CN105506766B - A kind of cocos fibre cellulose fiber and preparation method thereof - Google Patents
A kind of cocos fibre cellulose fiber and preparation method thereof Download PDFInfo
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- CN105506766B CN105506766B CN201610050279.3A CN201610050279A CN105506766B CN 105506766 B CN105506766 B CN 105506766B CN 201610050279 A CN201610050279 A CN 201610050279A CN 105506766 B CN105506766 B CN 105506766B
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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
- D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
- D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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Abstract
The present invention provides a kind of cocos fibre cellulose fiber, and the cocos fibre cellulose fiber is prepared by cellulose spin dope and tuckahoe extracts blending；The cocos fibre cellulose fiber, the weight/mass percentage composition of tuckahoe extracts is 8 ~ 15%；The present invention also provides the preparation method of above-mentioned cellulose fibre；Cocos fibre cellulose fiber prepared by the present invention, tuckahoe extracts content does fracture strength up to 1.8 ~ 2.5cN/dtex, wet breaking strength up to 1.36 ~ 1.56cN/dtex, dry elongation at break up to 18.5 ~ 22.8%, residual sulfur content as little as 4.8 ~ 6.2mg/100g, overlength fiber rate≤1.0%, the dry state ultimate strength coefficient of variation up to 8 ~ 15%（CV）≤12%；Phobotaxis to dust mite is good, walks quickly and keeps away rate up to 93 ~ 99%；Good antimicrobial effect；The sustained release phase of Poria cocos is long.
Description
Technical field
The present invention relates to a kind of cocos fibre cellulose fiber and preparation method thereof, belong to fiber preparation field.
Background technology
With the progress and the improvement of people's living standards of science and technology, pursuit of the people to material and cultural life is special
It is that dressing idea also constantly changes, increasing notice is placed on the comfortableness and functionally of textile by people.
Due to being striven by itself and natural climate, grain and cotton etc. factor is influenceed the natural fibers such as traditional cotton, fiber crops, silk, hair, fiber
Feature and the aspect of yield two all far from disclosure satisfy that actual demand.
At present, one of large fiber main source is the non-renewable fossil resources in the undergrounds such as oil, coal, and another is
The plantation of the lands such as cotton, fiber crops, silk, hair, the renewable resource of cultivation.Wherein synthetic fibers are non-renewable from fossil resources
Resource, with the lasting outburst of global energy crisis, the quantity of synthesis chemical fibre will be difficult to sustainable growth.Regenerate in recent years
The development of cellulose fibre alleviates the not enough pressure of textile fabric production capacity.
Added more than common regenerated celulose fibre using cotton linter and timber as raw material by raw material performance itself and production
The limitation of work technology, the feature slower development of regenerated celulose fibre lags behind people to textile actual performance all the time
Demand.Into having entered to meet people for the exploitation of the demand modified cellulose fibre of functions of textile fabrics since 21 century
In the booming stage, the modification of major enterprises and institutions and research institutions to regenerated cellulose has carried out substantial amounts of research.
The Chinese patent of Patent No. 200910183278.6 discloses a kind of mint fibers production technology, and it is by peppermint
Oily micro mist is added in viscose spinning dope in carbon disulfide yellowing processes, and addition is the 1%- of mass percent
20%, realize effective combination of peppermint and fiber；
Application number 201210454096.X Chinese patent disclose a kind of viscose rayon containing natural antibacterial agent and its
Preparation method, the patent using Folium Isatidis extract as antiseptic to be added in the form of powder solution in rayon spinning stoste,
Wherein the addition of Folium Isatidis extract is the 1%-7% of spinning solution.Then routinely wet spinning spinneret technological forming is obtained
Viscose rayon.
The production technology of comprehensive disclosed functional fibre cellulose fiber domestic and international at present, its production method is by peppermint, greatly
The plant extracts such as leafiness are added in spinning solution in the form of a powder, inevitably there is strong acid, highly basic, height among these
Warm the problems such as, causes the problem of plant component active principle is lost in, and not only have impact on product quality, can also cause the very big of resource
Waste.
The existing cellulose fibre containing plant extracts, has the following disadvantages：
（1）The content of plant extracts is low, and the fibre machinery poor performance of preparation, residual sulfur content are high, overlength fiber rate is big, dry state
The ultimate strength coefficient of variation is big；
（2）To dust mite without walking quickly and keeping away performance；
（3）There is no fungistatic effect or fungistatic effect poor；
（4）The sustained release phase of plant extracts is short, and active principle is lost in fast.
