CN107761183A - It is a kind of with antibacterial, health care, skin-protecting function vegetative fiber cellulose fiber and preparation method thereof - Google Patents
It is a kind of with antibacterial, health care, skin-protecting function vegetative fiber cellulose fiber and preparation method thereof Download PDFInfo
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- CN107761183A CN107761183A CN201711161644.9A CN201711161644A CN107761183A CN 107761183 A CN107761183 A CN 107761183A CN 201711161644 A CN201711161644 A CN 201711161644A CN 107761183 A CN107761183 A CN 107761183A
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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
- D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
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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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- 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
- B01J13/20—After-treatment of capsule walls, e.g. hardening
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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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
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- Textile Engineering (AREA)
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
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Abstract
The invention discloses it is a kind of with antibacterial, health care, skin-protecting function vegetative fiber cellulose fiber and preparation method thereof, with cellulose pulp, Radix Codonopsis extract, angelica extract and isatis root extract etc. for primary raw material, " the two layers of cyst wall " compound additive of preparation and cellulose fibre spinning solution are sufficiently mixed to the primary blended liquid for preparing high compound additive content, primary blended liquid is added in spinning solution using injection device before spinning and carries out " secondary mixing " raising mixing uniformity.Inhibiting rate >=93.8% of the fiber to staphylococcus aureus, to inhibiting rate >=90.2% of Escherichia coli, to inhibiting rate >=90.8% of Candida albicans, several amino acids content >=3.2mg/kg in fiber, containing 12 kinds of trace elements such as iron, selenium, zinc, potassium, calcium, phosphorus and vitamin B1, B2 etc., assign fiber excellent antibacterial, health care and skin-protecting function using feature component contained in Radix Codonopsis, Radix Angelicae Sinensis and Radix Isatidis.
Description
Technical field
The invention belongs to technical field of fiber preparation, is related to a kind of functional cellulose fiber producing processes, more particularly to
One kind prepares composite micro-capsule using the vegetalitas such as Radix Codonopsis, Radix Angelicae Sinensis and Radix Isatidis antiseptic and health-care and skin-care auxiliary agent as raw material, and
For prepare with antibacterial, health care, skin-protecting function cellulose fibre method.
Background technology
With the development of science and technology and growth in the living standard, there is the fiber and its textile of healthcare function no matter
Gratifying results are all achieved in technological development or product development.Meanwhile people are not only satisfied with to fiber textile
Simple function demand, high-performance, multi-functional fiber textile continue to bring out, the development of multi-functional fiber, are chemical fibre productions
One of important directions of industry development.Therefore, these have fashion and health concurrently, have the multifunctionality fiber such as health keeping and medical function
And piece market has a high potential, and the target pursued as people.
Chinese patent ZL201010592931.7 disclose in a kind of pearl with functions of skin protection and health care drug fiber and its
Preparation method, the skin-protection and health-care fiber in the patent is by cellulose fibre 90 ~ 95%；What pearl 2 ~ 5% and Chinese medicine 2 ~ 5% formed,
Chinese medicine is any of pseudo-ginseng, Radix Angelicae Sinensis, the red sage root or a variety of combinations.The fiber in preparation process, be by pearl powder, in
Medicine component is added directly into viscose glue stoste, due in production process of viscose fiber, to use sodium hydroxide, carbon disulfide with
And the industrial chemicals such as sulfuric acid, therefore pearl powder, traditional Chinese medicinal components can be destroyed in the fiber production process, have a strong impact on fibre
The feature of dimension.
Chinese patent CN201610091214.3 discloses a kind of with antiviral, antibacterial, the smalt of functions of skin protection and health care
Leaf fibre cellulose fiber and preparation method thereof, the preparation method comprise the following steps：1st, Folium Isatidis extract-Sodium Caseinate is compound micro-
The preparation of capsule；2nd, the preparation of co-blended spinning stoste；3rd, spinning and post processing.In the fiber manufacturing process, the smalt of preparation
The shaping system of leaf extract-Sodium Caseinate composite micro-capsule and cellulose fibre is incompatible, in microcapsules addition or follow-up
In fiber formation process, the destruction to microcapsules is larger, so as to influence the feature of subsequent fiber.
The content of the invention
In order to solve problems of the prior art, the invention discloses a kind of with antibacterial, health care, skin-protecting function
Vegetative fiber cellulose fiber and preparation method thereof, obtain one kind and contain Radix Codonopsis extract, angelica extract and isatis root extract
Fiber, compared with conventional viscose rayon, the fiber is to inhibiting rate >=93.8% of staphylococcus aureus, to Escherichia coli
Inhibiting rate >=90.2%, to inhibiting rate >=90.8% of Candida albicans, several amino acids content >=3.2mg/kg in fiber, contain
12 kinds of trace elements such as iron, selenium, zinc, potassium, calcium, phosphorus and vitamin B1, B2 etc., contained by Radix Codonopsis, Radix Angelicae Sinensis and Radix Isatidis
Feature component assign fiber excellent antibacterial, health care and skin-protecting function.
