CN112144144A - Alginate/cellulose composite fiber with flame retardant function and preparation method thereof - Google Patents
Alginate/cellulose composite fiber with flame retardant function and preparation method thereof Download PDFInfo
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- CN112144144A CN112144144A CN202011023432.6A CN202011023432A CN112144144A CN 112144144 A CN112144144 A CN 112144144A CN 202011023432 A CN202011023432 A CN 202011023432A CN 112144144 A CN112144144 A CN 112144144A
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- alginate
- preparation
- fiber
- cellulose
- composite fiber
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- 239000000835 fiber Substances 0.000 title claims abstract description 112
- 235000010443 alginic acid Nutrition 0.000 title claims abstract description 85
- 229920000615 alginic acid Polymers 0.000 title claims abstract description 85
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229940072056 alginate Drugs 0.000 title claims abstract description 79
- 229920002678 cellulose Polymers 0.000 title claims abstract description 71
- 239000001913 cellulose Substances 0.000 title claims abstract description 71
- 239000002131 composite material Substances 0.000 title claims abstract description 65
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical group N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 238000009987 spinning Methods 0.000 claims abstract description 81
- 230000015271 coagulation Effects 0.000 claims abstract description 52
- 238000005345 coagulation Methods 0.000 claims abstract description 52
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000648 calcium alginate Substances 0.000 claims abstract description 12
- 235000010410 calcium alginate Nutrition 0.000 claims abstract description 12
- 229960002681 calcium alginate Drugs 0.000 claims abstract description 12
- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=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](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 claims abstract description 12
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 12
- 239000011701 zinc Substances 0.000 claims abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 238000007670 refining Methods 0.000 claims abstract description 10
- 239000011550 stock solution Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 64
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 36
- 239000000661 sodium alginate Substances 0.000 claims description 36
- 235000010413 sodium alginate Nutrition 0.000 claims description 36
- 229940005550 sodium alginate Drugs 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 35
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 29
- 239000001110 calcium chloride Substances 0.000 claims description 28
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 28
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 22
- 229920003043 Cellulose fiber Polymers 0.000 claims description 18
- 238000004132 cross linking Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 239000011592 zinc chloride Substances 0.000 claims description 11
- 235000005074 zinc chloride Nutrition 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 238000007654 immersion Methods 0.000 claims description 7
- 229910021538 borax Inorganic materials 0.000 claims description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- 238000006477 desulfuration reaction Methods 0.000 claims description 6
- 230000023556 desulfurization Effects 0.000 claims description 6
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims description 6
- 239000004328 sodium tetraborate Substances 0.000 claims description 6
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 6
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 2
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 9
- 241000222122 Candida albicans Species 0.000 abstract description 6
- 241000588724 Escherichia coli Species 0.000 abstract description 6
- 229940095731 candida albicans Drugs 0.000 abstract description 6
- 229920000297 Rayon Polymers 0.000 description 25
- 239000003063 flame retardant Substances 0.000 description 20
- 238000005406 washing Methods 0.000 description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 241001474374 Blennius Species 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 8
- 238000004061 bleaching Methods 0.000 description 8
- 230000001112 coagulating effect Effects 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 230000005764 inhibitory process Effects 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 229960001126 alginic acid Drugs 0.000 description 6
- 239000000783 alginic acid Substances 0.000 description 6
- 150000004781 alginic acids Chemical class 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 150000001450 anions Chemical class 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000003009 desulfurizing effect Effects 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 description 4
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 238000010041 electrostatic spinning Methods 0.000 description 3
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 3
- 239000012991 xanthate Substances 0.000 description 3
- 229920001744 Polyaldehyde Polymers 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 241000512259 Ascophyllum nodosum Species 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 240000008790 Musa x paradisiaca Species 0.000 description 1
- 235000018290 Musa x paradisiaca Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000009982 effect on human Effects 0.000 description 1
- 210000003278 egg shell Anatomy 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- 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
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
- D06L4/10—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen
- D06L4/12—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen combined with specific additives
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
- D06L4/10—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen
- D06L4/13—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen using inorganic agents
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/155—Halides of elements of Groups 2 or 12 of the Periodic System
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/53—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/80—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides
- D06M11/82—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides with boron oxides; with boric, meta- or perboric acids or their salts, e.g. with borax
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
Abstract
The invention provides alginate/cellulose composite fiber with a flame-retardant function, wherein the alginate is zinc alginate and calcium alginate; the invention also provides a preparation method of the fiber. The preparation method comprises the steps of preparation of blended spinning stock solution, spinning and refining treatment; and the spinning comprises first coagulation bath forming, second coagulation bath forming, inter-disc drawing and plasticizing drawing. The fiber prepared by the invention has good biocompatibility, flame retardance, antibacterial activity and degradability, the dry breaking strength of the fiber is 2.36-2.58 cN/dtex, the moisture regain is 13.9-17.2%, the limiting oxygen index is 29.6-35.1%, the antibacterial rate to escherichia coli is more than or equal to 86.3%, reaches 86.3-93.2%, and the antibacterial rate to candida albicans is more than or equal to 83.1%, and reaches 83.1-89.7%.
