CN106929931A - A kind of viscose rayon containing isatis root extract and preparation method thereof - Google Patents
A kind of viscose rayon containing isatis root extract and preparation method thereof Download PDFInfo
- Publication number
- CN106929931A CN106929931A CN201710183744.5A CN201710183744A CN106929931A CN 106929931 A CN106929931 A CN 106929931A CN 201710183744 A CN201710183744 A CN 201710183744A CN 106929931 A CN106929931 A CN 106929931A
- Authority
- CN
- China
- Prior art keywords
- radix isatidis
- microcapsules
- preparation
- viscose rayon
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229920000297 Rayon Polymers 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 55
- 241000334160 Isatis Species 0.000 title claims abstract description 33
- 239000000284 extract Substances 0.000 title claims abstract description 33
- 238000000605 extraction Methods 0.000 title description 2
- 239000010231 banlangen Substances 0.000 claims abstract description 138
- 239000003094 microcapsule Substances 0.000 claims abstract description 108
- 239000000835 fiber Substances 0.000 claims abstract description 70
- 239000002253 acid Substances 0.000 claims description 47
- 238000009987 spinning Methods 0.000 claims description 47
- 238000003756 stirring Methods 0.000 claims description 40
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 39
- 239000000463 material Substances 0.000 claims description 31
- 239000000839 emulsion Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 229920000877 Melamine resin Polymers 0.000 claims description 24
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 23
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 23
- 206010011732 Cyst Diseases 0.000 claims description 22
- 208000031513 cyst Diseases 0.000 claims description 22
- 229920000642 polymer Polymers 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 20
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 17
- 239000003607 modifier Substances 0.000 claims description 17
- 238000013329 compounding Methods 0.000 claims description 16
- 239000004640 Melamine resin Substances 0.000 claims description 15
- 229920002472 Starch Polymers 0.000 claims description 15
- 239000008107 starch Substances 0.000 claims description 15
- 235000019698 starch Nutrition 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 238000000465 moulding Methods 0.000 claims description 14
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 14
- 239000003292 glue Substances 0.000 claims description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 229920002907 Guar gum Polymers 0.000 claims description 12
- 239000000665 guar gum Substances 0.000 claims description 12
- 229960002154 guar gum Drugs 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000002386 leaching Methods 0.000 claims description 11
- 235000010417 guar gum Nutrition 0.000 claims description 10
- -1 tertiary amino alkyl ether Chemical group 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
- 239000002994 raw material Substances 0.000 claims description 9
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 claims description 7
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 7
- 235000011152 sodium sulphate Nutrition 0.000 claims description 7
- 229920002678 cellulose Polymers 0.000 claims description 6
- 239000001913 cellulose Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000002775 capsule Substances 0.000 claims description 5
- 150000002170 ethers Chemical class 0.000 claims description 5
- 239000002608 ionic liquid Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- SFVFIFLLYFPGHH-UHFFFAOYSA-M stearalkonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 SFVFIFLLYFPGHH-UHFFFAOYSA-M 0.000 claims description 5
- WQSRXNAKUYIVET-UHFFFAOYSA-N sulfuric acid;zinc Chemical compound [Zn].OS(O)(=O)=O WQSRXNAKUYIVET-UHFFFAOYSA-N 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
- 239000012752 auxiliary agent Substances 0.000 claims description 4
- 230000033228 biological regulation Effects 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 241000196324 Embryophyta Species 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 210000000481 breast Anatomy 0.000 claims 1
- 239000013049 sediment Substances 0.000 claims 1
- 238000001694 spray drying Methods 0.000 claims 1
- 230000001112 coagulating effect Effects 0.000 abstract description 22
- 241000193830 Bacillus <bacterium> Species 0.000 abstract description 6
- 241000222122 Candida albicans Species 0.000 abstract description 6
- 241000712431 Influenza A virus Species 0.000 abstract description 6
- 241000713196 Influenza B virus Species 0.000 abstract description 6
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 6
- 208000037386 Typhoid Diseases 0.000 abstract description 6
- 229940095731 candida albicans Drugs 0.000 abstract description 6
- 201000008297 typhoid fever Diseases 0.000 abstract description 6
- 230000002147 killing effect Effects 0.000 abstract description 3
- 230000001629 suppression Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 60
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 22
- 229940068984 polyvinyl alcohol Drugs 0.000 description 22
- 239000010935 stainless steel Substances 0.000 description 15
- 229910001220 stainless steel Inorganic materials 0.000 description 15
- 238000005406 washing Methods 0.000 description 13
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 239000012153 distilled water Substances 0.000 description 9
- 239000003995 emulsifying agent Substances 0.000 description 9
- 239000003999 initiator Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- 229920001661 Chitosan Polymers 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- 230000002829 reductive effect Effects 0.000 description 6
- 238000007493 shaping process Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 230000000840 anti-viral effect Effects 0.000 description 4
- OOSUHIIJYDMCCW-UHFFFAOYSA-N cyanamide;formaldehyde Chemical compound O=C.NC#N OOSUHIIJYDMCCW-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000006870 function Effects 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- 238000005829 trimerization reaction Methods 0.000 description 4
- 239000004342 Benzoyl peroxide Substances 0.000 description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 3
- 229920001213 Polysorbate 20 Polymers 0.000 description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 3
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 3
- 239000002964 rayon Substances 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 230000036039 immunity Effects 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000000116 mitigating effect Effects 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000004901 spalling Methods 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011782 vitamin Substances 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 229930003231 vitamin Natural products 0.000 description 2
- 235000013343 vitamin Nutrition 0.000 description 2
- 150000003722 vitamin derivatives Chemical class 0.000 description 2
- ZXLOSLWIGFGPIU-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;acetate Chemical compound CC(O)=O.CCN1CN(C)C=C1 ZXLOSLWIGFGPIU-UHFFFAOYSA-N 0.000 description 1
- HPAVSHLOCSRBQS-UHFFFAOYSA-N CCCCCCCCCCCCCCCCCCCl(C)(C)CC1=CC=CC=C1 Chemical compound CCCCCCCCCCCCCCCCCCCl(C)(C)CC1=CC=CC=C1 HPAVSHLOCSRBQS-UHFFFAOYSA-N 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- 229920000433 Lyocell Polymers 0.000 description 1
- 239000004425 Makrolon Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- QDYLMAYUEZBUFO-UHFFFAOYSA-N cetalkonium chloride Chemical compound CCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 QDYLMAYUEZBUFO-UHFFFAOYSA-N 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 210000003743 erythrocyte Anatomy 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- 230000036737 immune function Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012778 molding material Substances 0.000 description 1
- SBNFWQZLDJGRLK-UHFFFAOYSA-N phenothrin Chemical compound CC1(C)C(C=C(C)C)C1C(=O)OCC1=CC=CC(OC=2C=CC=CC=2)=C1 SBNFWQZLDJGRLK-UHFFFAOYSA-N 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 230000007306 turnover Effects 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08G12/30—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with substituted triazines
- C08G12/32—Melamines
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention provides a kind of viscose rayon containing isatis root extract, the viscose rayon, the content of Radix Isatidis microcapsules is 9.1 9.79%, the dry fracture strength of fiber is 2.70 2.75cN/dtex, wet breaking strength is 1.70 1.75cN/dtex, elongation at break is 22 23%, to staphylococcus aureus bacteriostasis rate 99.0% 99.8%, it is 96.6 98.8% to the bacteriostasis rate of Candida albicans, is 97.2% 99.1% to typhoid bacillus bacteriostasis rate, there is very strong suppression killing action to influenza A virus, influenza B virus；The present invention also provides a kind of preparation method of the viscose rayon containing isatis root extract, including Radix Isatidis microcapsules is modified；The present invention reduces the loss of Radix Isatidis microcapsules in fiber manufacturing process, reduces the backwash rate of pulling away a prop of coagulating bath filter；Improve the uniformity that Radix Isatidis microcapsules are distributed in the fibre.
