CN106995943A - A kind of Chloranthus glaber efficient antibacterial antiviral cellulose fibre and preparation method thereof - Google Patents
A kind of Chloranthus glaber efficient antibacterial antiviral cellulose fibre and preparation method thereof Download PDFInfo
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- CN106995943A CN106995943A CN201710183270.4A CN201710183270A CN106995943A CN 106995943 A CN106995943 A CN 106995943A CN 201710183270 A CN201710183270 A CN 201710183270A CN 106995943 A CN106995943 A CN 106995943A
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- chitosan
- functional components
- extract
- mass ratio
- cellulose fibre
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 39
- 235000010842 Sarcandra glabra Nutrition 0.000 title claims abstract description 25
- 240000004274 Sarcandra glabra Species 0.000 title claims abstract description 25
- 230000000840 anti-viral effect Effects 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 20
- 239000000835 fiber Substances 0.000 claims abstract description 68
- 239000002245 particle Substances 0.000 claims abstract description 54
- 150000001875 compounds Chemical class 0.000 claims abstract description 51
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 48
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 48
- 239000000084 colloidal system Substances 0.000 claims abstract description 43
- 239000002131 composite material Substances 0.000 claims abstract description 43
- 229920001661 Chitosan Polymers 0.000 claims abstract description 40
- 238000009987 spinning Methods 0.000 claims abstract description 39
- 238000000465 moulding Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000000284 extract Substances 0.000 claims description 69
- 239000002253 acid Substances 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 35
- 235000016257 Mentha pulegium Nutrition 0.000 claims description 24
- 244000246386 Mentha pulegium Species 0.000 claims description 24
- 235000004357 Mentha x piperita Nutrition 0.000 claims description 24
- 235000001050 hortel pimenta Nutrition 0.000 claims description 24
- 241000334160 Isatis Species 0.000 claims description 22
- 239000004115 Sodium Silicate Substances 0.000 claims description 20
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 20
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 20
- 229920000297 Rayon Polymers 0.000 claims description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Substances CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 16
- 229960000583 acetic acid Drugs 0.000 claims description 16
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 16
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 12
- 239000003292 glue Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 229920002385 Sodium hyaluronate Polymers 0.000 claims description 8
- 229920002472 Starch Polymers 0.000 claims description 8
- 239000003505 polymerization initiator Substances 0.000 claims description 8
- 229920001451 polypropylene glycol Polymers 0.000 claims description 8
- 229940010747 sodium hyaluronate Drugs 0.000 claims description 8
- YWIVKILSMZOHHF-QJZPQSOGSA-N sodium;(2s,3s,4s,5r,6r)-6-[(2s,3r,4r,5s,6r)-3-acetamido-2-[(2s,3s,4r,5r,6r)-6-[(2r,3r,4r,5s,6r)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2- Chemical compound [Na+].CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 YWIVKILSMZOHHF-QJZPQSOGSA-N 0.000 claims description 8
- 239000008107 starch Substances 0.000 claims description 8
- 235000019698 starch Nutrition 0.000 claims description 8
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- 239000010231 banlangen Substances 0.000 claims description 7
- 238000002386 leaching Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 5
- 235000011152 sodium sulphate Nutrition 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000003431 cross linking reagent Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 230000035800 maturation Effects 0.000 claims description 4
- 239000002964 rayon Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 4
- 229960001763 zinc sulfate Drugs 0.000 claims description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 4
- 238000006477 desulfuration reaction Methods 0.000 claims description 3
- 230000023556 desulfurization Effects 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 abstract description 9
- 241000193830 Bacillus <bacterium> Species 0.000 abstract description 7
- 241000222122 Candida albicans Species 0.000 abstract description 7
- 241000712431 Influenza A virus Species 0.000 abstract description 7
- 241000713196 Influenza B virus Species 0.000 abstract description 7
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 7
- 208000037386 Typhoid Diseases 0.000 abstract description 7
- 229940095731 candida albicans Drugs 0.000 abstract description 7
- 201000008297 typhoid fever Diseases 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 6
- 230000002401 inhibitory effect Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000002155 anti-virotic effect Effects 0.000 description 10
- 230000001112 coagulating effect Effects 0.000 description 7
- 239000000956 alloy Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- 230000004520 agglutination Effects 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229940105902 mint extract Drugs 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 241000700605 Viruses Species 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 210000003743 erythrocyte Anatomy 0.000 description 2
- 235000020737 peppermint extract Nutrition 0.000 description 2
- 235000010265 sodium sulphite Nutrition 0.000 description 2
- 238000004901 spalling Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 241000758719 Chloranthaceae Species 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- STECJAGHUSJQJN-GAUPFVANSA-N Hyoscine Natural products C1([C@H](CO)C(=O)OC2C[C@@H]3N([C@H](C2)[C@@H]2[C@H]3O2)C)=CC=CC=C1 STECJAGHUSJQJN-GAUPFVANSA-N 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 229920000433 Lyocell Polymers 0.000 description 1
- STECJAGHUSJQJN-UHFFFAOYSA-N N-Methyl-scopolamin Natural products C1C(C2C3O2)N(C)C3CC1OC(=O)C(CO)C1=CC=CC=C1 STECJAGHUSJQJN-UHFFFAOYSA-N 0.000 description 1