The technical proposal of the invention is realized in this way：
The invention discloses it is a kind of with antibacterial, health care, skin-protecting function vegetative fiber cellulose fiber, containing mass percent not
Compound additive more than 15%, the compound additive are mixed by Radix Codonopsis extract, angelica extract and isatis root extract
Form.
The invention also discloses it is a kind of with antibacterial, health care, skin-protecting function vegetative fiber cellulose fiber preparation side
Method, this method are achieved by the steps of：
（1）The preparation of Radix Codonopsis extract, angelica extract and isatis root extract composite micro-capsule
1）The preparation of primary microcapsules slurry
Emulsifying agent and compound additive are added in distilled water, the high speed shear breast under the r/min rotating speeds of 2500r/min ~ 3000
Change scattered 20 ~ 30min, obtain emulsified solution；Initiator dissolving is added into emulsified solution, metering system is added after dissolving completely
Sour methyl esters, it is sufficiently stirred at 40 ~ 50 DEG C, obtains the emulsion dispersion system that emulsion particle diameter is D90≤2.568 μm；By emulsification point
Granular media system is warming up to 62 ~ 70 DEG C and polymerize, and polymerization time is 1.5 ~ 2.5h, and the primary of particle diameter D90≤2.782 μm is prepared
Microcapsules slurry；Preferably, the dosage of the emulsifying agent is the 0.5%~3.0% of compound additive dosage；It is compound in emulsified solution
The mass fraction of additive is 20% ~ 50%；The mass ratio of compound additive and methyl methacrylate is 4:1~1:1, initiator
Addition be methyl methacrylate quality 0.5% ~ 1.5%；Preferably, the emulsifying agent is lauryl sodium sulfate
(SDS), the initiator is benzoyl peroxide；
Wherein, the compound additive is mixed in any proportion by Radix Codonopsis extract, angelica extract and isatis root extract
Obtain；
2）The preparation of " two layers of cyst wall " compound additive slurry
To step 2）The beta-schardinger dextrin that mass fraction is 10% ~ 15% is added in the primary microcapsules slurry of gained, is 200 in rotating speed
After being dispersed with stirring 90~180min under conditions of~500r/min, obtain the compound additive that two layers of cyst wall are beta-schardinger dextrin and starch
Material, its solid content are 20%~50%, particle diameter D90≤2.917 μm；
3）Prepare cellulose fibre spinning solution
By the pulp of the degree of polymerization 800 ~ 1000 by dipping, squeezing, crushing, experienced, yellow generation cellulose xanthate；Cellulose
Xanthate acid carries out obtaining spinning solution after just dissolving；Dissolving, deaeration, filtering, maturation after spinning solution is carried out successively, fiber is made
Cellulose fiber spinning solution；By step 2）Obtained compound additive slurry and cellulose fibre spinning solution rotating speed be 300~
10 ~ 20min is stirred under conditions of 600r/min and obtains primary co-blended spinning stoste；
Wherein, first in the compound additive and cellulose fibre spinning solution of compound additive slurry in primary co-blended spinning stoste
Fine mass ratio is 1:2；
4）Prepare final cellulose fibre spinning solution
In order to improve scattered uniformity, by step 3）Obtained primary co-blended spinning stoste is added to using injection system before spinning
In viscose rayon stoste pipeline, final cellulose fibre spinning solution is obtained, dynamic mixer rotating speed in injection device before spinning >=
2500r/min；Preferably, compound additive is accounted in final cellulose fibre spinning solution in final cellulose fibre spinning solution
The mass percent of first fibre content is 5% ~ 15%；
（2）Spinning and post processing
Dynamic mixer rotating speed >=2500r/min in injection device before spinning；Wet spinning is carried out in spinning-drawing machine, it is anti-in coagulating bath
As-spun fibre should be obtained；As-spun fibre is cut off and post-processed after drafting machine drawing-off, wherein aftertreatment technology includes acid
Wash, desulfurization, washing, be crosslinked, oil, dry after, that is, obtain that there is antibacterial, health care, the vegetative fiber cellulose fiber of skin-protecting function.
Wherein, in the cross-linking process step in aftertreatment technology, crosslinker solution used is by citric acid or butanetetra-carboxylic acid：Secondary Asia
Sodium phosphate or sodium dihydrogen phosphate or disodium hydrogen phosphate：Water presses 50 ~ 100：5~25：1000 weight is than mixing, the crosslinking
Process is crosslinked to be continuous, each 10~20min of crosslinking time；40~70 DEG C of crosslinking temperature, so as to realize outer layer cyst wall and fiber
The crosslinking of cellulose fiber matrix, it is dehydrated after continuous crosslinking using roll.