Description
Technical field
It is particularly a kind of containing the viscose rayon of isatis root extract and its preparation side the present invention relates to a kind of viscose rayon
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, advantage is created 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；Will
Isatis root extract is added in viscose rayon, prepares the textile with healthcare functions such as antiviral, enhance immunities, symbol
Close the popular demand to the product with health care function of present society.
Chinese patent CN105381766A（Publication number）, disclose a kind of isatis root extract vitamin protein and be combined
The preparation method and applications of microcapsules, it first prepares isatis root extract vitamin protein composite micro-capsule, then will be multiple
Close microcapsules to be added in viscose glue stoste, prepare co-blended spinning liquid, spinning is carried out by the coagulating bath adjusted；By microcapsules
Change and crosslinking curing, prepare with antiviral and functions of skin protection and health care viscose rayon.
Chinese patent CN106192045A (publication number), discloses a kind of Radix Isatidis cellulose fibre and preparation method thereof,
Radix Isatidis is first made microcapsules by it, is then blended with spinning solution, and fiber, the Radix Isatidis cellulose of preparation are prepared by spinning
Fiber, the active ingredient sustained release phase is long, with good antibacterial, clearing heat and cooling blood, antiviral, enhance immunity effect.
There is following defect in above-mentioned patent：
（1）During fiber is prepared, if not using microcapsule coated, then isatis root extract is highly soluble in water,
One side Radix Isatidis active principle is easily destroyed by soda acid, on the other hand because fairly soluble reason major part will be lost in.
（2）If using microcapsule coated, Radix Isatidis microcapsules are also easily lost in.
Specifically the process of loss is：In rayon spinning stoste, between 8.2-9.2%, 90% or so is first fibre content in addition
The materials such as water, soluble-salt, wherein only first fibre can in spinning process coagulation forming, formed fiber.
In spinning process, when rayon spinning stoste and the blend solution of Radix Isatidis microcapsules, a flash of coagulating bath is sprayed into
Between, first fibre start shaping, then coat residence addition microcapsules, but in rayon spinning stoste can curing molding material,
Be exactly the fine content of first less than 10%, the microcapsules that first fibre can be coated in forming process are few, there is substantial amounts of microcapsules
Can with spinning viscose stoste the material such as 90% water, soluble-salt lost, cause a large amount of losses of Radix Isatidis microcapsules.
In actual experiment find, when microcapsules solid dry powder to first fibre addition 10% when, microcapsules in finished fiber
Content also less than 5%, substantial amounts of microencapsulation material enters coagulating bath after being lost in, and increased coagulating bath filter backwash rate of pulling away a prop and reaches
75%。
（3）Because Radix Isatidis is easily lost in, during fiber is prepared, the Radix Isatidis composition of fiber surface compares fibrous inside
Be easier be lost in so that in the fiber of finished product, the Radix Isatidis on surface is less, and more relatively more toward fibrous inside.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of containing the viscose rayon of isatis root extract and its preparation side
Method, to realize following goal of the invention：
（1）The loss of Radix Isatidis microcapsules in fiber manufacturing process is reduced, the backwash rate of pulling away a prop of coagulating bath filter is reduced；
（2）Improve the uniformity that Radix Isatidis microcapsules are distributed in the fibre.
In order to realize foregoing invention purpose, the technical solution adopted by the present invention is：
A kind of viscose rayon containing isatis root extract, the viscose rayon, the content of Radix Isatidis microcapsules is 9.1-9.79%,
The dry fracture strength of fiber is 2.70-2.75cN/dtex, and wet breaking strength is 1.70-1.75cN/dtex, and elongation at break is
22-23%.It is 96.6-98.8%, typhoid fever to Candida albicans bacteriostasis rate to staphylococcus aureus bacteriostasis rate 99.0%-99.8%
Bacillus bacteriostasis rate is 97.2%-99.1%, there is very strong suppression killing action to influenza A virus, influenza B virus；
The following is the further improvement to above-mentioned technical proposal：
A kind of preparation method of the viscose rayon containing isatis root extract, the preparation method, including Radix Isatidis microcapsules change
Property；Radix Isatidis microcapsules are modified by being modified for the Radix Isatidis microcapsules using modifier solution；The modifying agent is molten
Liquid, in parts by weight, including 3 parts of guar gum, 5 parts of shitosan, 1 part of polyvinyl alcohol, 30 parts of pure water, 100 parts of acetic acid.
The preparation method, including spinning moulding；The spinning moulding is carried out in acid bath, and 3-5% is added in the acid bath
Acid bath compounding agent solution；The acid bath compounding agent solution, in parts by weight, including following raw material components：Starch tertiary amino alkyl ether 6
Part, 5 parts of quaternary ammonium starch ethers, 10 parts of poly-quaternary ammonium salt, 3 parts of stearyl dimethyl benzyl ammonium chloride, chlorination dodecyl dimethyl
4 parts of hexadecyldimethyl benzyl ammonium, 100 parts of pure water.