- 208000002193 Pain Diseases 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- FUERBINMBLPVRD-UHFFFAOYSA-M [O-]S(O)=O.[Na+].S Chemical compound [O-]S(O)=O.[Na+].S FUERBINMBLPVRD-UHFFFAOYSA-M 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000001754 anti-pyretic effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 239000002221 antipyretic Substances 0.000 description 1
- 208000010668 atopic eczema Diseases 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000036737 immune function Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 206010022000 influenza Diseases 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 208000004296 neuralgia Diseases 0.000 description 1
- 230000036407 pain Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- STECJAGHUSJQJN-FWXGHANASA-N scopolamine Chemical compound C1([C@@H](CO)C(=O)O[C@H]2C[C@@H]3N([C@H](C2)[C@@H]2[C@H]3O2)C)=CC=CC=C1 STECJAGHUSJQJN-FWXGHANASA-N 0.000 description 1
- 229960002646 scopolamine Drugs 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 230000035900 sweating Effects 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Multicomponent Fibers (AREA)
Abstract
A kind of Chloranthus glaber efficient antibacterial antiviral cellulose fibre of present invention offer, the fiber, the content of chitosan functional components compound particle is 9.5 9.7%, and the content of silicic acid composite colloid is 2 3.5%;The present invention also provides a kind of preparation method of Chloranthus glaber efficient antibacterial antiviral cellulose fibre, including prepares chitosan functional components compound particle, prepares silicic acid composite colloid, blending, spinning moulding.The present invention reduces the loss or loss of functional components in fiber manufacturing process;Fiber prepared by the present invention, functional components are distributed in fibrocortex and surface portion;Fiber prepared by the present invention, is firmly combined with the functional components that graininess is embedded in fibrocortex or surface with fiber, is lost in washing and friction process few;In fiber of the present invention, influenza A virus and influenza B virus can be effective against, also there is higher inhibiting rate to staphylococcus aureus, Candida albicans, typhoid bacillus.
Description
Technical field
The present invention relates to a kind of viscose rayon, particularly a kind of Chloranthus glaber efficient antibacterial antiviral cellulose fibre and its system
Preparation Method, belongs to textile technology field.
Background technology
The development of functional fibre is the symbol of modern fiber science progress.Functional fibre, fibre in differentiation and high-performance are fine
The technological innovation for developing into traditional textile industry of dimension, creates advantage to the conversion of high-tech industry, is human lives
The raising of level contributes.Functional fibre refers in addition to the physical and mechanical properties that general fiber has, also with certain
Plant the tencel of specific function.
Radix Isatidis, is a kind of excellent Chinese medicine, with antibacterial, effect that is antiviral, antitumor, improving immunologic function;
Isatis root extract is added in viscose rayon, the textile with healthcare functions such as antiviral, raising immunity is prepared,
Meet the popular demand to the product with health care function of present society.
Chloranthus glaber, is Chloranthaceae perennial evergreen undershrub, is commonly called as spice all over the mountain, kwan-yin tea, nine joint flower, elder etc..
Its form is beautiful, four seasons fragrance, with high medicinal, edible and ornamental value;Complete stool hyoscine, can clearing heat and detoxicating, wind-dispelling
Promoting blood circulation, swelling and pain relieving, anti-inflammation.
Peppermint, is one of Chinese conventional Chinese medicine, and it is pungent cool property sweating antipyretic medicine, control influenza, headache, hot eyes,
Body heat, throat, gum such as swell and ache the disease, and external application can control neuralgia, pruitus, fash and eczema etc., and modern pharmacological research is found
The involatile constituent of peppermint has anti-inflammatory, it is antibacterial the effects such as.
Typically the extract of Radix Isatidis, Chloranthus glaber, peppermint is added in fiber respectively in the prior art, feature is prepared
Fiber, existing functional fiber has the following disadvantages:
(1)In fiber manufacturing process, isatis root extract, Herba Pileae Scriptae extract, the extract of peppermint soluble in water are caused
It is lost in, is also easy to be caused damage by soda acid destruction;
(2)It is usually that functional components and spinning solution are blended in the prior art, is then sprayed into coagulating bath and carries out spinning, because
The distribution of functional components in the fibre is random, that is to say, that a large amount of functional components can be distributed in the sandwich layer of fiber, point
Cloth fiber surface or cortex it is less;Because the extract of isatis root extract, Herba Pileae Scriptae extract, peppermint is contact
Anti-bacteria and anti-virus, so the functional components for being only distributed in fibrocortex or surface can just play effect, therefore feature into
Divide and be largely distributed in inside core fiber layer, cause a large amount of wastes, can also increase production cost;
(3)The functional components of fiber surface will also result in loss in washing and friction process, and then drop low-fiber antibacterial
Antiviral effect.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of Chloranthus glaber efficient antibacterial antiviral cellulose fibre and its preparation side
Method, to realize following goal of the invention:
(1)In fiber manufacturing process, isatis root extract, Herba Pileae Scriptae extract, the loss of the extract of peppermint or damage are reduced
Lose;
(2)Fiber prepared by the present invention, isatis root extract, Herba Pileae Scriptae extract, the extract profiles of peppermint are in fibrocortex
And surface portion, and outermost surface material has very strong adsorptivity;
(3)Fiber prepared by the present invention, is firmly combined with the functional components that graininess is embedded in fibrocortex or surface with fiber,
It is lost in washing and friction process few.