The content of the invention
The present invention is solves above technical problem, and there is provided a kind of cocos fibre element is fine in view of the deficiencies of the prior art
Dimension and preparation method thereof, to realize following goal of the invention：
（1）Cocos fibre cellulose fiber prepared by the present invention, tuckahoe extracts content up to 8 ~ 15%, do fracture strength up to 1.8 ~
2.5cN/dtex, wet breaking strength up to 1.36 ~ 1.56cN/dtex, dry elongation at break up to 18.5 ~ 22.8%, residual sulfur content as little as
4.8 ~ 6.2mg/100g, overlength fiber rate≤1.0%, the dry state ultimate strength coefficient of variation（CV）≤12%；
（2）Cocos fibre cellulose fiber prepared by the present invention, the phobotaxis to dust mite is good, walks quickly and keeps away rate up to 93 ~ 99%；
（3）Cocos fibre cellulose fiber prepared by the present invention, good antimicrobial effect, to the bacteriostasis rates of Escherichia coli up to 95.8 ~
97.8%, to the bacteriostasis rate of staphylococcus aureus up to 95.6 ~ 98.7%；To the bacteriostasis rate of Candida albicans up to 94.0 ~ 95.9%；
（4）Cocos fibre cellulose fiber prepared by the present invention, the sustained release phase of Poria cocos is long.
In order to solve the above technical problems, the technical scheme that the present invention takes is as follows：
A kind of cocos fibre cellulose fiber, the cocos fibre cellulose fiber is total to by cellulose spin dope and tuckahoe extracts
It is blended standby；The cocos fibre cellulose fiber, the weight/mass percentage composition of tuckahoe extracts is 8 ~ 15%.
The following is the further improvement to above-mentioned technical proposal：
The cocos fibre cellulose fiber, dry fracture strength be 1.8 ~ 2.5cN/dtex, wet breaking strength be 1.36 ~
1.56cN/dtex, dry elongation at break are that 18.5 ~ 22.8%, residual sulfur content is 4.8 ~ 6.2mg/100g.
A kind of preparation method of cocos fibre cellulose fiber, the preparation method includes the preparation of Poria cocos microcapsules, adds and divide
Powder, the preparation of spinning solution, spinning.
The Poria cocos microcapsules, particle diameter is 1.9-2.2 μm, and embedding rate is 95.4-96.7%, and drugloading rate is 93.7-94.6%.
The preparation of the Poria cocos microcapsules, including prepare organic phase, the preparation organic phase, by carboxymethyl cellulose, second
Base cellulose, polyisocyanates, polyacrylic acid, after mixing, are dissolved in isobutyl acetate with 50-60g/L concentration ratio, control
Temperature processed adds tuckahoe extracts, 6-10min is stirred under the conditions of 2500-3000r/min, clarification organic phase is obtained at 6-8 DEG C.
The carboxymethyl cellulose, ethyl cellulose, polyisocyanates, the mass ratio of polyacrylic acid are 4-6:3-6:2-
4:1-2；The tuckahoe extracts, the mass concentration in organic phase is 5-6g/L.
The preparation of the Poria cocos microcapsules, including powdered Poria cocos microcapsules are prepared, it is described to prepare the micro- glue of powdered Poria cocos
Capsule, by organic phase and 0.8-1.3% emulsifier aqueous solution according to part by weight be 8：2.5 mixing, in ice-water bath, with 2500-
3000r/min rotating speed stirring reaction 10-15 minutes, vacuumizes standing 1-2h, and suction filtration, 40-45 DEG C of drying obtains powdered Poria cocos
Microcapsules.
The addition dispersant, it is the scattered of 2.5-3.2% that weight/mass percentage composition is added into Poria cocos microcapsule suspensions
Agent, the dispersant, the mass ratio of each component is 3-6 parts of single-walled carbon nanotube, 5-6 parts of palladium tin modification nano titanium oxide,
3-6 parts of isopropanolamine, 1-4 parts of silicone resin, 1-3 parts of hydroxyl magnesium silicate, 1-4 parts of polyethylene glycol oxide.
The mol ratio of the preparation of the spinning solution, cellulose and acetic anhydride is 1:2 reactions, are made cellulose diacetate,
Acetone is dissolved in, the acetone soln that diacetate fiber cellulose content is 20-25% is configured to, then adds 8-10% cosolvent ethanol,
Spinning solution is made.
The spinning, coagulation bath temperature is 45 DEG C, and pH value is 4.8-5.2, and spinning speed is 110-120m/min, total stretching
Than for 65-75%；The coagulating bath includes HCL 1.2-1.5mol/L, carboxylic acid 0.2-0.3 mol/L, carboxyl esters hydrolase 300
MU/L, saturated aqueous common salt 4-8g/L, ethyl acetate 25-30ml/L.