The poly-quaternary ammonium salt is poly-quaternary ammonium salt 10；
The preparation of the modifier solution, comprises the following steps：
The preparation of A, poly-vinyl alcohol solution
According to the formula of modifying agent, each raw material components are weighed, pure water is put into agitator tank, start stirring, speed of agitator is
1200-1300r/min, while adding polyvinyl alcohol chip solid, temperature is warmed up to 95 from 25 DEG C with 5 DEG C per minute of speed
DEG C, 30min is incubated, until polyvinyl alcohol is completely dissolved, stirring is started always, prevent crystallization from separating out, poly-vinyl alcohol solution is obtained
Preparation.
The preparation of B, chitosan solution
Shitosan and acetic acid are mixed, dissolving, preparation obtains 5% shitosan acetic acid solution.
C, mixing
Chitosan solution prepared by step B, is placed in stand-by in stainless steel；
In the poly-vinyl alcohol solution for adding step A to prepare guar gum, after the stirring and dissolving of 800-900r/min, poly- second is prepared
The mixed liquor of enol and guar gum, is slowly dropped in the stainless steel containing shitosan acetic acid solution, and rate of addition is 0.5-
0.7 part/min, it is 40-45 DEG C to control the temperature of stainless steel, and speed of agitator is 900-1000r/min, completion of dropping, insulation
10-15 minutes, modifier solution is obtained.
The preparation method of the acid bath compounding agent solution, mixing adds pure water in filling, and starts stirring, and rotating speed is 500-
550r/min, is subsequently adding starch tertiary amino alkyl ether, the mixture of quaternary ammonium starch ethers, and charging rate is 1-1.5 parts/min, plus
Material is finished, and temperature is warmed up to 95 DEG C from 25 DEG C with 5 DEG C per minute of speed, is incubated 15 minutes, then cools to 60-65 DEG C, addition
Poly-quaternary ammonium salt, stearyl dimethyl benzyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride, stir, and cool to 25
DEG C, filtrate is filtered to take, obtain acid bath compounding agent solution.
The acid bath, sulfuric acid concentration 130-137g/l, sodium sulfate concentration 130-150g/l, sulfuric acid zinc concentration 4-6g/l, acid
The temperature of bath：50-53℃.
The spinning moulding, leaching length：420-480 millimeters, shower nozzle drawing-off：75-85%；Drawing-off 16-21% between disk, three baths are led
- 2~8%, four bath drawing-off 5-11% are stretched, speed 27-32m/min is spun.
The leaching length is preferably：450-470 millimeters, shower nozzle drawing-off is preferably：77-83%；Acid bath temperature is preferably 50-52
℃；More preferably leaching is grown：460 millimeters, shower nozzle drawing-off：77%；The temperature of acid bath：50℃.
The specific leaching length and shower nozzle drawing-off that the present invention is used can be improved and lead a linear velocity so that strand is stopped in acid bath
Time is short；Reduce the loss of Radix Isatidis microcapsules；
With reference to specific sulfuric acid, the concentration of sodium sulphate, and acid bath temperature higher, the deficiency of shaping can be made up, it is ensured that plate
The uniformity that blue root microcapsules are distributed in the fibre；
Further coordinate drawing-off, three bath drawing-offs, four bath drawing-offs, spinning speed between specific disk, while effect can be stated in realization,
Influence of the addition of Radix Isatidis to fibre machinery performance is reduced, keeps the fiber for preparing that there is preferable mechanical performance.
When the co-blended spinning liquid of spinning solution and modified Radix Isatidis microcapsule emulsion is injected to coagulating bath, first fibre starts
Forming and hardening.
Acid bath auxiliary agent of the present invention is dispersed in coagulating bath, and during spinning moulding, coagulating bath is uniformly repelled altogether
Modified Radix Isatidis microcapsules in blended ratio liquid, make the inside or surface of its cellulose for being firmly attached to firm shaping,
And be uniformly distributed.
The preparation method, also including preparing Radix Isatidis microcapsules；It is described to prepare Radix Isatidis microcapsules, including prepare trimerization
Cyanamide formaldehyde resin cyst material performed polymer；It is described to prepare melamine resin cyst material performed polymer, by 37% formaldehyde
Solution is put into reactor, and stirring, regulation pH value is 7.8-8.0, by 37% formalin：Melamine is 4:1 ratio adds
Enter melamine, be warming up to 65-70 DEG C, with 800-900r/min stirring reactions 0.8-1.2 hours under constant temperature, be made trimerization
Cyanamide formaldehyde resin cyst material performed polymer.
Find in actual applications, above-mentioned melamine resin cyst material performed polymer so that Radix Isatidis microcapsules
Combination with fiber is more firm, and the Radix Isatidis active principle of fiber surface can be avoided to be lost in washing or friction.
It is described to prepare Radix Isatidis microcapsules, also including preparing Radix Isatidis emulsion；It is described to prepare Radix Isatidis emulsion,
By in isatis root extract addition stainless steel, emulsifying agent, initiator and distilled water are added, control the temperature of stainless steel
It is 40-45 DEG C, speed of agitator is 1800-2000r/min, stirs 0.5-0.7 hours, forms the Radix Isatidis emulsion of stabilization；Its
The mass ratio of middle isatis root extract, emulsifying agent, initiator and distilled water is 100：5-7:1.8-2.0:350-370；
The emulsifying agent is Tween-20；The initiator is benzoyl peroxide.
It is described to prepare Radix Isatidis microcapsules, also including polymerisation；The polymerisation, by melamine resin capsule
Wall material performed polymer is dropwise added drop-wise in above-mentioned Radix Isatidis emulsion, the turning with 1500-1800r/min in 65-70 DEG C of water-bath
Speed stirring, is added dropwise citric acid reduction pH to 3.5-4.0, is acidified, and acidificatoin time is 0.5-0.8 hours, is then warmed up to 80-
82 DEG C, react 1.5-2 hours, then heat to 88-90 DEG C, solidify 45-60 minutes, it is after reaction terminates, gained reaction solution is quiet
Put, suction filtration and wash suction filtration with ethanol and obtain solid matter, washed respectively 1 time with petroleum ether, distilled water, centrifugation takes precipitation
Thing, Radix Isatidis microcapsules are obtained after being dried at 40 DEG C.
The particle diameter D97 of the Radix Isatidis microcapsules is 1-2 μm.
The melamine resin cyst material performed polymer is 2 with the mass ratio of isatis root extract:1.