In order to realize foregoing invention purpose, the technical solution adopted by the present invention is:
A kind of Chloranthus glaber efficient antibacterial antiviral cellulose fibre, the fiber, chitosan-functional components compound particle contains
Measure as 9.5-9.7%, the content of silicic acid composite colloid is in 2-3.5%.
The following is the further improvement to above-mentioned technical proposal:
The chitosan-functional components compound particle, including chitosan, functional components, poly-quaternary ammonium salt;
The functional components, are isatis root extract, Herba Pileae Scriptae extract, the compound of the extract of peppermint;
The isatis root extract, Herba Pileae Scriptae extract, the mass ratio of the extract of peppermint are 3:1:2;The Radix Isatidis is carried
Thing, Herba Pileae Scriptae extract, the quality sum of the extract of peppermint are taken, the mass ratio with chitosan is 1:3;The poly-quaternary ammonium salt
Mass ratio with chitosan is 1:3.8-4.1.
A kind of preparation method of Chloranthus glaber efficient antibacterial antiviral cellulose fibre, including prepare chitosan-feature into
Divide compound particle, prepare silicic acid composite colloid, blending, spinning moulding.
It is described prepare chitosan-functional components compound particle, by isatis root extract, Herba Pileae Scriptae extract, peppermint
Extract is dissolved in pure water, obtains the functional components solution that mass concentration is 1.4-1.6mg/mL;Functional components are molten
During liquid adds mass concentration as 0.7-0.9mg/mL chitosan-acetic acid solution using 18-22mL/h speed, mixing speed is controlled
For 350-450r/min, poly-quaternary ammonium salt is added, filtering, deaeration after then stirring obtain the shell containing functional components and gathered
Sweet and sour acid solution;Then sprayed into 4-6ml/min speed in sodium hydroxide solution, granulation, the chitosan of 1-2 microns of generation-
Functional components compound particle.
The preparation method of the chitosan-acetic acid solution, chitosan is dissolved in 1% acetum, obtains mass concentration
It is 4 with 10% vinegar acid for adjusting pH for 0.7-0.9mg/mL chitosan-acetic acid solution.
The isatis root extract, Herba Pileae Scriptae extract, the mass ratio of the extract of peppermint are 3:1:2;
The isatis root extract, Herba Pileae Scriptae extract, the quality sum of the extract of peppermint, the mass ratio with chitosan is
1:3;
The mass ratio of the poly-quaternary ammonium salt and chitosan is 1:3.8-4.1.
It is described to prepare silicic acid composite colloid, by 5% sodium silicate aqueous solution and Sodium Hyaluronate, starch along succinate monoester
It is well mixed, crosslinking agent N, N ,-methylene-bisacrylamide, and polymerization initiator sodium peroxydisulfate are added, mixed material is obtained;It is mixed
Compound material is heated 8 hours at 48-52 DEG C in the reactor, is slowly warming up to 80 DEG C, controlling reaction temperature is 80 ± 2 DEG C, is filled with
Nitrogen pressurizes, and control reaction pressure reacts 2h in below 0.48-0.51MPa;DL-2000D PPGs are added, 95 are warming up to
± 2 DEG C, reaction pressure reacts 1h in below 0.48-0.51MPa, then adds in acid bath, and silicic acid composite colloid is made, and uniformly
Be scattered in acid bath.
The sodium metasilicate is 3 along the mass ratio of succinate monoester with Sodium Hyaluronate, starch:1:1;
N, the N, the quality of-methylene-bisacrylamide and the mass ratio of sodium metasilicate are:0.45-0.55:100;
The quality of the polymerization initiator sodium peroxydisulfate and the mass ratio of sodium metasilicate are 0.18-0.22:100;
The quality of the PPG and the mass ratio of sodium metasilicate are 0.9-1.1:100.
The blending, by obtained chitosan-functional components compound particle, is proportionally added into rayon spinning liquid, obtains
Co-blended spinning liquid;
The mass ratio of alpha cellulose is 0.10-0.105 in the chitosan-functional components compound particle, with viscose glue stoste:
1;
The viscose glue stoste, content of alphacellulose is 9.0-9.2%, and total alkali is 3.0-3.3%, viscosity 30-40s, maturation
Spend for 15-17ml (10% ammonium chloride value).