It is dipping, squeezing, crushing, experienced, yellow in technical solution of the present invention, just dissolving, rear dissolving, deaeration, filtering, ripe
Into, spin before injection, pickling, desulfurization, wash, oil, the routine operation that process is those skilled in the art such as dry.
In technical solution of the present invention：Radix Codonopsis is containing polysaccharide, phenols, sterol, volatile oil, vitamin B1, B2, a variety of human bodies
Various trace elements such as necessary amino acid, scutellarein glucosid, saponin and Alkaloid, iron, selenium, zinc etc., have and increase
The effects such as strong immunity, expansion blood vessel, decompression, improvement microcirculation, enhancing hematopoiesis function；Radix Angelicae Sinensis have anti anoxia, cosmetology,
Replenishing and activating blood, antibacterial, anti arteriosclerosis effect, can adjust body's immunity；Radix Isatidis contains alkaloid, organic acid, Huang
Ketone, lignanoids, esters, amino acids, ucleosides, coumarin kind compound etc., wherein organic acid have obvious antibacterial,
Anti-endotoxin effect, and then make Radix Isatidis that there are good heat-clearing toxin-expelling functions and promoting blood circulation and removing blood stasis and immunological regulation, improve immune
The effect of function.
In view of Radix Codonopsis, Radix Angelicae Sinensis, Radix Isatidis have good feature, while it contains amino acid, trace element, vitamin
Deng functional materials for health care, skin care, improving immunity of human body etc. has good action.Therefore this technology with Radix Codonopsis, when
It is feature component to return with Radix Isatidis, prepare be suitable for cellulosic fibre forming and application there is antibacterial, health care, skin care
Functional additive, so as to develop with antibacterial, health care, skin-protecting function vegetative fiber cellulose fiber and its textile, it is right
China's textile industry and the health of people tool are of great significance.
The preparation of functional viscose fiber of the present invention is with cellulose pulp, Radix Codonopsis extract, angelica extract and plate
Blue root extract etc. is primary raw material, and prepared by Radix Codonopsis extract, angelica extract and isatis root extract have " two layers of capsule
The compound additive of wall ", wherein, " two layers of cyst wall " not only improves Radix Codonopsis extract, angelica extract and isatis root extract
Stability, and later use outer layer cyst wall is crosslinked with cellulose, reduces the loss of active principle in fiber.It will prepare
Compound additive and cellulose fibre spinning solution be sufficiently mixed the primary blended liquid for preparing high compound additive content, utilization
Primary blended liquid is added in spinning solution by injection device before spinning carries out " secondary mixing " raising mixing uniformity.Subsequently through
Adjustment post processing body lotion, is realized " crosslinking between outer layer cyst wall and cellulose fibre matrix ".Pass through above-mentioned technique adjustment and control
System, prepare active ingredient and be lost in less, and be uniformly dispersed, realize the functional raising of fiber.
The present invention compared with prior art, has the advantages that：
（1）" two layers of cyst wall " not only improves Radix Codonopsis extract, the stability of angelica extract and isatis root extract, while after
It is continuous to be crosslinked using outer layer cyst wall with cellulose, network structure is formed, reduces the loss of feature component in fiber；
（2）The compound additive of preparation and cellulose fibre spinning solution are sufficiently mixed and prepare the first of high compound additive content
Level blended liquid, primary blended liquid is added in spinning solution using injection device before spinning and carries out " secondary mixing " raising mixing
Even property；Body lotion is post-processed subsequently through adjustment, is realized " crosslinking between outer layer cyst wall and cellulose fibre matrix "；
（3）By technique adjustment and control, prepare active ingredient and be lost in less, and be uniformly dispersed, realize fiber feature
Raising；
（4）The functional viscose fiber prepared has good antibacterial, health care and skin-protecting function, with conventional viscose rayon phase
Inhibiting rate >=93.8% than, the fiber to staphylococcus aureus, to inhibiting rate >=90.2% of Escherichia coli, to Candida albicans
Inhibiting rate >=90.8% of bacterium, several amino acids content >=3.2mg/kg in fiber, contain 12 kinds of iron, selenium, zinc, potassium, calcium, phosphorus etc.