Description
Technical Field
The invention belongs to the technical field of fiber preparation, and particularly relates to alginate/cellulose composite fiber with a flame retardant function and a preparation method thereof.
Background
The composite fiber is a modified fiber developed in the 60's of the 20 th century, and a bicomponent fiber having both polymer characteristics can be obtained by utilizing the composite fiber manufacturing technology.
Due to good hygroscopicity, comfortable wearing, natural degradation and excellent spinnability, the cellulose fiber (viscose fiber) has wide application and is mainly prepared by wet spinning. The alginate fiber as a novel biodegradable regenerated fiber is prepared from alginic acid separated from seaweed plants (such as kelp and seaweed) as a raw material, and the product has the functions of good biocompatibility, degradable absorptivity, hygroscopicity (moisture regain of 12-17%), flame retardance (oxygen index can reach 45), bacteriostasis, radiation resistance and the like. Alginate fibres are used herein to mean alginate fibres, of which calcium alginate fibres are most commonly used. Pure alginate fibers are white and have poor flame retardancy. The alginate/cellulose composite fiber has the characteristics of both alginate fiber and cellulose fiber, provides a new idea and method for the development of the composite fiber, and has a better development prospect.
Chinese patent CN200710014964.1 discloses a bioactive seaweed viscose fiber. The viscose fiber in the patent technology contains seaweed particles and zinc or silver, is prepared by utilizing the existing viscose fiber production equipment, and contains seaweed components with the functions of beautifying and protecting skin, so that the viscose fiber has a good health-care effect on human skin.
Chinese patent CN200610044595.6 discloses an anion cellulose/alginate composite fiber and a preparation method thereof. The patent technology prepares a sodium alginate viscous solution and anion generator function finishing agent slurry under certain process conditions, then mixes the sodium alginate viscous solution and the anion generator function finishing agent slurry with cellulose xanthate according to a certain proportion to prepare spinning dope, and then prepares the anion cellulose/alginate composite fiber through spinning and refining steps.
Chinese CN200610044596.0 discloses a cellulose/alginate composite fiber and a preparation method thereof, and the main technical points of the patent are as follows: firstly, preparing sodium alginate viscous solution under certain process conditions, then mixing the solution with cellulose xanthate according to a certain proportion to prepare spinning dope, and then spinning and refining to prepare the cellulose/alginate composite fiber.
Chinese patent CN200310110168.X discloses one kind of viscose active alginate fiber and its production process, and the viscose fiber contains alginate in 1-8 wt%. The production method of the viscose alginate fiber is characterized in that: the process comprises the steps of dissolving sodium alginate powder in NaOH solution with the concentration of 0.5mol/L, wherein the weight ratio of the sodium alginate powder to the NaOH solution is 1: 20-100, uniformly adding the seaweed colloidal solution into viscose in the process of dissolving fiber xanthate, mixing and grinding to prepare spinning solution, and spinning viscose active seaweed filaments or short filaments by using the spinning solution under specific acid bath composition and spinning process parameters.
The patent technologies all disclose seaweed/cellulose composite fibers, but the seaweed/cellulose composite fibers are basically sodium alginate or seaweed particles, and the substances have extremely strong hydrophilicity, so that the fibers or fabrics made of the seaweed/cellulose composite fibers are poor in washing fastness, and are difficult to use as textile fabrics; meanwhile, the above patent only utilizes the characteristics of moisture absorption, bacteriostasis and the like of the alginate fiber, and does not consider the flame retardance, and the flame-retardant composite fiber is a technical problem which is mainly solved by the patent technology.
Chinese patent CN201610568557.4 discloses a preparation method of a flame-retardant composite viscose fiber with good moisture absorption and air permeability, belonging to the technical field of viscose fiber preparation. The patent technology mainly uses a self-made hemp stem core viscose solution and a banana viscose solution as raw materials, carries out electrostatic spinning on the raw materials to obtain a composite viscose fiber, then carries out selective oxidation on sodium alginate by sodium periodate to prepare polyaldehyde sodium alginate, puts the composite viscose fiber obtained by spinning into the polyaldehyde sodium alginate solution for soaking and crosslinking, soaks the crosslinked composite viscose fiber in a calcium chloride solution, and finally, the composite viscose fiber is filtered and dried to obtain the flame-retardant composite viscose fiber with good moisture absorption and air permeability. The patent technology adopts electrostatic spinning, the electrostatic spinning does not reach the level of mass production, and meanwhile, the alginate is coated on the surface of the fiber by an after-finishing method, so that the performance of the viscose fiber is exerted less, and the problem of washing fastness exists in subsequent application.
