composite micro-capsule is joined in viscose glue stoste, the gross mass of isatis root extract, vitamin and gelatin is 10.5% of alpha cellulose quality, prepares co-blended spinning liquid after mixing through common process;
Step b: spinning and post processing
Co-blended spinning liquid is carried out spinning by the coagulating bath adjusted, and nascent tow obtains shaping tow after drawing-off; Shaping tow is concise through cut-out, mitigation sulfur removal technology, finish application bath and washing, after oven dry, obtains having Radix Isatidis cellulose fibre that is antiviral, functions of skin protection and health care;
In coagulating bath, the concentration of sulfuric acid is 107g/L, the concentration of aluminum sulfate is 4.8g/L, sulfuric acid zinc concentration is 6.9g/L, the concentration of sodium sulphate is 307g/L; Desulfurization is bathed: Na
2sO
34.3g/L, oil bath: 3.5g/L, does not bleach, bake out temperature: 116 DEG C, and drying time is 35min.
Prepared by the present embodiment having is antiviral, the specification of the Radix Isatidis cellulose fibre of functions of skin protection and health care is 2.22dtex*56mm, through antiviral test and ingredient analysis, compared with conventional viscose rayon, it is 84.3% to the inactivation ratio of influenza A virus, to the inactivation ratio 82.2% of herpesviral, containing the vitamin of 0.525% and the gelatin protein of 7.88% in fiber, containing several amino acids trace element, product physical index can reach the requirement of GB/T14463-2008 " viscose staple fibre " Grade A.
Embodiment 5
The preparation of the isatis root extract vitamin protein composite micro-capsule of the present embodiment
Step 1: preparation has the mixing and emulsifying solution of isatis root extract and vitamin
Class of emulsifying agent department 80 is joined in distilled water, is stirred well under room temperature and dissolves completely, form emulsifier solution; Join in emulsifier solution by isatis root extract and vitamin, the mass ratio of isatis root extract and vitamin is 5:1, and high speed shear emulsion dispersion 10min under 2000r/min rotating speed obtains the mixing and emulsifying solution containing isatis root extract and vitamin; Wherein the quality of emulsifying agent is 3.0% of isatis root extract and vitamin gross weight, and in mixing and emulsifying solution, the gross mass mark of isatis root extract and vitamin is 40%;
Step 2: prepare isatis root extract vitamin protein composite micro-capsule
Preparation mass fraction is the gelatin solution of 8%, and mixing and emulsifying solution step 1 gained being contained isatis root extract and vitamin joins in gelatin solution, and the gross mass of isatis root extract and vitamin and the mass ratio of gelatin are 1:1; The gumwater that mass fraction is 10.0% is added after stirring, in gumwater, in the content of Arabic gum and gelatin solution, the mass ratio of gelatin is 1:2, continuing stirring makes gelatin solution fully mix with gumwater, forms stable O/w emulsion; Adjust ph is 6.5, heating water bath 55 DEG C, stirs and carries out complex coacervation, obtain suspension;
Suspension is cooled to 10 DEG C, add curing agent TGase and regulate pH to be 9.5, carry out cross-linking reaction 20min, reduce mixing speed, filter after continuing reaction 2.0h, namely obtain with isatis root extract-vitamin for core, gelatin is the isatis root extract vitamin protein composite micro-capsule of wall material, its particle diameter D97≤2.486 μm;
The preparation method of the Radix Isatidis cellulose fibre of the present embodiment, comprises 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, the content of alpha cellulose is 9.5%; Front injection device is spun in utilization, isatis root extract vitamin protein composite micro-capsule is joined in viscose glue stoste, the gross mass of isatis root extract, vitamin and gelatin is 20.0% of alpha cellulose quality, prepares co-blended spinning liquid after mixing through common process;
Step b: spinning and post processing
Co-blended spinning liquid is carried out spinning by the coagulating bath adjusted, and nascent tow obtains shaping tow after drawing-off; Shaping tow is concise through cut-out, mitigation sulfur removal technology, finish application bath and washing, after oven dry, obtains having Radix Isatidis cellulose fibre that is antiviral, functions of skin protection and health care;
In coagulating bath, the concentration of sulfuric acid is 120g/L, the concentration of aluminum sulfate is 5g/L, sulfuric acid zinc concentration is 5g/L, the concentration of sodium sulphate is 320g/L; Desulfurization is bathed: Na
2sO
32.0g/L, oil bath: 2.0g/L, does not bleach, bake out temperature: 120 DEG C, and drying time is 30min.
Prepared by the present embodiment having is antiviral, the specification of the Radix Isatidis cellulose fibre of functions of skin protection and health care is 3.33dtex*56mm, through antiviral test and ingredient analysis, compared with conventional viscose rayon, it is 92.6% to the inactivation ratio of influenza A virus, to the inactivation ratio 91.8% of herpesviral, containing the vitamin of 0.664% and the gelatin protein of 10.0% in fiber, containing several amino acids trace element, product physical index can reach the requirement of GB/T14463-2008 " viscose staple fibre " Grade A.