Trace element and vitamin B1, B2 etc., therefore the fiber has good antibacterial, health care, skin-protecting function.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of specification is the preparation of the 1.33dtex*38mm vegetative fiber cellulose fiber with antibacterial, health care and skin-protecting function
Method is as follows：
（1）The preparation of Radix Codonopsis extract, angelica extract and isatis root extract composite micro-capsule
1）The preparation of primary microcapsules
By emulsifier sodium lauryl sulfate and compound additive（I.e.：Radix Codonopsis extract, angelica extract and Radix Isatidis carry
Take thing）It is added in distilled water, the dosage of emulsifier sodium lauryl sulfate is that Radix Codonopsis extract, angelica extract and plate are blue
The 0.5% of root extract gross weight, high speed shearing emulsification disperses 20min under 3000r/min rotating speeds, obtains emulsified solution, mixes
The total mass fraction of Radix Codonopsis extract, angelica extract and isatis root extract is 20% in emulsified solution, Radix Codonopsis extract,
Angelica extract and isatis root extract are arbitrary proportion；The dissolving of initiator benzoyl peroxide is added into emulsified solution,
Methyl methacrylate is added after dissolving completely, is stirred at 50 DEG C, it is the emulsification point that D90 is 2.357 μm to obtain particle diameter
Granular media system, then heat to 62 DEG C and polymerize, polymerization time 2.5h, the primary that particle diameter D90 is 2.698 μm is prepared and answers
Close microcapsules slurry；Wherein（Radix Codonopsis extract, angelica extract and isatis root extract）Total amount and methacrylic acid have
It is 1 to imitate composition quality ratio:1, the addition of initiator benzoyl peroxide is the 0.5% of methyl methacrylate quality, after emulsification
Emulsion；
2）The preparation of " two layers of cyst wall " compound additive
The beta-schardinger dextrin that mass fraction is 10% is added into the primary microcapsules slurry of above-mentioned preparation, is 500r/min in rotating speed
Under conditions of be sufficiently stirred scattered 180min after, you can obtain the compound additive slurry that two layers of cyst wall are beta-schardinger dextrin, it is solid
Content is 20%, and particle diameter D90 is 2.905 μm；
3）Prepare cellulose fibre spinning solution
By the pulp of the degree of polymerization 700 by dipping, squeezing, crushing, experienced, yellow generation cellulose xanthate；Cellulose yellow acid
Ester carries out obtaining spinning solution after just dissolving；Dissolving, deaeration, filtering, maturation after spinning solution is carried out successively, cellulose fiber is made
Tie up spinning solution；In rotating speed it is 300r/min by the compound additive slurry of preparation and cellulose fibre spinning solution, through 20min
Be stirred and prepare primary co-blended spinning stoste, wherein compound additive is spun with cellulose fibre in primary co-blended spinning stoste
First fibre mass ratio is 1 in silk stock solution:2；
4）Prepare final cellulose fibre spinning solution
In order to improve scattered uniformity, by step 3）Obtained primary co-blended spinning stoste is added to using injection system before spinning
In viscose rayon stoste pipeline, final cellulose fibre spinning solution is obtained, dynamic mixer rotating speed is in injection device before spinning
2500r/min；Compound additive accounts for first fibre in final cellulose fibre spinning solution and contained in final cellulose fibre spinning solution
The mass percent of amount is 5%；
（2）Spinning and post processing
Wet spinning is carried out in spinning-drawing machine, reacts to obtain as-spun fibre with coagulating bath；By as-spun fibre after drafting machine drawing-off
Cut off and post-processed, wherein aftertreatment technology include pickling, desulfurization, washing, be crosslinked, oil, dry after, that is, had
Antibacterial, health care, the vegetative fiber cellulose fiber of skin-protecting function.
In aftertreatment technology：The component of crosslinker solution used and the weight ratio of each component are citric acid：Sodium hypophosphite：Water
=50:5:1000；Cross-linking process is crosslinked to be continuous, each crosslinking time 20min；70 DEG C of crosslinking temperature, so as to realize outer layer cyst wall
With the crosslinking of cellulose fibre matrix, it is dehydrated after continuous crosslinking using roll.
By to 1.33dtex*38mm made from the preparation method described in embodiment 1, there is antibacterial, health care and skin care work(
The vegetative fiber cellulose fiber of energy carries out antibacterial test and ingredient analysis, and compared with conventional viscose rayon, the fiber is to golden yellow
Staphylococcic inhibiting rate is 93.8%, and the inhibiting rate to Escherichia coli is 90.2%, and the inhibiting rate to Candida albicans is
90.8%, several amino acids content is 3.2mg/kg in fiber, contains 12 kinds of trace elements such as iron, selenium, zinc, potassium, calcium, phosphorus and dimension
Raw plain B1, B2 etc., therefore the fiber has good antibacterial, health care, skin-protecting function.