The Radix Isatidis microcapsules it is modified, during Radix Isatidis microcapsules are added into modifier solution, in 700-800r/min
Stirring under be dispersed in modifier solution, it is then static 60-80 minutes, then stir 5- under the conditions of 300-400r/min
7 minutes, it is spray-dried, and is adjusted pH value to neutrality, is obtained modified Radix Isatidis microcapsules.
The preparation method, also including preparing modified microcapsule emulsion；It is described to prepare modified microcapsule emulsion,
Modified Radix Isatidis microcapsules are added into ionic liquid, under the conditions of 50-53 DEG C, -0.012~-0.014MPa, with 400-
The rotating speed of 450r/min, dispersed with stirring 30-35 minutes, prepares modified Radix Isatidis microcapsule emulsion.
The ionic liquid is 1- ethyl-3-methylimidazole acetate.
The preparation method, also including preparing co-blended spinning liquid；Described to prepare co-blended spinning liquid, the modified plate is blue
Radix Isatidis microcapsules and the mass ratio of alpha cellulose in viscose glue stoste are 0.098-0.10 in root microcapsule emulsion:1；It is described viscous
Collagen solution, content of alphacellulose is 9.5-9.8%, and total alkali is 3.0-3.3%, and viscosity 45-50s, degree of ripeness is 15-
17ml。
By adopting the above-described technical solution, having the technical effect that of reaching of the present invention：
（1）Radix Isatidis viscose rayon prepared by the present invention, the content of Radix Isatidis microcapsules is 9.1-9.79% in fiber, is coagulated on year-on-year basis
The backwash rate reduction 50-55% admittedly bath filter is pulled away a prop, water consumption reduces 500-520 side/day, coagulating bath crystalline product sal glauberi
Middle Radix Isatidis is reduced to below 100-110ppm.
（2）Radix Isatidis viscose rayon prepared by the present invention, Radix Isatidis is evenly distributed in the fibre；And Radix Isatidis microcapsules
With being firmly combined with for fiber, the Radix Isatidis active principle of fiber surface can be avoided from being lost in washing or friction；By examination
Issue after examination and approval now, after washing 50 times, the loss late of the Radix Isatidis of fiber surface is only 2.0-2.5%.
（3）Radix Isatidis viscose rayon prepared by the present invention, the dry fracture strength 2.70-2.75cN/dtex of fiber, wet fracture
Intensity is 1.70-1.75cN/dtex, and elongation at break is 22-23%, good hygroscopicity, and the regain of fiber is 14-15%, and
The wearability of common viscose fiber can be improved, fibre density is 1.42-1.45g/cm3.
（4）Radix Isatidis viscose rayon prepared by the present invention, can be effective against influenza A virus and influenza B virus,
Also there is inhibiting rate higher to staphylococcus aureus, Candida albicans, typhoid bacillus, to staphylococcus aureus bacteriostasis rate
99.0%-99.8%, the bacteriostasis rate to Candida albicans is 96.6-98.8%, is 97.2%-99.1% to typhoid bacillus bacteriostasis rate, right
Influenza A virus, influenza B virus have very strong suppression killing action.
Specific 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, can also make certain adjustments and improvements.These belong to guarantor of the invention
Shield scope.
A kind of preparation method of the viscose rayon containing isatis root extract of embodiment 1
Comprise the following steps：
（1）Prepare Radix Isatidis microcapsules
A, prepare Radix Isatidis emulsion
By in isatis root extract addition stainless steel, emulsifying agent, initiator and distilled water are added, control the temperature of stainless steel
It is 40 DEG C, speed of agitator is 1800r/min, stirs 0.5 hour, forms the Radix Isatidis emulsion of stabilization；
Wherein the mass ratio of isatis root extract, emulsifying agent, initiator and distilled water is 100：5:1.8:350；
The emulsifying agent is Tween-20；The initiator is benzoyl peroxide.
, prepare melamine resin cyst material performed polymer
37% formalin is put into reactor, is stirred, regulation pH value is 7.8, by 37% formalin：Melamine is
4:1 ratio adds melamine, is warming up to 65 DEG C, with 800r/min stirring reactions 0.8 hour under constant temperature, is made trimerization
Cyanamide formaldehyde resin cyst material performed polymer.
, polymerisation
Melamine resin cyst material performed polymer is dropwise added drop-wise in above-mentioned Radix Isatidis emulsion, in 65 DEG C of water-baths
Stirred with the rotating speed of 1500r/min, citric acid reduction pH is added dropwise to 3.5, be acidified, acidificatoin time is 0.5 hour, Ran Housheng
Temperature is reacted 1.5 hours to 80 DEG C, then heats to 88 DEG C, is solidified 45 minutes, after reaction terminates, gained reaction solution is stood, is taken out
Filter and wash suction filtration with ethanol and obtain solid matter, washed respectively 1 time with petroleum ether, distilled water, centrifugation, taking precipitate,
Radix Isatidis microcapsules are obtained after being dried at 40 DEG C.
The particle diameter D97 of the Radix Isatidis microcapsules is 1-2 μm.
The melamine resin cyst material performed polymer is 2 with the mass ratio of isatis root extract:1.
Find in actual applications, above-mentioned melamine resin cyst material performed polymer so that Radix Isatidis microcapsules
Combination with fiber is more firm, and the Radix Isatidis active principle of fiber surface can be avoided to be lost in washing or friction.
（2）Radix Isatidis microcapsules it is modified
By Radix Isatidis microcapsules add modifier solution in, in being dispersed in modifier solution under the stirring of 700r/min,
Then static 60 minutes, then stirred 5 minutes under the conditions of 300r/min, be spray-dried, and adjust pH value to neutrality so that
Cationic polysaccharide-guar gum and shitosan on Radix Isatidis surface of microcapsule uniform adsorption in modifying agent and be modified, changed
Radix Isatidis microcapsules after property.
The modifier solution, in parts by weight, including 3 parts of guar gum, 5 parts of shitosan, 1 part of polyvinyl alcohol, pure water
30 parts, 100 parts of acetic acid.
The polyvinyl alcohol, is chip solid；
The preparation of the modifier solution, comprises the following steps：
The preparation of A, poly-vinyl alcohol solution
According to the formula of modifying agent, each raw material components are weighed, pure water is put into agitator tank, start stirring, speed of agitator is
1200r/min, while adding polyvinyl alcohol chip solid, temperature is warmed up to 95 DEG C, insulation from 25 DEG C with 5 DEG C per minute of speed
30min, until polyvinyl alcohol is completely dissolved, starts stirring always, prevents crystallization from separating out, and the preparation of poly-vinyl alcohol solution is obtained.