Using technical scheme, the beneficial effect of acquisition is：
（1）Cocos fibre cellulose fiber prepared by the present invention, tuckahoe extracts content be 8 ~ 15%, do fracture strength be 1.8 ~
2.5cN/dtex, wet breaking strength be 1.36 ~ 1.56cN/dtex, dry elongation at break be 18.5 ~ 22.8%, residual sulfur content be 4.8 ~
6.2mg/100g, overlength fiber rate≤1.0%, the dry state ultimate strength coefficient of variation（CV）≤12%；
（2）Cocos fibre cellulose fiber prepared by the present invention, the rate of walking quickly and keeping away to dust mite is 93 ~ 99%；After 40 times are washed,
Rate is walked quickly and kept away for 90.4-96.2% to dust mite；
（3）Cocos fibre cellulose fiber prepared by the present invention, the bacteriostasis rate to Escherichia coli is 95.8 ~ 97.8%, to golden yellow
Staphylococcic bacteriostasis rate is up to 95.6 ~ 98.7%；To the bacteriostasis rate of Candida albicans up to 94.0 ~ 95.9%, after washing 45 times, to gold
The bacteriostasis rate of staphylococcus aureus is up to 88.9 ~ 92.3%；To the bacteriostasis rates of Escherichia coli up to 90.2 ~ 94.3%, to Candida albicans
Bacteriostasis rate up to 87.4 ~ 91.6%；
（4）Cocos fibre cellulose fiber prepared by the present invention, the effect of the sustained release phase length also with Poria cocos, the sustained release phase of Poria cocos
Up to 1-1.5；
（5）The cocos fibre cellulose fiber prepared using 100% present invention spins fabric, and have some improvement work to hyperglycaemia
Try the cocos fibre cellulose fiber prepared using 100% present invention on, 200 people and spin fabric, after 3 months, fasting blood-glucose from
7.3-7.5 mmol/L, are averagely reduced to 6.4-6.8 mmol/L, and two hours blood glucoses are average from 11.3-11.5mmol/L after the meal
It is reduced to 9.4-9.8 mmol/L.
Embodiment
The preferred embodiments of the present invention are illustrated below, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
The specification of embodiment 1 is the preparation method of 1.11dtex*32mm cocos fibre cellulose fiber
The preparation of step 1, Poria cocos microcapsules
（1）The selection of raw material
From tuckahoe extracts, as the raw material of Poria cocos microcapsules, the tuckahoe extracts are brownish-yellow powder, 100%
80 mesh sieves are crossed, pachymaran content is 60%, content of ashes≤3.2%, moisture≤3.8%, content of beary metal≤5ppm, lead
Content≤1ppm, the ppm of arsenic content≤0.5, the ppm of mercury content≤0.4, total number of bacteria≤500cfu/g, total number of molds≤50
Cfu/g, salmonella and Escherichia coli must not detect.
（2）Prepare organic phase
Composition A is made from carboxymethyl cellulose, ethyl cellulose, polyisocyanates, polyacrylic acid, and to be dissolved in acetic acid different
In butyl acetate solution, the carboxymethyl cellulose, ethyl cellulose, polyisocyanates, the consumption of polyacrylic acid are according to parts by weight
Composition：5 parts of carboxymethyl cellulose, 3 parts of ethyl cellulose, 4 parts of polyisocyanates, 1 part of polyacrylic acid；Control composition A is in second
Mass concentration in sour isobutyl ester solution is 50g/L；Control temperature at 7 DEG C, the acetic acid that tuckahoe extracts are added into composition A is different
In butyl acetate solution, the mass concentration of tuckahoe extracts is 5g/L；8min is stirred under the conditions of 3000r/min, clarification organic phase is obtained
B。
（3）Prepare powdered Poria cocos microcapsules
From the aqueous solution of emulsifying agent preparation 1.0%, organic phase B and 1.0% emulsifier aqueous solution is added to 2500r/
In min high speed Stirring kettle, the consumption of the emulsifier aqueous solution of the organic phase B and 1.0% is by weight：
Organic phase B：8 parts, 1.0% emulsifier aqueous solution：2.5 parts, in ice-water bath, reaction 12 minutes is stirred, standing is vacuumized
1.5h, suction filtration, 40 DEG C of dryings obtain powdered Poria cocos microcapsules C；
The emulsifying agent is APES and AEO, and mass ratio is 2:1.
Prepared Poria cocos microcapsules, particle diameter is 1.9 μm, sphericity and favorable dispersibility, and embedding rate is 95.4%, carries medicine
Measure as 93.7%.
The preparation of step 2, Poria cocos microcapsule suspensions
Poria cocos microcapsules C 120g are dissolved in appropriate petroleum ether and absolute ethyl alcohol, then add deionized water 1000ml,
10ml emulsifying agent is added, Poria cocos microcapsule suspensions are prepared.
Step 3, addition dispersant
Into above-mentioned Poria cocos microcapsule suspensions, the dispersant of addition 2.5%, is uniformly dispersed, and resulting solution is D liquid.