Claims (10)
1. a preparation method for isatis root extract vitamin protein composite micro-capsule, is characterized in that, comprise the following steps:
Step 1: preparation has the mixing and emulsifying solution of isatis root extract and vitamin
Emulsifying agent is joined in distilled water, be stirred well under room temperature and dissolve completely, form emulsifier solution; Isatis root extract and vitamin are joined in emulsifier solution, high speed shear emulsion dispersion 10 ~ 40min under 1000r/min ~ 2000r/min rotating speed, obtain the mixing and emulsifying solution containing isatis root extract and vitamin; Wherein the quality of emulsifying agent is 1.0% ~ 3.0% of isatis root extract and vitamin gross weight, and in mixing and emulsifying solution, the gross mass mark of isatis root extract and vitamin is 15% ~ 40%;
Step 2: prepare isatis root extract vitamin protein composite micro-capsule
Preparation mass fraction is the gelatin solution of 5.0% ~ 8.0%, and mixing and emulsifying solution step 1 gained being contained isatis root extract and vitamin joins in gelatin solution, and the gross mass of isatis root extract and vitamin and the mass ratio of gelatin are 1:1 ~ 3; Adding mass fraction after stirring is 6.0% ~ 10.0% gumwater, continues stirring and gelatin solution is fully mixed with gumwater, form stable O/w emulsion; Adjust ph is 3.0 ~ 6.5, and heating water bath stirs and carries out complex coacervation, obtains suspension;
Suspension is cooled to 1 ~ 10 DEG C, add curing agent and regulate pH to be 7.5 ~ 9.5, carry out cross-linking reaction 20 ~ 50min, reduce mixing speed, filter after continuing reaction 1.0 ~ 2.0h, namely obtain with isatis root extract-vitamin for core, gelatin is the isatis root extract vitamin protein composite micro-capsule of wall material.
2. the preparation method of isatis root extract vitamin protein composite micro-capsule according to claim 1, is characterized in that, described emulsifying agent is one or more in lauryl sodium sulfate (SDS), OP-10, Tween 80 or class 80 of department.
3. the preparation method of isatis root extract vitamin protein composite micro-capsule according to claim 1, is characterized in that, the mass ratio of described isatis root extract and vitamin is 1 ~ 5:1.
4. the preparation method of isatis root extract vitamin protein composite micro-capsule according to claim 1, is characterized in that, in described gumwater, in the content of Arabic gum and gelatin solution, the mass ratio of gelatin is 1:1 ~ 2.
5. the preparation method of isatis root extract vitamin protein composite micro-capsule according to claim 1, it is characterized in that, described curing agent is the one in TGase, peroxidase, carbodiimide or glutaraldehyde.
6. the preparation method of isatis root extract vitamin protein composite micro-capsule according to claim 1, is characterized in that, described with isatis root extract-vitamin for core, gelatin is particle diameter D97≤2.5 μm of the microcapsules of wall material.
7. a preparation method for Radix Isatidis cellulose fibre, is characterized in that, comprises 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, the content of alpha cellulose is 7.2% ~ 9.5%; Front injection device is spun in utilization, isatis root extract vitamin protein composite micro-capsule described in claim 1 is joined in viscose glue stoste, the gross mass of isatis root extract, vitamin and gelatin is 8.0% ~ 20.0% of alpha cellulose quality, prepares co-blended spinning liquid after mixing through common process;
Step b: spinning and post processing
Co-blended spinning liquid is carried out spinning by the coagulating bath adjusted, and nascent tow obtains shaping tow after drawing-off; Shaping tow is concise through cut-out, mitigation sulfur removal technology, finish application bath and washing, after oven dry, obtains having Radix Isatidis cellulose fibre that is antiviral, functions of skin protection and health care.
8. the preparation method of Radix Isatidis cellulose fibre according to claim 7, it is characterized in that, in described coagulating bath, the concentration of sulfuric acid is 80 ~ 120g/L, the concentration of aluminum sulfate is 2.0 ~ 5.0g/L, sulfuric acid zinc concentration is 5.0 ~ 10.0g/L, the concentration of sodium sulphate is 280 ~ 320g/L.
9. the preparation method of Radix Isatidis cellulose fibre according to claim 7, is characterized in that, described desulfurization bath: Na
2sO
32.0 ~ 8.0g/L, oil bath: 2.0 ~ 6.0g/L, does not bleach, bake out temperature: 100 ~ 120 DEG C, and drying time is 30 ~ 50min.
10. one kind has Radix Isatidis cellulose fibre that is antiviral, functions of skin protection and health care, the Radix Isatidis cellulose fibre prepared by preparation method of Radix Isatidis cellulose fibre according to claim 7, it is characterized in that, isatis root extract containing 2.0 ~ 10.0wt%, the vitamin of 0.5 ~ 5.0wt% and the protein gelatin of 2.0 ~ 10.0wt%.
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