Embodiment 2
A kind of specification is the preparation of the 1.67dtex*38mm vegetative fiber cellulose fiber with antibacterial, health care and skin-protecting function
Method is as follows：
（1）The preparation of Radix Codonopsis extract, angelica extract and isatis root extract composite micro-capsule
1）The preparation of primary microcapsules
Emulsifier sodium lauryl sulfate and Radix Codonopsis extract, angelica extract and isatis root extract are added to distillation
In water, the dosage of emulsifier sodium lauryl sulfate is Radix Codonopsis extract, angelica extract and isatis root extract gross weight
1.2%, high speed shearing emulsification disperses 22min under 2880r/min rotating speeds, obtains emulsified solution, Radix Codonopsis in mixing and emulsifying solution
The total mass fraction of extract, angelica extract and isatis root extract be 26%, Radix Codonopsis extract, angelica extract and
Isatis root extract is arbitrary proportion；The dissolving of initiator benzoyl peroxide is added into emulsified solution, is added after dissolving completely
Methyl methacrylate, it is the emulsion dispersion system that D90 is 2.567 μm to be sufficiently stirred to obtain particle diameter at 48 DEG C, is then heated up
It is polymerize to 65 DEG C, polymerization time 2.2h, the primary composite micro-capsule slurry that particle diameter D90 is 2.764 μm is prepared；
Wherein（Radix Codonopsis extract, angelica extract and Radix Isatidis extraction）The active ingredient mass ratio of total amount and methacrylic acid
For 2:1, the addition of initiator benzoyl peroxide is the 0.75% of methyl methacrylate quality；
2）The preparation of " two layers of cyst wall " compound additive
The beta-schardinger dextrin that mass fraction is 11.1% is added into the primary microcapsules slurry of above-mentioned preparation, is 436 r/ in rotating speed
After min sufficient condition is dispersed with stirring 156min, you can obtain the compound additive slurry that two layers of cyst wall are beta-schardinger dextrin, finally
The solid content of compound additive slurry is 28.8%, and particle diameter D90 is 2.913 μm；
3）Prepare cellulose fibre spinning solution
By the pulp of the degree of polymerization 865 by dipping, squeezing, crushing, experienced, yellow generation cellulose xanthate；Cellulose yellow acid
Ester carries out obtaining spinning solution after just dissolving；Dissolving, deaeration, filtering, maturation after spinning solution is carried out successively, cellulose fiber is made
Tie up spinning solution；In rotating speed it is 365r/min by the compound additive slurry of preparation and cellulose fibre spinning solution, through 18min
Be stirred and prepare primary co-blended spinning stoste, wherein compound additive is spun with cellulose fibre in primary co-blended spinning stoste
First fibre mass ratio is 1 in silk stock solution:2；
4）Prepare final cellulose fibre spinning solution
In order to improve scattered uniformity, by step 3）Obtained primary co-blended spinning stoste is added to using injection system before spinning
In viscose rayon stoste pipeline, final cellulose fibre spinning solution is obtained, dynamic mixer rotating speed is in injection device before spinning
2880r/min；Compound additive accounts for first fibre in final cellulose fibre spinning solution and contained in final cellulose fibre spinning solution
The mass percent of amount is 7.9%；
（2）Spinning and post processing
Wet spinning is carried out in spinning-drawing machine, is reacted with coagulating bath, obtains as-spun fibre；As-spun fibre drafting machine drawing-off is laggard
Row cut-out and post processing, wherein aftertreatment technology include pickling, desulfurization, washing, be crosslinked, oil, dry after, that is, obtain having and resist
Bacterium, health care, the vegetative fiber cellulose fiber of skin-protecting function.
In aftertreatment technology：The component of crosslinker solution used and the weight ratio of each component are citric acid：Sodium dihydrogen phosphate：Water
=62:13:1000；Cross-linking process is crosslinked to be continuous, each crosslinking time 17min；65.8 DEG C of crosslinking temperature, so as to realize outer layer
The crosslinking of cyst wall and cellulose fibre matrix, it is dehydrated after continuous crosslinking using roll.
By to 1.67dtex*38mm made from the preparation method described in embodiment 2, there is antibacterial, health care and skin care work(
The vegetative fiber cellulose fiber of energy carries out antibacterial test and ingredient analysis, and compared with conventional viscose rayon, the fiber is to golden yellow
Staphylococcic inhibiting rate is 94.9%, and the inhibiting rate to Escherichia coli is 91.5%, and the inhibiting rate to Candida albicans is
92.2%, several amino acids content is 4.1mg/kg in fiber, contains 12 kinds of trace elements such as iron, selenium, zinc, potassium, calcium, phosphorus and dimension
Raw plain B1, B2 etc., therefore the fiber has good antibacterial, health care, skin-protecting function.