The dispersant, the mass ratio of each component is 5 parts of single-walled carbon nanotube, 6 parts of palladium tin modification nano titanium oxide,
6 parts of isopropanolamine, 4 parts of silicone resin, 2 parts of hydroxyl magnesium silicate, 3 parts of polyethylene glycol oxide.
The palladium tin modification nano titanium oxide, the molar percentage of palladium is 0.8%, the molar percentage of tin（With tin/(tin
+ titanium) meter, the wherein mole accounting of tin is 20-30%；
The polyethylene glycol oxide, molecule relative mass 1x105~1x106。
The preparation of step 4, spinning solution
The mol ratio of cellulose and acetic anhydride is 1:2 reaction, through partly-hydrolysed, washing, stabilization processes, squeezing, drying,
Crush, cellulose diacetate be made, cellulose diacetate is dissolved in acetone, using batch dissolution technique, dissolve 7 hours,
The acetone soln that diacetate fiber cellulose content is 20% is configured to, 10% cosolvent ethanol is then added, through twice filter mistake
Filter and continuous defoaming, are made spinning solution.
The cellulose diacetate, esterification degree is 190-200, is 53.8-55.6% with reference to acid.
Step 5, spinning solution and Poria cocos mixing
By D liquid, according to the mass ratio of spinning solution 17%, it is added in spinning solution, vacuum row is stood after dispersed with stirring
Bubble, obtains E liquid.
Step 6, spinning
Above-mentioned E liquid enters coagulating bath after measuring pump-metered through candle filter and spinning head, and coagulation bath temperature is 45 DEG C, pH
It is worth for 4.8-5.2, spinning speed is 110-120m/min, and total drawing ratio is 65-75%.
Described coagulating bath includes HCL 1.2mol/L, the mol/L of carboxylic acid 0.3,300 mU of carboxyl esters hydrolase/L, full
With saline solution 8g/L, ethyl acetate 25ml/L.
Step 7, post processing
Wash, wash by alcohol, oiling, baking operation, be made product of the present invention.
By being carried out to 1.11dtex*32mm cocos fibres cellulose fiber product made from the preparation method described in embodiment 1
Detection, the testing result of wherein leading indicator is shown in Table 1：
Table 1
The specification of embodiment 2 is the preparation method of 1.33dtex*38mm cocos fibre cellulose fiber
The preparation of step 1, Poria cocos microcapsules
（1）The selection of raw material
From tuckahoe extracts, as the raw material of Poria cocos microcapsules, the tuckahoe extracts are brownish-yellow powder, 100%
80 mesh sieves are crossed, pachymaran content is 65%, content of ashes≤3.5%, moisture≤3.3%, content of beary metal≤5ppm, lead
Content≤1ppm, the ppm of arsenic content≤0.5, the ppm of mercury content≤0.4, total number of bacteria≤500cfu/g, total number of molds≤50
Cfu/g, salmonella and Escherichia coli must not detect.
（2）Prepare organic phase
Composition A is made from carboxymethyl cellulose, ethyl cellulose, polyisocyanates, polyacrylic acid, and to be dissolved in acetic acid different
In butyl acetate solution, the carboxymethyl cellulose, ethyl cellulose, polyisocyanates, the consumption of polyacrylic acid are according to parts by weight
Composition：6 parts of carboxymethyl cellulose, 4 parts of ethyl cellulose, 2 parts of polyisocyanates, 2 parts of polyacrylic acid；Control composition A is in second
Mass concentration in sour isobutyl ester solution is 60g/L；Control temperature at 8 DEG C, the acetic acid that tuckahoe extracts are added into composition A is different
In butyl acetate solution, the mass concentration of tuckahoe extracts is 6g/L；10min is stirred under the conditions of 2500r/min, clarification organic phase is obtained
B。
（3）Prepare powdered Poria cocos microcapsules
From the aqueous solution of emulsifying agent preparation 1.3%, organic phase B and 1.3% emulsifier aqueous solution is added to 2500r/
In min high speed Stirring kettle, the consumption of the emulsifier aqueous solution of the organic phase B and 1.3% is by weight：
Organic phase B：8 parts, 1.3% emulsifier aqueous solution：2.5 parts, in ice-water bath, reaction 15 minutes is stirred, standing is vacuumized
2h, suction filtration, 45 DEG C of dryings obtain powdered Poria cocos microcapsules C；
The emulsifying agent is APES and AEO, and mass ratio is 2.5:1.
Prepared Poria cocos microcapsules, particle diameter is 2.0 μm, sphericity and favorable dispersibility, and embedding rate is 95.8%, carries medicine
Measure as 94.0%.
The preparation of step 2, Poria cocos microcapsule suspensions
Poria cocos microcapsules C 120g are dissolved in appropriate petroleum ether and absolute ethyl alcohol, then add deionized water 1000ml,
10ml emulsifying agent is added, Poria cocos microcapsule suspensions are prepared.