The preparation of B, chitosan solution
Shitosan and acetic acid are mixed, dissolving, preparation obtains 5% shitosan acetic acid solution.
C, mixing
Chitosan solution prepared by step B, is placed in stand-by in stainless steel；
In the poly-vinyl alcohol solution for adding step A to prepare guar gum, after the stirring and dissolving of 800r/min, polyvinyl alcohol is prepared
With the mixed liquor of guar gum, be slowly dropped in the stainless steel containing shitosan acetic acid solution, rate of addition be 0.5 part/
Min, it is 40 DEG C to control the temperature of stainless steel, and speed of agitator is 900r/min, and completion of dropping is incubated 10 minutes, is obtained modified
Agent solution.
（3）Prepare modified Radix Isatidis microcapsule emulsion
Modified Radix Isatidis microcapsules are added into ionic liquid, under the conditions of 50 DEG C, -0.012MPa, with turning for 400r/min
Speed, dispersed with stirring 30 minutes prepares modified Radix Isatidis microcapsule emulsion.
（4）Prepare co-blended spinning liquid
With cellulose pulp as raw material, viscose glue stoste is obtained through conventional viscose preparation technology, by modified Radix Isatidis microcapsules
Emulsion carries out standing and defoaming, using injection device before spinning, by the Radix Isatidis microcapsule emulsion addition viscose glue stoste after deaeration, makes
Standby co-blended spinning liquid；
In the modified Radix Isatidis microcapsule emulsion in Radix Isatidis microcapsules and viscose glue stoste alpha cellulose mass ratio
It is 0.099:1.
The viscose glue stoste, content of alphacellulose is 9.5-9.8%, and total alkali is 3.0-3.3%, viscosity 45-50s,
Degree of ripeness is 15-17ml (10% ammonium chloride value).
（5）Spinning moulding
The coagulating bath that the addition of co-blended spinning liquid is adjusted is carried out into spinning, 3% acid bath compounding agent solution is added in acid bath, stirring is equal
It is even, in the acid bath, sulfuric acid concentration 130g/l, sodium sulfate concentration 130g/l, sulfuric acid zinc concentration 4g/l, the temperature of acid bath：50℃；
Leaching length：450 millimeters, shower nozzle drawing-off：77%；Speed 27m/min is spun in drawing-off 16% between disk, three bath drawing-off -2%, four bath drawing-offs 5%.
The acid bath compounding agent solution, in parts by weight, including following raw material components：
6 parts of starch tertiary amino alkyl ether, 5 parts of quaternary ammonium starch ethers, 10 parts of poly-quaternary ammonium salt, stearyl dimethyl benzyl ammonium chloride 3
Part, 4 parts of dodecyl dimethyl benzyl ammonium chloride, 100 parts of pure water.
The poly-quaternary ammonium salt is poly-quaternary ammonium salt 10；
The preparation method of acid bath compounding agent solution, comprises the following steps：
Mixing adds pure water in filling, and starts stirring, and rotating speed is 500r/min, is subsequently adding starch tertiary amino alkyl ether, quaternary ammonium
The mixture of starch ether, charging rate is 1 part/min, and charging is finished, and temperature is warmed up to 95 from 25 DEG C with 5 DEG C per minute of speed
DEG C, 15 minutes are incubated, reuse recirculated cooling water and cool to 60 DEG C, add poly-quaternary ammonium salt, octadecyl dimethyl benzyl chlorination
Ammonium, dodecyl dimethyl benzyl ammonium chloride, stir, and cool to 25 DEG C, filter to take filtrate, obtain acid bath compounding agent solution.
When the co-blended spinning liquid of spinning solution and modified Radix Isatidis microcapsule emulsion is injected to coagulating bath, first fibre starts
Forming and hardening.
Acid bath auxiliary agent of the present invention and modified Radix Isatidis microcapsules, are interacted, and modified Radix Isatidis can be allowed micro-
Capsule is uniformly adhered on the fiber surface of firm generation to the fiber flow after the fine shaping of first.
（6）Post processing
Gained tow is refined, dried by cut-out, mitigation sulfur removal technology, finish application bath and washing, obtains Radix Isatidis of the present invention
Viscose rayon.
Radix Isatidis viscose rayon prepared by the embodiment of the present invention 1, the content of Radix Isatidis microcapsules is 9.3% in fiber, is prepared
During the loss late of Radix Isatidis microcapsules pull away a prop backwash rate reduction by 50% for coagulating bath filter on year-on-year basis, water consumption reduce 500 sides/
My god, Radix Isatidis is reduced to below 100ppm in coagulating bath crystalline product sal glauberi.
Radix Isatidis viscose rayon prepared by the embodiment of the present invention 1, Radix Isatidis is evenly distributed in the fibre；And Radix Isatidis is micro-
Being firmly combined with for capsule and fiber, can avoid the Radix Isatidis active principle of fiber surface from being lost in washing or friction；Through
Overtesting finds that after washing 50 times, the loss late of the Radix Isatidis of fiber surface is only 2.0%.
Radix Isatidis viscose rayon prepared by the embodiment of the present invention 1, the dry fracture strength of fiber is 2.75cN/dtex, wet disconnected
Resistance to spalling is 1.75cN/dtex, and elongation at break is 22%, good hygroscopicity, and the regain of fiber is 15%, and can be improved general
The wearability of logical viscose rayon, fibre density is 1.42g/cm3.To staphylococcus aureus bacteriostasis rate 99.1%, to Candida albicans
Bacterium bacteriostasis rate 96.6%, to typhoid bacillus bacteriostasis rate 97.3%, RCA is used to influenza A virus, influenza B virus
Method detects that potency reaches 8.
A kind of preparation method of the viscose rayon containing isatis root extract of embodiment 2, comprises the following steps：
（1）Prepare Radix Isatidis microcapsules
A, prepare Radix Isatidis emulsion
By in isatis root extract addition stainless steel, emulsifying agent, initiator and distilled water are added, control the temperature of stainless steel
It is 45 DEG C, speed of agitator is 2000r/min, stirs 0.7 hour, forms the Radix Isatidis emulsion of stabilization；
Wherein the mass ratio of isatis root extract, emulsifying agent, initiator and distilled water is 100： 7: 2.0: 370；
The emulsifying agent is Tween-20；The initiator is benzoyl peroxide.