The spinning moulding, the silicic acid composite colloid containing 5-7%, shower nozzle drawing-off in acid bath:Drawing-off between -10~-6%, disk
18-22%, three bath 36-41%, four bath drawing-off 9-14%, spins speed 25-30m/min, leaching length:1000-1070 millimeters, in acid bath, sulfuric acid
Concentration 95-100g/l, sodium sulphate 350-360g/l, zinc sulfate 4-6g/l, acid temperature:43.5-45.5 degree Celsius, finished fiber is used
Sodium sulfite desulfurization, post-processes to obtain fibrous finished product.
The present invention is grown using specific shower nozzle drawing-off and leaching so that strand residence time in acid bath is long, increases chitosan
Ion and silicic acid composite colloid attracting time, reduce the loss of functional component;
The present invention is using the compound particle of specific chitosan-functional components, the specific silicic acid composite colloid of preparation and controls
Suitable concn, the spinning solution of silicic acid composite colloid relatively low viscosity, specific acid bath composition and spinning moulding bar in relieving haperacidity bath
Part so that compound particle, the silicic acid composite colloid of chitosan-functional components are just dispersed in the cortex and table of fiber
Face, and it is difficult for drop-off.
Specifically spinning moulding process is:In spinning moulding, when compound particle/viscose glue of chitosan-functional components
Spinning solution co-mixing system is sprayed into after coagulating bath from spinning head, and nascent strand is in viscous state, and internal chitosan feature is answered
Close particle by silicic acid composite colloid particle in acid bath to be attracted, transported from the sandwich layer of the viscous state of pre-profiling to the cortex of strand
Dynamic, silicic acid composite colloid is moved by the attraction of chitosan feature compound particle in strand to strand cortex in coagulating bath, with
Gradually forming and hardening of the strand in acid bath, chitosan feature compound particle is finally distributed in strand with silicic acid composite colloid
Skin portion and surface, strand goes out behind bath face, and relative motion thoroughly finishes, and chitosan feature compound particle is answered with silicic acid
Rubber alloy body is firmly coated on fibrocortex part, it is not easy to which dissolution comes off in the form of granules by after fiber solidifying.
The present invention using isatis root extract, Herba Pileae Scriptae extract, peppermint extract three it is compound as feature into
Point, with synergistic function, optimal antiviral and antibacterial effect can be reached.
By adopting the above-described technical solution, the present invention reach have the technical effect that:
(1)Chitosan-functional components compound particle in anti-bacteria and anti-virus fiber prepared by the present invention, fiber
Content be 9.5-9.7%, the content of silicic acid composite colloid is in 2-3.5%;Reduce loss and the chance of feature extract
Strong acid, caustic digestion.
(2)Anti-bacteria and anti-virus fiber prepared by the present invention, functional components are evenly distributed on fiber surface, and have very strong
Adsorption function, enables antiviral and antibacterial to play maximum performance;
And being firmly combined with for functional components and fiber, can avoid the active principle of fiber surface with washing or friction
It is lost in;Found through overtesting, after washing 50 times, chitosan-functional components compound particle loss late is only 0.7-1.1%.
(3)Anti-bacteria and anti-virus fiber prepared by the present invention, the dry fracture strength 2.80-2.85cN/dtex of fiber, wet fracture
Intensity is 1.78-1.82cN/dtex, and elongation at break is 22.7-23.4%, good hygroscopicity, and the regain of fiber is 15.5-
17.5%。
(4)In fiber of the present invention, Radix Isatidis, Chloranthus glaber and mint extract, chitosan, silicic acid composite colloid are combined,
Influenza A virus and influenza B virus can be effective against, to staphylococcus aureus, Candida albicans, typhoid bacillus
There is higher inhibiting rate, be 99.5%-99.8% to staphylococcus aureus bacteriostasis rate, be to the bacteriostasis rate of Candida albicans
97.2-97.8%, it is 98.2%-98.7% to typhoid bacillus bacteriostasis rate, to influenza A virus, influenza B virus using red thin
Born of the same parents' agglutination detects that potency reaches 8-9.
Embodiment
With reference to embodiment, the present invention is described in detail.Following examples will be helpful to those skilled in the art
The present invention is further understood, but the invention is not limited in any way.It should be pointed out that to one of ordinary skill in the art
For, without departing from the inventive concept of the premise, it can also make certain adjustments and improvements.These belong to the guarantor of the present invention
Protect scope.