Step 3, addition dispersant
Into above-mentioned Poria cocos microcapsule suspensions, the dispersant of addition 3.2%, is uniformly dispersed, and resulting solution is D liquid.
The dispersant, the mass ratio of each component is 6 parts of single-walled carbon nanotube, 5 parts of palladium tin modification nano titanium oxide,
5 parts of isopropanolamine, 2 parts of silicone resin, 3 parts of hydroxyl magnesium silicate, 4 parts of polyethylene glycol oxide.
The palladium tin modification nano titanium oxide, the molar percentage of palladium is 0.9%, the molar percentage of tin（With tin/(tin
+ titanium) meter, the wherein mole accounting of tin is 20-30%；
The polyethylene glycol oxide, molecule relative mass 1x105~1x106。
The preparation of step 4, spinning solution
The mol ratio of cellulose and acetic anhydride is 1:2 reaction, through partly-hydrolysed, washing, stabilization processes, squeezing, drying,
Crush, cellulose diacetate be made, cellulose diacetate is dissolved in acetone, using batch dissolution technique, dissolve 7 hours,
The acetone soln that diacetate fiber cellulose content is 25% is configured to, 10% cosolvent ethanol is then added, through twice filter mistake
Filter and continuous defoaming, are made spinning solution.
The cellulose diacetate, esterification degree is 190-200, is 53.8-55.6% with reference to acid.
Step 5, spinning solution and Poria cocos mixing
By D liquid, according to the mass ratio of spinning solution 20%, it is added in spinning solution, vacuum row is stood after dispersed with stirring
Bubble, obtains E liquid.
Step 6, spinning
Above-mentioned E liquid enters coagulating bath after measuring pump-metered through candle filter and spinning head, and coagulation bath temperature is 45 DEG C, pH
It is worth for 4.8-5.2, spinning speed is 110-120m/min, and total drawing ratio is 65-75%.
Described coagulating bath includes HCL 1.5mol/L, the mol/L of carboxylic acid 0.2,300 mU of carboxyl esters hydrolase/L, full
With saline solution 6g/L, ethyl acetate 30ml/L.
Step 7, post processing
Wash, wash by alcohol, oiling, baking operation, be made product of the present invention.
By being carried out to 1.33dtex*38mm cocos fibres cellulose fiber product made from the preparation method described in embodiment 2
Detection, the wherein testing result of leading indicator such as table 2：
Table 2
The specification of embodiment 3 is the preparation method of 1.67dtex*38mm cocos fibre cellulose fiber
The preparation of step 1, Poria cocos microcapsules
（1）The selection of raw material
From tuckahoe extracts, as the raw material of Poria cocos microcapsules, the tuckahoe extracts are brownish-yellow powder, 100%
80 mesh sieves are crossed, pachymaran content is 70%, content of ashes≤2.8%, moisture≤3.2%, content of beary metal≤5ppm, lead
Content≤1ppm, the ppm of arsenic content≤0.5, the ppm of mercury content≤0.4, total number of bacteria≤500cfu/g, total number of molds≤50
Cfu/g, salmonella and Escherichia coli must not detect.
（2）Prepare organic phase
Composition A is made from carboxymethyl cellulose, ethyl cellulose, polyisocyanates, polyacrylic acid, and to be dissolved in acetic acid different
In butyl acetate solution, the carboxymethyl cellulose, ethyl cellulose, polyisocyanates, the consumption of polyacrylic acid are according to parts by weight
Composition：5 parts of carboxymethyl cellulose, 4 parts of ethyl cellulose, 3 parts of polyisocyanates, 2 parts of polyacrylic acid；Control composition A is in second
Mass concentration in sour isobutyl ester solution is 55g/L；Control temperature at 6 DEG C, the acetic acid that tuckahoe extracts are added into composition A is different
In butyl acetate solution, the mass concentration of tuckahoe extracts is 5g/L；6min is stirred under the conditions of 2500r/min, clarification organic phase is obtained
B。
（3）Prepare powdered Poria cocos microcapsules
From the aqueous solution of emulsifying agent preparation 0.8%, organic phase B and 0.8% emulsifier aqueous solution is added to 2500r/
In min high speed Stirring kettle, the consumption of the emulsifier aqueous solution of the organic phase B and 0.8% is by weight：
Organic phase B：8 parts, 0.8% emulsifier aqueous solution：2.5 parts, in ice-water bath, reaction 10 minutes is stirred, standing is vacuumized
1h, suction filtration, 40 DEG C of dryings obtain powdered Poria cocos microcapsules C；
The emulsifying agent is APES and AEO, and mass ratio is 2:1.