Embodiment 3
A kind of specification is the preparation of the 1.56dtex*38mm vegetative fiber cellulose fiber with antibacterial, health care and skin-protecting function
Method is as follows：
（1）The preparation of Radix Codonopsis extract, angelica extract and isatis root extract composite micro-capsule
1）The preparation of primary microcapsules
Emulsifier sodium lauryl sulfate and Radix Codonopsis extract, angelica extract and isatis root extract are added to distillation
In water, the dosage of emulsifier sodium lauryl sulfate is Radix Codonopsis extract, angelica extract and isatis root extract gross weight
2.3%, high speed shearing emulsification disperses 26min under 2678 r/min rotating speeds, obtains emulsified solution, party in mixing and emulsifying solution
The total mass fraction of conopsea extraction, angelica extract and isatis root extract be 38%, Radix Codonopsis extract, angelica extract with
And isatis root extract is arbitrary proportion.The addition initiator benzoyl peroxide dissolving into emulsified solution, adds after dissolving completely
Enter methyl methacrylate, it is the emulsion dispersion system that D90 is 2.568 μm to be sufficiently stirred to obtain particle diameter at 45 DEG C, Ran Housheng
Warm to 68 DEG C are polymerize, polymerization time 1.8h, and the primary composite micro-capsule slurry that particle diameter D90 is 2.782 μm is prepared；
Wherein（Radix Codonopsis extract, angelica extract and Radix Isatidis extraction）The active ingredient mass ratio of total amount and methacrylic acid
For 3:1, the addition of initiator benzoyl peroxide is the 1.20% of methyl methacrylate quality；
2）The preparation of " two layers of cyst wall " compound additive
The beta-schardinger dextrin that mass fraction is 13.5% is added into the primary microcapsules slurry of above-mentioned preparation, is 350r/ in rotating speed
Scattered 115min is sufficiently stirred under conditions of min, after, you can the compound additive slurry that two layers of cyst wall are beta-schardinger dextrin is obtained,
Its solid content is 39.2%, and particle diameter D90 is 2.917 μm；
3）Prepare cellulose fibre spinning solution
The pulp for polymerizeing 916 is passed through into dipping, squeezing, crushed, experienced, yellow generation cellulose xanthate；Cellulose xanthate
Carry out obtaining spinning solution after just dissolving；Dissolving, deaeration, filtering, maturation after spinning solution is carried out successively, cellulose fibre is made
Spinning solution；In rotating speed it is 525r/min by the compound additive slurry of preparation and cellulose fibre spinning solution, through 15min
Be stirred and prepare primary co-blended spinning stoste, wherein compound additive is spun with cellulose fibre in primary co-blended spinning stoste
First fibre mass ratio is 1 in silk stock solution:2；
4）Prepare final cellulose fibre spinning solution
In order to improve scattered uniformity, by step 3）Obtained primary co-blended spinning stoste is added to using injection system before spinning
In viscose rayon stoste pipeline, final cellulose fibre spinning solution is obtained, dynamic mixer rotating speed is in injection device before spinning
2950r/min；Compound additive accounts for first fibre in final cellulose fibre spinning solution and contained in final cellulose fibre spinning solution
The mass percent of amount is 12.8%；
（2）Spinning and post processing
Wet spinning is carried out in spinning-drawing machine, is reacted with coagulating bath, obtains as-spun fibre；As-spun fibre drafting machine drawing-off is laggard
Row cut-out and post processing, wherein aftertreatment technology include pickling, desulfurization, washing, be crosslinked, oil, dry after, that is, obtain having and resist
Bacterium, health care, the vegetative fiber cellulose fiber of skin-protecting function.
In aftertreatment technology：The component of crosslinker solution used and the weight ratio of each component are butanetetra-carboxylic acid：Disodium hydrogen phosphate：
Water=85:20:1000；Cross-linking process is crosslinked to be continuous, each crosslinking time 13min；55.6 DEG C of crosslinking temperature, so as to realize outer layer
The crosslinking of cyst wall and cellulose fibre matrix, it is dehydrated after crosslinking using roll.
By to 1.56dtex*38mm made from the preparation method described in embodiment 3, there is antibacterial, health care and skin care work(
The vegetative fiber cellulose fiber of energy carries out antibacterial test and ingredient analysis, and compared with conventional viscose rayon, the fiber is to golden yellow
Staphylococcic inhibiting rate is 95.2%, and the inhibiting rate to Escherichia coli is 92.8%, and the inhibiting rate to Candida albicans is
93.5%, several amino acids content is 5.2mg/kg in fiber, contains 12 kinds of trace elements such as iron, selenium, zinc, potassium, calcium, phosphorus and dimension
Raw plain B1, B2 etc., therefore the fiber has good antibacterial, health care, skin-protecting function.