A kind of preparation method of Chloranthus glaber efficient antibacterial antiviral cellulose fibre of embodiment 1
Comprise the following steps:
(1)Prepare chitosan-functional components compound particle
Chitosan is dissolved in 1% acetum, the chitosan-acetic acid solution that mass concentration is 0.8mg/mL is obtained, with 10%
Vinegar acid for adjusting pH is 4;
The extract of isatis root extract, Herba Pileae Scriptae extract, peppermint is dissolved in pure water, mass concentration is obtained for 1.5mg/
ML functional components solution;
Functional components solution is added in chitosan-acetic acid solution with 20mL/h speed, it is 400r/ to control mixing speed
Min, adds poly-quaternary ammonium salt, and filtering, deaeration, obtain the chitosan-acetic acid solution containing functional components after then stirring;
Then sprayed into 5ml/min speed in sodium hydroxide solution, granulation, chitosan-functional components of 1-2 microns of generation
Compound particle;
The isatis root extract, Herba Pileae Scriptae extract, the mass ratio of the extract of peppermint are 3:1:2;
The isatis root extract, Herba Pileae Scriptae extract, the quality sum of the extract of peppermint, the mass ratio with chitosan is
1:3。
The mass ratio of the poly-quaternary ammonium salt and chitosan is 1:4.
(2)Prepare silicic acid composite colloid
5% sodium silicate aqueous solution is well mixed with Sodium Hyaluronate, starch along succinate monoester, crosslinking agent N, N is added ,-sub-
Bisacrylamide, and polymerization initiator sodium peroxydisulfate, obtain mixed material;
Mixed material is heated 8 hours at 50 DEG C in the reactor, is slowly warming up to 80 DEG C, controlling reaction temperature is 80 ± 2 DEG C, is filled
Enter nitrogen pressurization, control reaction pressure reacts 2h in below 0.5MPa;DL-2000D PPGs are added, 95 ± 2 are warming up to
DEG C, reaction pressure reacts 1h in 0. below 5MPa, then adds in acid bath, silicic acid composite colloid is made, and be uniformly scattered in
In acid bath.
The sodium metasilicate is 3 along the mass ratio of succinate monoester with Sodium Hyaluronate, starch:1:1;
N, the N, the quality of-methylene-bisacrylamide and the mass ratio of sodium metasilicate are:0.5:100;
The quality of the polymerization initiator sodium peroxydisulfate and the mass ratio of sodium metasilicate are 0.2:100;
The quality of the PPG and the mass ratio of sodium metasilicate are 1:100.
(3)Blending
By step(1)Obtained chitosan-functional components compound particle, is proportionally added into blended, mistake in rayon spinning liquid
After filter, deaeration, maturation, co-blended spinning liquid is obtained.
The mass ratio of alpha cellulose is 0.10 in the chitosan-functional components compound particle, with viscose glue stoste:1;
The viscose glue stoste, content of alphacellulose is 9.0-9.2%, and total alkali is 3.0-3.3%, viscosity 30s, and degree of ripeness is
15-17ml (10% ammonium chloride value).
(4)Spinning moulding
Co-blended spinning liquid is added in the acid bath adjusted and carries out spinning, containing 5% silicic acid composite colloid in acid bath, shower nozzle is led
Stretch:- 10%, speed 25m/min, leaching length are spun in drawing-off 18% between disk, three baths 36%, four bath drawing-offs 9%:1000 millimeters, in acid bath, sulfuric acid
Concentration 95g/l, sodium sulphate 350g/l, zinc sulfate 4g/l, acid temperature:43.5 degrees Celsius, finished fiber uses sodium sulfite desulfurization, after
Handle to obtain fibrous finished product.
The present invention is grown using specific shower nozzle drawing-off and leaching so that strand residence time in acid bath is long, increases chitosan
Ion and silicic acid composite colloid attracting time, reduce the loss of functional component;
The present invention is using the compound particle of specific chitosan-functional components, the specific silicic acid composite colloid of preparation and controls
Suitable concn, the spinning solution of silicic acid composite colloid relatively low viscosity, specific acid bath composition and spinning moulding bar in relieving haperacidity bath
Part so that compound particle, the silicic acid composite colloid of chitosan-functional components are just dispersed in the cortex and table of fiber
Face, and it is difficult for drop-off.
Specifically spinning moulding process is:In spinning moulding, when compound particle/viscose glue of chitosan-functional components
Spinning solution co-mixing system is sprayed into after coagulating bath from spinning head, and nascent strand is in viscous state, and internal chitosan feature is answered
Close particle by silicic acid composite colloid particle in acid bath to be attracted, transported from the sandwich layer of the viscous state of pre-profiling to the cortex of strand
Dynamic, silicic acid composite colloid is moved by the attraction of chitosan feature compound particle in strand to strand cortex in coagulating bath, with
Gradually forming and hardening of the strand in acid bath, chitosan feature compound particle is finally distributed in strand with silicic acid composite colloid
Skin portion and surface, strand goes out behind bath face, and relative motion thoroughly finishes, and chitosan feature compound particle is answered with silicic acid
Rubber alloy body is firmly coated on fibrocortex part, it is not easy to which dissolution comes off in the form of granules by after fiber solidifying.