Prepared Poria cocos microcapsules, particle diameter is 1.9-2.2 μm, sphericity and favorable dispersibility, and embedding rate is 96.0%,
Drugloading rate is 94.2%.
The preparation of step 2, Poria cocos microcapsule suspensions
Poria cocos microcapsules C 100g are dissolved in appropriate petroleum ether and absolute ethyl alcohol, then add deionized water 1000ml,
10ml emulsifying agent is added, Poria cocos microcapsule suspensions are prepared.
Step 3, addition dispersant
Into above-mentioned Poria cocos microcapsule suspensions, the dispersant of addition 2.8%, is uniformly dispersed, and resulting solution is D liquid.
The dispersant, the mass ratio of each component is 3 parts of single-walled carbon nanotube, 6 parts of palladium tin modification nano titanium oxide,
3 parts of isopropanolamine, 1 part of silicone resin, 2 parts of hydroxyl magnesium silicate, 3 parts of polyethylene glycol oxide.
The palladium tin modification nano titanium oxide, the molar percentage of palladium is 0.6%, the molar percentage of tin（With tin/(tin
+ titanium) meter, the wherein mole accounting of tin is 20-30%；
The polyethylene glycol oxide, molecule relative mass 1x105~1x106。
The preparation of step 4, spinning solution
The mol ratio of cellulose and acetic anhydride is 1:2 reaction, through partly-hydrolysed, washing, stabilization processes, squeezing, drying,
Crush, cellulose diacetate be made, cellulose diacetate is dissolved in acetone, using batch dissolution technique, dissolve 7 hours,
The acetone soln that diacetate fiber cellulose content is 20% is configured to, 8% cosolvent ethanol is then added, is filtered through twice filter
And continuous defoaming, spinning solution is made.
The cellulose diacetate, esterification degree is 190-200, is 53.8-55.6% with reference to acid.
Step 5, spinning solution and Poria cocos mixing
By D liquid, according to the mass ratio of spinning solution 20%, it is added in spinning solution, vacuum row is stood after dispersed with stirring
Bubble, obtains E liquid.
Step 6, spinning
Above-mentioned E liquid enters coagulating bath after measuring pump-metered through candle filter and spinning head, and coagulation bath temperature is 45 DEG C, pH
It is worth for 4.8-5.2, spinning speed is 110-120m/min, and total drawing ratio is 65-75%.
Described coagulating bath includes HCL 1.5mol/L, the mol/L of carboxylic acid 0.2,300 mU of carboxyl esters hydrolase/L, full
With saline solution 4g/L, ethyl acetate 25ml/L.
Step 7, post processing
Wash, wash by alcohol, oiling, baking operation, be made product of the present invention.
By being carried out to 1.67dtex*38mm cocos fibres cellulose fiber product made from the preparation method described in embodiment 3
Detection, the testing result of wherein leading indicator is shown in Table 3：
Table 3
The specification of embodiment 4 is the preparation method of 2.22dtex*38mm cocos fibre cellulose fiber
The preparation of step 1, Poria cocos microcapsules
（1）The selection of raw material
From tuckahoe extracts, as the raw material of Poria cocos microcapsules, the tuckahoe extracts are brownish-yellow powder, 100%
80 mesh sieves are crossed, pachymaran content is 60%, content of ashes≤3.0%, moisture≤3.0%, content of beary metal≤5ppm, lead
Content≤1ppm, the ppm of arsenic content≤0.5, the ppm of mercury content≤0.4, total number of bacteria≤500cfu/g, total number of molds≤50
Cfu/g, salmonella and Escherichia coli must not detect.
（2）Prepare organic phase
Composition A is made from carboxymethyl cellulose, ethyl cellulose, polyisocyanates, polyacrylic acid, and to be dissolved in acetic acid different
In butyl acetate solution, the carboxymethyl cellulose, ethyl cellulose, polyisocyanates, the consumption of polyacrylic acid are according to parts by weight
Composition：4 parts of carboxymethyl cellulose, 6 parts of ethyl cellulose, 3 parts of polyisocyanates, 1 part of polyacrylic acid；Control composition A is in second
Mass concentration in sour isobutyl ester solution is 60g/L；Control temperature at 8 DEG C, the acetic acid that tuckahoe extracts are added into composition A is different
In butyl acetate solution, the mass concentration of tuckahoe extracts is 6g/L；8min is stirred under the conditions of 2500r/min, clarification organic phase is obtained
B。
（3）Prepare powdered Poria cocos microcapsules
From the aqueous solution of emulsifying agent preparation 0.9%, organic phase B and 0.9% emulsifier aqueous solution is added to 3000r/
In min high speed Stirring kettle, the consumption of the emulsifier aqueous solution of the organic phase B and 0.9% is by weight：
Organic phase B：8 parts, 0.9% emulsifier aqueous solution：2.5 parts, in ice-water bath, reaction 12 minutes is stirred, standing is vacuumized
1.2h, suction filtration, 45 DEG C of dryings obtain powdered Poria cocos microcapsules C；
The emulsifying agent is APES and AEO, and mass ratio is 2:1.