Embodiment 4
A kind of specification is the 2.22dtex*56mm preparation with antiviral, functions of skin protection and health care Radix Isatidis cellulose fibre
Method is as follows：
（1）The preparation of Radix Codonopsis extract, angelica extract and isatis root extract composite micro-capsule
1）The preparation of primary microcapsules
Emulsifier sodium lauryl sulfate (SDS) and Radix Codonopsis extract, angelica extract and isatis root extract are added
Into distilled water, the dosage of emulsifier sodium lauryl sulfate (SDS) carries for Radix Codonopsis extract, angelica extract and Radix Isatidis
The 3.0% of thing gross weight is taken, high speed shearing emulsification disperses 30min under 2500r/min rotating speeds, obtains emulsified solution, mixing and emulsifying
The total mass fraction of Radix Codonopsis extract, angelica extract and isatis root extract is 50% in solution, Radix Codonopsis extract, Radix Angelicae Sinensis
Extract and isatis root extract are arbitrary proportion.The dissolving of initiator benzoyl peroxide, dissolving are added into emulsified solution
Methyl methacrylate is added after completely, it is the Emulsified Dispersion that D90 is 2.459 μm to be sufficiently stirred to obtain particle diameter at 40 DEG C
System, then heats to 70 DEG C and is polymerize, polymerization time 1.5h, and it is 2.653 μm primary compound micro- that particle diameter D90, which is prepared,
Capsule slurry；
Wherein（Radix Codonopsis extract, angelica extract and Radix Isatidis extraction）The active ingredient mass ratio of total amount and methacrylic acid
For 4:1, the addition of initiator benzoyl peroxide is the 1.5% of methyl methacrylate quality；
2）The preparation of " two layers of cyst wall " compound additive
The beta-schardinger dextrin that mass fraction is 15% is added into the primary microcapsules slurry of above-mentioned preparation, is 200r/min in rotating speed
Under conditions of be sufficiently stirred scattered 90min after, you can obtain two layers of cyst wall be beta-schardinger dextrin compound additive slurry, it contains admittedly
Measure as 50%, particle diameter D90 is 2.896 μm；
3）Prepare cellulose fibre spinning solution
The pulp for polymerizeing 1000 is passed through into dipping, squeezing, crushed, experienced, yellow generation cellulose xanthate；Cellulose xanthate
Carry out obtaining spinning solution after just dissolving；Dissolving, deaeration, filtering, maturation after spinning solution is carried out successively, cellulose fibre is made
Spinning solution；In rotating speed it is 600r/min by the compound additive slurry of preparation and cellulose fibre spinning solution, through 10min
Be stirred and prepare primary co-blended spinning stoste；Compound additive is spun with cellulose fibre in wherein primary co-blended spinning stoste
First fibre mass percent is 1 in silk stock solution:2；
4）Prepare final cellulose fibre spinning solution
In order to improve scattered uniformity, by step 3）Obtained primary co-blended spinning stoste is added to using injection system before spinning
In viscose rayon stoste pipeline, final cellulose fibre spinning solution is obtained, dynamic mixer rotating speed is in injection device before spinning
3100r/min；Compound additive accounts for first fibre in final cellulose fibre spinning solution and contained in final cellulose fibre spinning solution
The mass percent of amount is 15%；
（2）Spinning and post processing
Wet spinning is carried out in spinning-drawing machine, is reacted with coagulating bath, obtains as-spun fibre；As-spun fibre drafting machine drawing-off is laggard
Row cut-out and post processing, wherein aftertreatment technology include pickling, desulfurization, washing, be crosslinked, oil, dry after, that is, obtain having and resist
Bacterium, health care, the vegetative fiber cellulose fiber of skin-protecting function；
In aftertreatment technology：The component of the crosslinker solution and the weight ratio of each component are butanetetra-carboxylic acid：Disodium hydrogen phosphate：Water=
100:25:1000；Cross-linking process is crosslinked to be continuous, each crosslinking time 10min；40 DEG C of crosslinking temperature, so as to realize outer layer cyst wall
With the crosslinking of cellulose fibre matrix, it is dehydrated after crosslinking using roll.
By to 2.22dtex*56mm made from the preparation method described in embodiment 4, there is antibacterial, health care and skin care work(
The vegetative fiber cellulose fiber of energy carries out antibacterial test and ingredient analysis, and compared with conventional viscose rayon, the fiber is to golden yellow
Staphylococcic inhibiting rate is 96.8%, and the inhibiting rate to Escherichia coli is 95.6%, and the inhibiting rate to Candida albicans is
95.7%, several amino acids content is 6.4mg/kg in fiber, contains 12 kinds of trace elements such as iron, selenium, zinc, potassium, calcium, phosphorus and dimension
Raw plain B1, B2 etc., therefore the fiber has good antibacterial, health care, skin-protecting function.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (7)
1. a kind of have antibacterial, health care, the vegetative fiber cellulose fiber of skin-protecting function, it is characterised in that：Contain mass percent
Compound additive no more than 15%, the compound additive are mixed by Radix Codonopsis extract, angelica extract and isatis root extract
Close what is formed.