, prepare melamine resin cyst material performed polymer
37% formalin is put into reactor, is stirred, regulation pH value is 8.0, by 37% formalin：Melamine is
4:1 ratio adds melamine, is warming up to 70 DEG C, with 900r/min stirring reactions 1.2 hours under constant temperature, is made trimerization
Cyanamide formaldehyde resin cyst material performed polymer.
, polymerisation
Melamine resin cyst material performed polymer is dropwise added drop-wise in above-mentioned Radix Isatidis emulsion, in 70 DEG C of water-baths
Stirred with the rotating speed of 1800r/min, citric acid reduction pH is added dropwise to 4.0, be acidified, acidificatoin time is 0.8 hour, Ran Housheng
Temperature is reacted 2 hours to 82 DEG C, then heats to 90 DEG C, is solidified 60 minutes, after reaction terminates, gained reaction solution is stood, is taken out
Filter and wash suction filtration with ethanol and obtain solid matter, washed respectively 1 time with petroleum ether, distilled water, centrifugation, taking precipitate,
Radix Isatidis microcapsules are obtained after being dried at 40 DEG C.
The particle diameter D97 of the Radix Isatidis microcapsules is 1-2 μm.
The melamine resin cyst material performed polymer is 2 with the mass ratio of isatis root extract:1.
Find in actual applications, above-mentioned melamine resin cyst material performed polymer so that Radix Isatidis microcapsules
Combination with fiber is more firm, and the Radix Isatidis active principle of fiber surface can be avoided to be lost in washing or friction.
（2）Radix Isatidis microcapsules it is modified
By Radix Isatidis microcapsules add modifier solution in, in being dispersed in modifier solution under the stirring of 800r/min,
Then static 80 minutes, then stirred 7 minutes under the conditions of 400r/min, be spray-dried, and adjust pH value to neutrality so that
Cationic polysaccharide-guar gum and shitosan on Radix Isatidis surface of microcapsule uniform adsorption in modifying agent and be modified, changed
Radix Isatidis microcapsules after property.
The modifier solution, in parts by weight, including 3 parts of guar gum, 5 parts of shitosan, 1 part of polyvinyl alcohol, pure water
30 parts, 100 parts of acetic acid.
The polyvinyl alcohol, is chip solid；
The preparation of the modifier solution, comprises the following steps：
The preparation of A, poly-vinyl alcohol solution
According to the formula of modifying agent, each raw material components are weighed, pure water is put into agitator tank, start stirring, speed of agitator is
1300r/min, while adding polyvinyl alcohol chip solid, temperature is warmed up to 95 DEG C, insulation from 25 DEG C with 5 DEG C per minute of speed
30min, until polyvinyl alcohol is completely dissolved, starts stirring always, prevents crystallization from separating out, and the preparation of poly-vinyl alcohol solution is obtained.
The preparation of B, chitosan solution
Shitosan and acetic acid are mixed, dissolving, preparation obtains 5% shitosan acetic acid solution.
C, mixing
Chitosan solution prepared by step B, is placed in stand-by in stainless steel；
In the poly-vinyl alcohol solution for adding step A to prepare guar gum, after the stirring and dissolving of 900r/min, polyvinyl alcohol is prepared
With the mixed liquor of guar gum, be slowly dropped in the stainless steel containing shitosan acetic acid solution, rate of addition be 0.7 part/
Min, it is 45 DEG C to control the temperature of stainless steel, and speed of agitator is 1000r/min, and completion of dropping is incubated 15 minutes, is obtained and changes
Property agent solution.
（3）Prepare modified microcapsule emulsion
Modified Radix Isatidis microcapsules are added into ionic liquid, under the conditions of 53 DEG C, -0.014MPa, with turning for 450r/min
Speed, dispersed with stirring 35 minutes prepares modified Radix Isatidis microcapsule emulsion.
（4）Prepare co-blended spinning liquid
With cellulose pulp as raw material, viscose glue stoste is obtained through conventional viscose preparation technology, by modified Radix Isatidis microcapsules
Emulsion carries out standing and defoaming, using injection device before spinning, by the Radix Isatidis microcapsule emulsion addition viscose glue stoste after deaeration, makes
Standby co-blended spinning liquid；
In the modified Radix Isatidis microcapsule emulsion in Radix Isatidis microcapsules and viscose glue stoste alpha cellulose mass ratio
It is 0.10:1.
The viscose glue stoste, content of alphacellulose is 9.5-9.8%, and total alkali is 3.0-3.3%, viscosity 45-50s,
Degree of ripeness is 15-17ml (10% ammonium chloride value).
（5）Spinning moulding
The coagulating bath that the addition of co-blended spinning liquid is adjusted is carried out into spinning, 5% acid bath compounding agent solution is added in acid bath, stirring is equal
It is even, in the acid bath, sulfuric acid concentration 137g/l, sodium sulfate concentration 150g/l, sulfuric acid zinc concentration 6g/l, the temperature of acid bath： 52
℃；Leaching length：470 millimeters, shower nozzle drawing-off： 83%；Speed 32m/ is spun in drawing-off 21% between disk, three bath drawing-offs 8%, four bath drawing-offs 11%
min。
The specific leaching length and shower nozzle drawing-off that the present invention is used can be improved and lead a linear velocity so that strand is stopped in acid bath
Time is short；Reduce the loss of Radix Isatidis microcapsules.
The present invention can make up shaping not using specific sulfuric acid, the concentration of sodium sulphate, and acid bath temperature higher
Foot, it is ensured that the uniformity that Radix Isatidis microcapsules are distributed in the fibre.
The acid bath compounding agent solution, in parts by weight, including following raw material components：
6 parts of starch tertiary amino alkyl ether, 5 parts of quaternary ammonium starch ethers, 10 parts of poly-quaternary ammonium salt, stearyl dimethyl benzyl ammonium chloride 3
Part, 4 parts of dodecyl dimethyl benzyl ammonium chloride, 100 parts of pure water.
The poly-quaternary ammonium salt is poly-quaternary ammonium salt 10；
The preparation method of acid bath compounding agent solution, comprises the following steps：
Mixing adds pure water in filling, and starts stirring, and rotating speed is 550r/min, is subsequently adding starch tertiary amino alkyl ether, quaternary ammonium
The mixture of starch ether, charging rate is 1.5 parts/min, and charging is finished, and temperature is warmed up to from 25 DEG C with 5 DEG C per minute of speed
95 DEG C, 15 minutes are incubated, reuse recirculated cooling water and cool to 65 DEG C, add poly-quaternary ammonium salt, octadecyl dimethyl benzyl chlorine
Change ammonium, dodecyl dimethyl benzyl ammonium chloride, stir, cool to 25 DEG C, filter to take filtrate, obtain acid bath compounding agent solution.