Prepared Poria cocos microcapsules, particle diameter is 2.2 μm, sphericity and favorable dispersibility, and embedding rate is 96.7%, carries medicine
Measure as 94.6%.
The preparation of step 2, Poria cocos microcapsule suspensions
Poria cocos microcapsules C 110g are dissolved in appropriate petroleum ether and absolute ethyl alcohol, then add deionized water 1000ml,
15ml emulsifying agent is added, Poria cocos microcapsule suspensions are prepared.
Step 3, addition dispersant
Into above-mentioned Poria cocos microcapsule suspensions, the dispersant of addition 2.8%, is uniformly dispersed, and resulting solution is D liquid.
The dispersant, the mass ratio of each component is 6 parts of single-walled carbon nanotube, 5 parts of palladium tin modification nano titanium oxide,
3 parts of isopropanolamine, 2 parts of silicone resin, 1 part of hydroxyl magnesium silicate, 1 part of polyethylene glycol oxide.
The palladium tin modification nano titanium oxide, the molar percentage of palladium is 0.8%, the molar percentage of tin（With tin/(tin
+ titanium) meter, the wherein mole accounting of tin is 20-30%；
The polyethylene glycol oxide, molecule relative mass 1x105~1x106。
The preparation of step 4, spinning solution
The mol ratio of cellulose and acetic anhydride is 1:2 reaction, through partly-hydrolysed, washing, stabilization processes, squeezing, drying,
Crush, cellulose diacetate be made, cellulose diacetate is dissolved in acetone, using batch dissolution technique, dissolve 7 hours,
The acetone soln that diacetate fiber cellulose content is 20% is configured to, 8% cosolvent ethanol is then added, is filtered through twice filter
And continuous defoaming, spinning solution is made.
The cellulose diacetate, esterification degree is 190-200, is 53.8-55.6% with reference to acid.
Step 5, spinning solution and Poria cocos mixing
By D liquid, according to the mass ratio of spinning solution 25%, it is added in spinning solution, vacuum row is stood after dispersed with stirring
Bubble, obtains E liquid.
Step 6, spinning
Above-mentioned E liquid enters coagulating bath after measuring pump-metered through candle filter and spinning head, and coagulation bath temperature is 45 DEG C, pH
It is worth for 4.8-5.2, spinning speed is 110-120m/min, and total drawing ratio is 65-75%.
Described coagulating bath includes HCL 1.5mol/L, the mol/L of carboxylic acid 0.2,300 mU of carboxyl esters hydrolase/L, full
With saline solution 4g/L, ethyl acetate 25ml/L.
Step 7, post processing
Wash, wash by alcohol, oiling, baking operation, be made product of the present invention.
By being carried out to 2.22dtex*38mm cocos fibres cellulose fiber product made from the preparation method described in embodiment 4
Detection, the testing result of wherein leading indicator is shown in Table 4：
Table 4
To 1-4 of the embodiment of the present invention prepare cocos fibre cellulose fiber also carried out the sustained release phase, to staphylococcus aureus,
Candida albicans fungistatic effect is tested, 5 are the results are shown in Table；
Table 5
Cocos fibre cellulose fiber performance prepared by the present invention is summarized：
（1）By being detected to the cocos fibre cellulose fiber prepared by above-described embodiment 1 ~ 4, obtained cellulose fiber
Dimension, tuckahoe extracts content is 8 ~ 15%, and dry fracture strength is that 1.8 ~ 2.5cN/dtex, wet breaking strength are 1.36 ~ 1.56cN/
Dtex, dry elongation at break be 18.5 ~ 22.8%, residual sulfur content be 4.8 ~ 6.2mg/100g, overlength fiber rate≤1.0%, dry state break
Split the strength coefficient of variation（CV）≤12%.
（2）Cocos fibre cellulose fiber prepared by the present invention, the rate of walking quickly and keeping away to dust mite is 93 ~ 99%；After 40 times are washed,
Rate is walked quickly and kept away for 90.4-96.2% to dust mite.
（3）Cocos fibre cellulose fiber prepared by the present invention, the bacteriostasis rate to Escherichia coli is 95.8 ~ 97.8%,
To the bacteriostasis rate of staphylococcus aureus up to 95.6 ~ 98.7%；To the bacteriostasis rate of Candida albicans up to 94.0 ~ 95.9%
, after washing 45 times, to the bacteriostasis rate of staphylococcus aureus up to 88.9 ~ 92.3%；The bacteriostasis rate of Escherichia coli is reached
90.2 ~ 94.3%, to the bacteriostasis rate of Candida albicans up to 87.4 ~ 91.6%.