(1)Chitosan-functional components compound particle in anti-bacteria and anti-virus fiber prepared by the embodiment of the present invention 1, fiber
Content be 9.5%, the content of silicic acid composite colloid is 2%;Reduce the loss of feature extract and meet strong acid, caustic digestion.
(2)Anti-bacteria and anti-virus fiber prepared by the embodiment of the present invention 1, functional components are evenly distributed on fiber surface, resist
Virus and antibacterial can play maximum performance;
And being firmly combined with for functional components and fiber, can avoid the active principle of fiber surface with washing or friction
It is lost in;Found through overtesting, after washing 50 times, chitosan-functional components compound particle loss late is only 0.7%.
(3)Anti-bacteria and anti-virus fiber prepared by the embodiment of the present invention 1, the dry fracture strength 2.80cN/dtex of fiber is wet disconnected
Resistance to spalling is 1.78cN/dtex, and elongation at break is 22.7%, good hygroscopicity, and the regain of fiber is 15.5%.
(4)In fiber prepared by the embodiment of the present invention 1, Radix Isatidis, Chloranthus glaber and mint extract, chitosan, silicic acid are multiple
Rubber alloy body phase is combined, and influenza A virus and influenza B virus can be effective against, to staphylococcus aureus, Candida albicans
Bacterium, typhoid bacillus also have higher inhibiting rate, are 99.5% to staphylococcus aureus bacteriostasis rate, to the antibacterial of Candida albicans
Rate is 97.2%, is 98.2% to typhoid bacillus bacteriostasis rate, and erythrocyte agglutination method is used to influenza A virus, influenza B virus
Detection, potency reaches 8.
A kind of preparation method of Chloranthus glaber efficient antibacterial antiviral cellulose fibre of embodiment 2
Comprise the following steps:
(1)Prepare chitosan-functional components compound particle
Chitosan is dissolved in 1% acetum, the chitosan-acetic acid solution that mass concentration is 0.8mg/mL is obtained, with 10%
Vinegar acid for adjusting pH is 4;
The extract of isatis root extract, Herba Pileae Scriptae extract, peppermint is dissolved in pure water, mass concentration is obtained for 1.5mg/
ML functional components solution;
Functional components solution is added in chitosan-acetic acid solution with 20mL/h speed, it is 400r/ to control mixing speed
Min, adds poly-quaternary ammonium salt, and filtering, deaeration, obtain the chitosan-acetic acid solution containing functional components after then stirring;
Then sprayed into 5ml/min speed in sodium hydroxide solution, granulation, chitosan-functional components of 1-2 microns of generation
Compound particle;
The isatis root extract, Herba Pileae Scriptae extract, the mass ratio of the extract of peppermint are 3:1:2;
The isatis root extract, Herba Pileae Scriptae extract, the quality sum of the extract of peppermint, the mass ratio with chitosan is
1:3。
The mass ratio of the poly-quaternary ammonium salt and chitosan is 1:4.
(2)Prepare silicic acid composite colloid
5% sodium silicate aqueous solution is well mixed with Sodium Hyaluronate, starch along succinate monoester, crosslinking agent N, N is added ,-sub-
Bisacrylamide, and polymerization initiator sodium peroxydisulfate, obtain mixed material;
Mixed material is heated 8 hours at 50 DEG C in the reactor, is slowly warming up to 80 DEG C, controlling reaction temperature is 80 ± 2 DEG C, is filled
Enter nitrogen pressurization, control reaction pressure reacts 2h in below 0.5MPa;DL-2000D PPGs are added, 95 ± 2 are warming up to
DEG C, reaction pressure reacts 1h in 0. below 5MPa, then adds in acid bath, silicic acid composite colloid is made, and be uniformly scattered in
In acid bath.
The sodium metasilicate is 3 along the mass ratio of succinate monoester with Sodium Hyaluronate, starch:1:1;
N, the N, the quality of-methylene-bisacrylamide and the mass ratio of sodium metasilicate are:0.5:100;
The quality of the polymerization initiator sodium peroxydisulfate and the mass ratio of sodium metasilicate are 0.2:100;
The quality of the PPG and the mass ratio of sodium metasilicate are 1:100.
(3)Blending
By step(1)Obtained chitosan-functional components compound particle, is proportionally added into blended, mistake in rayon spinning liquid
After filter, deaeration, maturation, co-blended spinning liquid is obtained.
The mass ratio of alpha cellulose is 0.105 in the chitosan-functional components compound particle, with viscose glue stoste:
1;
The viscose glue stoste, content of alphacellulose is 9.0-9.2%, and total alkali is 3.0-3.3%, viscosity 40s, and degree of ripeness is
15-17ml (10% ammonium chloride value).