When the co-blended spinning liquid of spinning solution and modified Radix Isatidis microcapsule emulsion is injected to coagulating bath, first fibre starts
Forming and hardening.
Acid bath auxiliary agent of the present invention is dispersed in coagulating bath, and during spinning moulding, coagulating bath is uniformly repelled altogether
Modified Radix Isatidis microcapsules in blended ratio liquid, make the inside or surface of its cellulose for being firmly attached to firm shaping,
And be uniformly distributed.
（6）Post processing
Gained tow is refined, dried by cut-out, mitigation sulfur removal technology, finish application bath and washing, obtains Radix Isatidis of the present invention
Viscose rayon.
Radix Isatidis viscose rayon prepared by the embodiment of the present invention 2, the content of Radix Isatidis microcapsules is 9.5% in fiber, on year-on-year basis
Coagulating bath filter is pulled away a prop backwash rate reduction by 55%, and water consumption reduces 520 sides/day, and plate is blue in coagulating bath crystalline product sal glauberi
Root is reduced to below 110ppm.
Radix Isatidis viscose rayon prepared by the embodiment of the present invention 2, Radix Isatidis is evenly distributed in the fibre；And Radix Isatidis is micro-
Being firmly combined with for capsule and fiber, can avoid the Radix Isatidis active principle of fiber surface from being lost in washing or friction；Through
Overtesting finds that after washing 50 times, the loss late of the Radix Isatidis of fiber surface is only 2.5%.
Radix Isatidis viscose rayon prepared by the embodiment of the present invention 2, the dry fracture strength of fiber is 2.70cN/dtex, wet disconnected
Resistance to spalling is 1.70cN/dtex, and elongation at break is 23%, good hygroscopicity, and the regain of fiber is 14%, and can be improved general
The wearability of logical viscose rayon, fibre density is 1.45g/cm3.To staphylococcus aureus bacteriostasis rate 99.7%, to Candida albicans
Bacterium bacteriostasis rate 98.5%, is 98.9% to typhoid bacillus bacteriostasis rate, solidifying using red blood cell to influenza A virus, influenza B virus
Collection method detects that potency reaches 9.
The selection of the microcapsule wall material of embodiment 3
Using the preparation method of the Radix Isatidis viscose rayon described in embodiment 1, only change step（1）In preparing Radix Isatidis microcapsules
The classification of cyst material, using the cyst material described in table 1 below, prepares viscose rayon respectively, determines the viscous of each group preparation
Glue fiber, after washing 50 times, the loss late of the Radix Isatidis of fiber surface.
The selection of the microcapsule wall material of table 1
Above-mentioned Lauxite, polystyrene, PIC, Arabic gum, makrolon buy finished product, described three from market
Melamine-formaldehyde resin cyst material performed polymer is the melamine resin capsule prepared using preparation method described in embodiment 1
Wall material performed polymer.
From the result of table 1, group 3 is most preferably selection, i.e., the melamine resin cyst wall that prepared by the present invention
Material performed polymer is most preferred cyst material, and it causes that the combination of Radix Isatidis microcapsules and fiber is more firm, it is possible to reduce fine
The turnover rate that the Radix Isatidis active principle in dimension table face is caused with washing or friction.
The spinning moulding technique of embodiment 4 is preferred
Using the preparation method of the Radix Isatidis viscose rayon described in embodiment 1, only change step（5）Leaching in spinning moulding grows,
Shower nozzle drawing-off, acid bath temperature, prepare viscose rayon respectively, and Radix Isatidis microcapsules contains in viscose rayon prepared by measure each group
Amount, and Radix Isatidis microcapsules distributivity in the fibre, distribution are more uniform, and score is higher, and full marks are 10 points, are specifically shown in Table 2.
The spinning moulding technique of table 2 is preferred
The coagulating bath that the addition of co-blended spinning liquid is adjusted is carried out into spinning, the acid bath compounding agent solution of 3-5%, stirring are added in acid bath
Uniformly, in the acid bath, sulfuric acid concentration 130-137g/l, sodium sulfate concentration 130-150g/l, sulfuric acid zinc concentration 4-6g/l, acid bath
Temperature：50-53℃；Leaching length：420-480 millimeters, shower nozzle drawing-off：75-85%；Drawing-off 16-21% between disk, three bath drawing-offs -2~
8%, four bath drawing-off 5-11%, spin speed 27-32m/min.
The spinning moulding technique of table 2 is preferred
From the result of table 2, group 10 is most preferred, i.e. leaching is grown：460 millimeters, shower nozzle drawing-off：77%；
The temperature of acid bath：50 DEG C is most preferred condition.
The content of Radix Isatidis in viscose rayon prepared by the present invention, is calculate fine relative to first；
Coagulating bath of the present invention, is acid bath.
Unless otherwise indicated, the percentage employed in the present invention is percetage by weight, ratio of the present invention,
It is 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 being described in detail to the present invention with reference to the foregoing embodiments, for a person skilled in the art, it still may be used
Modified with to the technical scheme described in foregoing embodiments, or equivalent is carried out to which part technical characteristic.
All any modification, equivalent substitution and improvements within the spirit and principles in the present invention, made etc., should be included in of the invention
Within protection domain.
Claims (10)
1. a kind of viscose rayon containing isatis root extract, it is characterised in that：The viscose rayon, the content of Radix Isatidis microcapsules
It is 9.1-9.79%, the dry fracture strength of fiber is 2.70-2.75cN/dtex, and wet breaking strength is 1.70-1.75cN/dtex,
Elongation at break is 22-23%.
2. a kind of preparation method of the viscose rayon containing isatis root extract, it is characterised in that：The preparation method, including plate is blue
Root microcapsules it is modified；Radix Isatidis microcapsules are modified by being modified for the Radix Isatidis microcapsules using modifier solution；Institute
Modifier solution is stated, in parts by weight, including 3 parts of guar gum, 5 parts of shitosan, 1 part of polyvinyl alcohol, 30 parts of pure water, acetic acid
100 parts.