（4）Cocos fibre cellulose fiber prepared by the present invention, the effect of the sustained release phase length also with Poria cocos, the sustained release phase of Poria cocos
Up to 1-1.5.
（5）The cocos fibre cellulose fiber prepared using 100% present invention spins fabric, and have some improvement work to hyperglycaemia
Try the cocos fibre cellulose fiber prepared using 100% present invention on, 200 people and spin fabric, after 3 months, fasting blood-glucose from
7.3-7.5 mmol/L, are averagely reduced to 6.4-6.8 mmol/L, and two hours blood glucoses are average from 11.3-11.5mmol/L after the meal
It is reduced to 9.4-9.8 mmol/L.
Cellulose fibre cost input prepared by embodiment 3 is minimum, and the cellulose fibre performance highest prepared, is
A kind of optimal production and processing method.
Unless otherwise indicated, the percentage employed in the present invention is mass percent, and described ratio is quality
Ratio.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic.
Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., should be included in the present invention's
Within protection domain.
Claims (4)
1. a kind of preparation method of cocos fibre cellulose fiber, it is characterised in that：The cocos fibre cellulose fiber is spun by cellulose
Prepared by silk stock solution and tuckahoe extracts blending；The cocos fibre cellulose fiber, the weight/mass percentage compositions of tuckahoe extracts for 8 ~
15%；
The preparation method includes the preparation of Poria cocos microcapsules, adds dispersant, the preparation of spinning solution, spinning；
The addition dispersant, the dispersant that weight/mass percentage composition is 2.5-3.2%, institute are added into Poria cocos microcapsule suspensions
Dispersant is stated, the mass ratio of each component is 3-6 parts of single-walled carbon nanotube, 5-6 parts of palladium tin modification nano titanium oxide, isopropanol
3-6 parts of amine, 1-4 parts of silicone resin, 1-3 parts of hydroxyl magnesium silicate, 1-4 parts of polyethylene glycol oxide；
The Poria cocos microcapsules, particle diameter is 1.9-2.2 μm, and embedding rate is 95.4-96.7%, and drugloading rate is 93.7-94.6%；
The preparation of the Poria cocos microcapsules, including organic phase is prepared, the preparation organic phase is fine by carboxymethyl cellulose, ethyl
Element, polyisocyanates, polyacrylic acid are tieed up, after mixing, is dissolved in 50-60g/L concentration ratio in isobutyl acetate, control temperature
Degree adds tuckahoe extracts, 6-10min is stirred under the conditions of 2500-3000r/min, clarification organic phase is obtained at 6-8 DEG C；
The carboxymethyl cellulose, ethyl cellulose, polyisocyanates, the mass ratio of polyacrylic acid are 4-6:3-6:2-4:1-
2；The tuckahoe extracts, the mass concentration in organic phase is 5-6g/L；
The preparation of the Poria cocos microcapsules, including powdered Poria cocos microcapsules are prepared, it is described to prepare powdered Poria cocos microcapsules, will
Organic phase and 0.8-1.3% emulsifier aqueous solution are 8 according to part by weight：2.5 mixing, in ice-water bath, with 2500-
3000r/min rotating speed stirring reaction 10-15 minutes, vacuumizes standing 1-2h, and suction filtration, 40-45 DEG C of drying obtains powdered Poria cocos
Microcapsules.
2. a kind of preparation method of cocos fibre cellulose fiber according to claim 1, it is characterised in that：The cocos fibre
Cellulose fiber, dry fracture strength is that 1.8 ~ 2.5cN/dtex, wet breaking strength are that 1.36 ~ 1.56cN/dtex, dry elongation at break are
18.5 ~ 22.8%, residual sulfur content is 4.8 ~ 6.2mg/100g.
3. a kind of preparation method of cocos fibre cellulose fiber according to claim 1, it is characterised in that：The spinning solution
Preparation, the mol ratio of cellulose and acetic anhydride is 1:2 reactions, are made cellulose diacetate, are dissolved in acetone, be configured to two acetic acid
Content of cellulose is 20-25% acetone soln, then adds 8-10% cosolvent ethanol, spinning solution is made.
4. a kind of preparation method of cocos fibre cellulose fiber according to claim 1, it is characterised in that：The spinning, coagulates
Gu bath temperature is 45 DEG C, pH value is 4.8-5.2, and spinning speed is 110-120m/min, and total drawing ratio is 65-75%；The solidification
Bath includes HCL 1.2-1.5mol/L, carboxylic acid 0.2-0.3 mol/L, 300 mU of carboxyl esters hydrolase/L, saturated aqueous common salt 4-
8g/L, ethyl acetate 25-30ml/L.
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