(4)Spinning moulding
Co-blended spinning liquid is added in the acid bath adjusted and carries out spinning, containing 7% silicic acid composite colloid in acid bath, shower nozzle is led
Stretch:- 6%, speed 30m/min, leaching length are spun in drawing-off 22% between disk, three baths 41%, four bath drawing-offs 14%:1070 millimeters, in acid bath, sulphur
Acid concentration 100g/l, sodium sulphate 360g/l, zinc sulfate 6g/l, acid temperature:45.5 degrees Celsius, finished fiber is de- using sodium sulfite
Sulphur, post-processes to obtain fibrous finished product.
The present invention is grown using specific shower nozzle drawing-off and leaching so that strand residence time in acid bath is long, increases chitosan
Ion and silicic acid composite colloid attracting time, reduce the loss of functional component;
The present invention is using the compound particle of specific chitosan-functional components, the specific silicic acid composite colloid of preparation and controls
Suitable concn, the spinning solution of silicic acid composite colloid relatively low viscosity, specific acid bath composition and spinning moulding bar in relieving haperacidity bath
Part so that compound particle, the silicic acid composite colloid of chitosan-functional components are just dispersed in the cortex and table of fiber
Face, and it is difficult for drop-off.
Specifically spinning moulding process is:In spinning moulding, when compound particle/viscose glue of chitosan-functional components
Spinning solution co-mixing system is sprayed into after coagulating bath from spinning head, and nascent strand is in viscous state, and internal chitosan feature is answered
Close particle by silicic acid composite colloid particle in acid bath to be attracted, transported from the sandwich layer of the viscous state of pre-profiling to the cortex of strand
Dynamic, silicic acid composite colloid is moved by the attraction of chitosan feature compound particle in strand to strand cortex in coagulating bath, with
Gradually forming and hardening of the strand in acid bath, chitosan feature compound particle is finally distributed in strand with silicic acid composite colloid
Skin portion and surface, strand goes out behind bath face, and relative motion thoroughly finishes, and chitosan feature compound particle is answered with silicic acid
Rubber alloy body is firmly coated on fibrocortex part, it is not easy to which dissolution comes off in the form of granules by after fiber solidifying.
(1)Chitosan-functional components compound particle in anti-bacteria and anti-virus fiber prepared by the embodiment of the present invention 2, fiber
Content be 9.7%, the content of silicic acid composite colloid is 3.5%;Reduce the loss of feature extract and meet strong acid, alkali point
Solution.
(2)Anti-bacteria and anti-virus fiber prepared by the embodiment of the present invention 2, functional components are evenly distributed on fiber surface, resist
Virus and antibacterial can play maximum performance;And being firmly combined with for functional components and fiber, can avoid fiber table
The active principle in face is lost in washing or friction;Found through overtesting, after washing 50 times, chitosan-functional components are multiple
It is only 1.1% to close particle loss rate.
(3)Anti-bacteria and anti-virus fiber prepared by the embodiment of the present invention 2, the dry fracture strength 2.85cN/dtex of fiber is wet disconnected
Resistance to spalling is 1.82cN/dtex, and elongation at break is 23.4%, good hygroscopicity, and the regain of fiber is 17.5%.
(4)In fiber prepared by the embodiment of the present invention 2, Radix Isatidis, Chloranthus glaber and mint extract, chitosan, silicic acid are multiple
Rubber alloy body phase is combined, and influenza A virus and influenza B virus can be effective against, to staphylococcus aureus, Candida albicans
Bacterium, typhoid bacillus also have higher inhibiting rate, are 99.8% to staphylococcus aureus bacteriostasis rate, to the antibacterial of Candida albicans
Rate is 97.8%, is 98.7% to typhoid bacillus bacteriostasis rate, and erythrocyte agglutination method is used to influenza A virus, influenza B virus
Detection, potency reaches 9.
Unless otherwise indicated, the percentage employed in the present invention is percetage by weight, ratio of the present invention,
For mass 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 (10)
1. a kind of Chloranthus glaber efficient antibacterial antiviral cellulose fibre, it is characterised in that:The fiber, chitosan-feature into
The content for dividing compound particle is 9.5-9.7%, and the content of silicic acid composite colloid is in 2-3.5%.
2. a kind of Chloranthus glaber efficient antibacterial antiviral cellulose fibre according to claim 1, it is characterised in that:The shell
Glycan-functional components compound particle, including chitosan, functional components, poly-quaternary ammonium salt;
The functional components, are isatis root extract, Herba Pileae Scriptae extract, the compound of the extract of peppermint;
The isatis root extract, Herba Pileae Scriptae extract, the mass ratio of the extract of peppermint are 3:1:2;The Radix Isatidis is carried
Thing, Herba Pileae Scriptae extract, the quality sum of the extract of peppermint are taken, the mass ratio with chitosan is 1:3;The poly-quaternary ammonium salt
Mass ratio with chitosan is 1:3.8-4.1.
3. a kind of preparation method of Chloranthus glaber efficient antibacterial antiviral cellulose fibre, it is characterised in that:Including prepare chitosan-
Functional components compound particle, prepare silicic acid composite colloid, blending, spinning moulding.