3. the preparation method of a kind of viscose rayon containing isatis root extract according to claim 2, it is characterised in that：Institute
State preparation method, including spinning moulding；The spinning moulding is carried out in acid bath, and the acid bath auxiliary agent of 3-5% is added in the acid bath
Solution；The acid bath compounding agent solution, in parts by weight, including following raw material components：6 parts of starch tertiary amino alkyl ether, quaternary ammonium form sediment
5 parts of powder ether, 10 parts of poly-quaternary ammonium salt, 3 parts of stearyl dimethyl benzyl ammonium chloride, 4 parts of dodecyl dimethyl benzyl ammonium chloride,
100 parts of pure water.
4. the preparation method of a kind of viscose rayon containing isatis root extract according to claim 3, it is characterised in that：Institute
State acid bath, sulfuric acid concentration 130-137g/l, sodium sulfate concentration 130-150g/l, sulfuric acid zinc concentration 4-6g/l, the temperature of acid bath：
50-53℃。
5. the preparation method of a kind of viscose rayon containing isatis root extract according to claim 3, it is characterised in that：Institute
State spinning moulding, leaching length：420-480 millimeters, shower nozzle drawing-off：75-85%；Drawing-off 16-21% between disk, three bath drawing-off -2~8%, four
Bath drawing-off 5-11%, spins speed 27-32m/min.
6. the preparation method of a kind of viscose rayon containing isatis root extract according to claim 1, it is characterised in that：Institute
Preparation method is stated, also including preparing Radix Isatidis microcapsules；It is described to prepare Radix Isatidis microcapsules, including prepare melamino-formaldehyde tree
Adipose capsule wall material performed polymer；It is described to prepare melamine resin cyst material performed polymer, 37% formalin is put into
In reactor, stirring, regulation pH value is 7.8-8.0, by 37% formalin：Melamine is 4:1 ratio adds melamine
Amine, is warming up to 65-70 DEG C, with 800-900r/min stirring reactions 0.8-1.2 hours under constant temperature, is made melamino-formaldehyde
Resin cyst material performed polymer.
7. the preparation method of a kind of viscose rayon containing isatis root extract according to claim 2, it is characterised in that：Institute
The modified of Radix Isatidis microcapsules is stated, during Radix Isatidis microcapsules are added into modifier solution, in the stirring of 700-800r/min
Under be dispersed in modifier solution, it is then static 60-80 minutes, then under the conditions of 300-400r/min stir 5-7 minutes, carry out
Spray drying, and pH value to neutrality is adjusted, obtain modified Radix Isatidis microcapsules.
8. the preparation method of a kind of viscose rayon containing isatis root extract according to claim 2, it is characterised in that：Institute
Preparation method is stated, also including preparing modified microcapsule emulsion；It is described to prepare modified microcapsule emulsion, will be modified
Radix Isatidis microcapsules add ionic liquid, under the conditions of 50-53 DEG C, -0.012~-0.014MPa, with turning for 400-450r/min
Speed, dispersed with stirring 30-35 minutes, prepares modified Radix Isatidis microcapsule emulsion.
9. the preparation method of a kind of viscose rayon containing isatis root extract according to claim 2, it is characterised in that：Institute
Preparation method is stated, also including preparing co-blended spinning liquid；It is described to prepare co-blended spinning liquid, the modified Radix Isatidis microcapsules breast
Radix Isatidis microcapsules and the mass ratio of alpha cellulose in viscose glue stoste are 0.098-0.10 in liquid:1；The viscose glue stoste, first
It is 9.5-9.8% to plant content of cellulose, and total alkali is 3.0-3.3%, and viscosity 45-50s, degree of ripeness is 15-17ml.
10. the preparation method of a kind of viscose rayon containing isatis root extract according to claim 3, it is characterised in that：
The preparation method of the acid bath compounding agent solution, mixing adds pure water in filling, and starts stirring, and rotating speed is 500-550r/min, so
Starch tertiary amino alkyl ether, the mixture of quaternary ammonium starch ethers are added afterwards, and charging rate is 1-1.5 parts/min, and charging is finished, temperature
95 DEG C are warmed up to from 25 DEG C with 5 DEG C per minute of speed, 15 minutes are incubated, then cool to 60-65 DEG C, addition poly-quaternary ammonium salt, ten
Eight zephirans, dodecyl dimethyl benzyl ammonium chloride, stir, and cool to 25 DEG C, filter to take filter
Liquid, obtains acid bath compounding agent solution.
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| CN202010357353.2A CN111534875B (en) | 2017-03-24 | 2017-03-24 | Efficient antibacterial antiviral isatis root viscose fiber and preparation method thereof |
| CN201710183744.5A CN106929931B (en) | 2017-03-24 | 2017-03-24 | Viscose fiber containing isatis root extract and preparation method thereof |
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| CN111218751A (en) * | 2019-12-16 | 2020-06-02 | 江苏悦达家纺有限公司 | Isatis tinctoria viscose jacquard fabric and production method thereof |
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| CN111909507A (en) * | 2020-07-02 | 2020-11-10 | 青岛百草新材料股份有限公司 | Radix isatidis modified polyamide masterbatch for superfine fibers |
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| CN109505017A (en) * | 2018-11-29 | 2019-03-22 | 山传雷 | A kind of lavender plant source composite cellulose fiber and preparation method thereof |
| CN109576808A (en) * | 2018-11-29 | 2019-04-05 | 山传雷 | A kind of inorganic fire-retarded intelligent temperature adjusting fiber cellulose fiber and preparation method thereof |
| CN109505018B (en) * | 2018-11-29 | 2021-07-16 | 青岛邦特生态纺织科技有限公司 | Antibacterial and anti-mite Tiancha fiber and preparation method thereof |
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| CN111218751A (en) * | 2019-12-16 | 2020-06-02 | 江苏悦达家纺有限公司 | Isatis tinctoria viscose jacquard fabric and production method thereof |
| CN111621871A (en) * | 2020-07-02 | 2020-09-04 | 中科纺织研究院（青岛）有限公司 | Radix isatidis extract modified polyamide fiber and preparation method thereof |
| CN111909507A (en) * | 2020-07-02 | 2020-11-10 | 青岛百草新材料股份有限公司 | Radix isatidis modified polyamide masterbatch for superfine fibers |
| CN112176451A (en) * | 2020-07-09 | 2021-01-05 | 青岛尼希米生物科技有限公司 | Antibacterial and antiviral cellulose fiber and preparation method and application thereof |
| CN112176451B (en) * | 2020-07-09 | 2021-06-15 | 青岛尼希米生物科技有限公司 | Antibacterial and antiviral cellulose fiber and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111534875A (en) | 2020-08-14 |
| CN111534875B (en) | 2022-10-18 |
| CN106929931B (en) | 2020-05-12 |
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