2. it is a kind of with antibacterial, health care, skin-protecting function vegetative fiber cellulose fiber preparation method, it is characterised in that be logical
Cross following steps realization：
（1）The preparation of Radix Codonopsis extract, angelica extract and isatis root extract composite micro-capsule
1）The preparation of primary microcapsules slurry
Emulsifying agent and compound additive are added in distilled water, the high speed shear breast under the r/min rotating speeds of 2500r/min ~ 3000
Change scattered 20 ~ 30min, obtain emulsified solution；Initiator dissolving is added into emulsified solution, metering system is added after dissolving completely
Sour methyl esters, it is sufficiently stirred at 40 ~ 50 DEG C, obtains the emulsion dispersion system that emulsion particle diameter is D90≤2.568 μm；By emulsification point
Granular media system is warming up to 62 ~ 70 DEG C and polymerize, and polymerization time is 1.5 ~ 2.5h, and the primary of particle diameter D90≤2.782 μm is prepared
Microcapsules slurry；
Wherein, the compound additive is mixed in any proportion by Radix Codonopsis extract, angelica extract and isatis root extract
Obtain；
2）The preparation of " two layers of cyst wall " compound additive slurry
To step 2）The beta-schardinger dextrin that mass fraction is 10% ~ 15% is added in the primary microcapsules slurry of gained, is 200 in rotating speed
After being dispersed with stirring 90~180min under conditions of~500r/min, obtain the compound additive that two layers of cyst wall are beta-schardinger dextrin and starch
Material, its solid content are 20%~50%, particle diameter D90≤2.917 μm；
3）Prepare cellulose fibre spinning solution
By the pulp of the degree of polymerization 800 ~ 1000 by dipping, squeezing, crushing, experienced, yellow generation cellulose xanthate；Cellulose
Xanthate acid carries out obtaining spinning solution after just dissolving；Dissolving, deaeration, filtering, maturation after spinning solution is carried out successively, fiber is made
Cellulose fiber spinning solution；By step 2）Obtained compound additive slurry and cellulose fibre spinning solution rotating speed be 300~
10 ~ 20min is stirred under conditions of 600r/min and obtains primary co-blended spinning stoste；
4）Prepare final cellulose fibre spinning solution
By step 3）Obtained primary co-blended spinning stoste is added in viscose rayon stoste pipeline using injection system before spinning, and is obtained
To final cellulose fibre spinning solution, dynamic mixer rotating speed >=2500r/min in injection device before spinning；
（2）Spinning and post processing
Wet spinning is carried out in spinning-drawing machine, reacts to obtain as-spun fibre in coagulating bath；By as-spun fibre after drafting machine drawing-off
Cut off and post-processed, wherein aftertreatment technology include pickling, desulfurization, washing, be crosslinked, oil, dry after, that is, had
Antibacterial, health care, the vegetative fiber cellulose fiber of skin-protecting function.
3. as claimed in claim 2 with antibacterial, health care, skin-protecting function vegetative fiber cellulose fiber preparation method, it is special
Sign is：Step 1）In, the dosage of the emulsifying agent is the 0.5%~3.0% of compound additive dosage；It is compound in emulsified solution to add
The mass fraction for adding agent is 20% ~ 50%；The mass ratio of compound additive and methyl methacrylate is 4:1~1:1, initiator
Addition is the 0.5% ~ 1.5% of methyl methacrylate quality.
4. as claimed in claim 3 with antibacterial, health care, skin-protecting function vegetative fiber cellulose fiber preparation method, it is special
Sign is：Step 1）In, the emulsifying agent is lauryl sodium sulfate, and the initiator is benzoyl peroxide.
5. as claimed in claim 2 with antibacterial, health care, skin-protecting function vegetative fiber cellulose fiber preparation method, it is special
Sign is：Step 3）In, the compound additive and cellulose fiber spinning of compound additive slurry in primary co-blended spinning stoste
The fine mass ratio of first is 1 in stoste:2.
6. as claimed in claim 2 with antibacterial, health care, skin-protecting function vegetative fiber cellulose fiber preparation method, it is special
Sign is：Step 4）In, compound additive is accounted in final cellulose fibre spinning solution in final cellulose fibre spinning solution
The mass percent of first fibre content is 5% ~ 15%.
7. as claimed in claim 2 with antibacterial, health care, skin-protecting function vegetative fiber cellulose fiber preparation method, it is special
Sign is：In cross-linking process step in the aftertreatment technology of step 2, crosslinker solution used is by citric acid or butanetetra-carboxylic acid：
Sodium hypophosphite or sodium dihydrogen phosphate or disodium hydrogen phosphate：Water presses 50 ~ 100：5~25：1000 weight is somebody's turn to do than what is mixed
Cross-linking process is crosslinked to be continuous, each 10~20min of crosslinking time；40~70 DEG C of crosslinking temperature, roll is used after continuous crosslinking
Dehydration.
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