4. a kind of preparation method of Chloranthus glaber efficient antibacterial antiviral cellulose fibre according to claim 3, its feature
It is:The spinning moulding, the silicic acid composite colloid containing 5-7%, shower nozzle drawing-off in acid bath:Drawing-off 18- between -10~-6%, disk
22%, three bath 36-41%, four bath drawing-off 9-14%, spin speed 25-30m/min, leaching length:1000-1070 millimeters, in acid bath, sulfuric acid is dense
Spend 95-100g/l, sodium sulphate 350-360g/l, zinc sulfate 4-6g/l, acid temperature:43.5-45.5 degree Celsius, finished fiber is using sub-
Sodium sulphate desulfurization, post-processes to obtain fibrous finished product.
5. a kind of preparation method of Chloranthus glaber efficient antibacterial antiviral cellulose fibre according to claim 3, its feature
It is:It is described to prepare chitosan-functional components compound particle, by isatis root extract, Herba Pileae Scriptae extract, peppermint extraction
Thing is dissolved in pure water, obtains the functional components solution that mass concentration is 1.4-1.6mg/mL;By functional components solution with
18-22mL/h speed adds mass concentration in 0.7-0.9mg/mL chitosan-acetic acid solution, to control the mixing speed to be
350-450r/min, adds poly-quaternary ammonium salt, and filtering, deaeration, obtain the chitosan containing functional components after then stirring
Acetum;Then sprayed into 4-6ml/min speed in sodium hydroxide solution, granulation, chitosan-work(of 1-2 microns of generation
Can property composition compound particle.
6. a kind of preparation method of Chloranthus glaber efficient antibacterial antiviral cellulose fibre according to claim 5, its feature
It is:The preparation method of the chitosan-acetic acid solution, chitosan is dissolved in 1% acetum, is obtained mass concentration and is
0.7-0.9mg/mL chitosan-acetic acid solution, is 4 with 10% vinegar acid for adjusting pH.
7. a kind of preparation method of Chloranthus glaber efficient antibacterial antiviral cellulose fibre according to claim 5, its feature
It is:
The isatis root extract, Herba Pileae Scriptae extract, the mass ratio of the extract of peppermint are 3:1:2;
The isatis root extract, Herba Pileae Scriptae extract, the quality sum of the extract of peppermint, the mass ratio with chitosan is
1:3;
The mass ratio of the poly-quaternary ammonium salt and chitosan is 1:3.8-4.1.
8. a kind of preparation method of Chloranthus glaber efficient antibacterial antiviral cellulose fibre according to claim 3, its feature
It is:It is described to prepare silicic acid composite colloid, 5% sodium silicate aqueous solution is mixed with Sodium Hyaluronate, starch along succinate monoester
Uniformly, crosslinking agent N, N ,-methylene-bisacrylamide, and polymerization initiator sodium peroxydisulfate are added, mixed material is obtained;Mixture
Material is heated 8 hours at 48-52 DEG C in the reactor, is slowly warming up to 80 DEG C, controlling reaction temperature is 80 ± 2 DEG C, is filled with nitrogen
Pressurization, control reaction pressure reacts 2h in below 0.48-0.51MPa;DL-2000D PPGs are added, 95 ± 2 are warming up to
DEG C, reaction pressure reacts 1h in below 0.48-0.51MPa, then adds in acid bath, and silicic acid composite colloid is made, and uniformly
It is scattered in acid bath.
9. a kind of preparation method of Chloranthus glaber efficient antibacterial antiviral cellulose fibre according to claim 8, its feature
It is:
The sodium metasilicate is 3 along the mass ratio of succinate monoester with Sodium Hyaluronate, starch:1:1;
N, the N, the quality of-methylene-bisacrylamide and the mass ratio of sodium metasilicate are:0.45-0.55:100;
The quality of the polymerization initiator sodium peroxydisulfate and the mass ratio of sodium metasilicate are 0.18-0.22:100;
The quality of the PPG and the mass ratio of sodium metasilicate are 0.9-1.1:100.
10. a kind of preparation method of Chloranthus glaber efficient antibacterial antiviral cellulose fibre according to claim 3, its feature
It is:The blending, by obtained chitosan-functional components compound particle, is proportionally added into rayon spinning liquid, is blended
Spinning solution;
The mass ratio of alpha cellulose is 0.10-0.105 in the chitosan-functional components compound particle, with viscose glue stoste:
1;
The viscose glue stoste, content of alphacellulose is 9.0-9.2%, and total alkali is 3.0-3.3%, viscosity 30-40s, maturation
Spend for 15-17ml (10% ammonium chloride value).
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Also Published As
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CN108716028B (en) | 2020-11-20 |
CN106995943B (en) | 2018-08-07 |
CN108624975A (en) | 2018-10-09 |
CN108754654A (en) | 2018-11-06 |
CN108624975B (en) | 2020-05-12 |
CN108754654B (en) | 2020-09-08 |
CN108716028A (en) | 2018-10-30 |
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