Disclosure of Invention
In view of the problems in the prior art, the invention provides an alginate/cellulose composite fiber with a flame retardant function and a preparation method thereof, and the following purposes are achieved:
the prepared fiber has good biocompatibility, flame retardance, antibacterial activity and degradability;
the prepared fiber has good washing fastness.
In order to solve the technical problems, the invention adopts the following technical scheme:
the preparation method of the alginate/cellulose composite fiber with the flame retardant function comprises the following steps:
1. preparation of blended spinning dope
Cellulose pulp is used as a raw material, and a cellulose fiber spinning solution is prepared by a subsequent known viscose preparation process, wherein the cellulose fiber spinning solution comprises 8.2-9.5% of alpha cellulose and 4.3-5.8% (mass fraction) of sodium hydroxide;
dissolving a proper amount of sodium alginate with the polymerization degree of 600-800 in water, and preparing a sodium alginate spinning solution with the mass fraction of 5.2-8.5% through the processes of filtering, defoaming and the like;
the prepared sodium alginate spinning solution is added into the cellulose fiber spinning solution by a pre-spinning injection process, and is used in series through a dynamic mixer and a static mixer, so that the multifunctional additive and the spinning solution are fully and uniformly mixed, and the blended spinning solution is prepared.
Preferably, the mass ratio of sodium alginate to alpha cellulose in the sodium alginate spinning solution is 20-40: 80-60 calculated by sodium alginate to alpha cellulose in the cellulose fiber spinning solution.
Spinning of alginate/cellulose composite fiber with flame retardant function
(1) First coagulation bath forming
And spinning the prepared blended spinning solution by a spinning device and an adjusted first coagulating bath. The first coagulation bath consists of: 20-35 g/L hydrochloric acid, 30-60 g/L calcium chloride and 5.5-10.5 g/L zinc chloride, the coagulation bath temperature is 35-45 ℃, and the immersion bath time is 0.5-1.1 s.
After the first coagulation bath, the sodium alginate in the blended spinning solution is formed and converted into calcium alginate and zinc alginate, so that the formation of alginic acid is avoided, and the primary forming of cellulose in the blended spinning solution is realized.
(2) Second coagulation bath forming
And (4) carrying out a second coagulation bath on the tows after passing through the first coagulation bath, so that the cellulose is completely molded. The composition of the second coagulation bath is as follows: 30-35 g/L hydrochloric acid and 10.5-15.5 g/L zinc chloride, the coagulation bath temperature is 35-45 ℃, and the dipping bath time is 0.2-0.8 s. After two times of coagulating baths, the forming of alginate and cellulose in the fiber is realized.
The alginate is zinc alginate and calcium alginate, and the alginate and the cellulose exist in an interpenetrating copolymer network structure form.
(3) Inter-disc drawing and plastification drawing
And (3) carrying out disc-to-disc drafting on the fiber tows subjected to the coagulation bath twice, wherein the drafting rate is 43-52%. And (3) feeding the tows drafted between the discs into a plasticizing bath, wherein the plasticizing bath comprises: 5.0-10.0 g/L hydrochloric acid, 6.0-15.0 g/L calcium chloride, the temperature is 90-95 ℃, the plasticizing drafting is 8.0-15%, and the tow subjected to plasticizing drafting is cut off.
3. Refining treatment of alginate/cellulose composite fiber with flame retardant function
And (3) washing, cross-linking and finishing, desulfurizing, calcium chloride finishing, oiling, bleaching, drying and the like are carried out on the cut fiber, so as to prepare the alginate/cellulose composite fiber with the flame retardant function.
Washing with deionized water at the water washing temperature of 65-75 ℃;
the bath liquid used for the crosslinking finishing comprises: 0.5-1.0 g/L boric acid and 1.0-2.5 g/L sodium tetraborate, wherein the temperature is 50-65 ℃, the boric acid and the sodium tetraborate pass through two continuous bath stations, and the treatment time of each bath station is 5.0-8.0 min;
the bath liquid used in the desulfurization procedure is as follows: 3.0-8.0 g/L of sodium sulfide at 65-85 ℃;
the bath solution used in the calcium chloride finishing procedure is as follows: calcium chloride 4.0-10.0 g/L, pH 8.0-9.0, temperature 40-60 ℃; the treatment time is 1.0-5.0 min;
the oiling and bleaching process is a bath station, and the bath solution comprises the following components: 3.0-6.0 g/L of oil agent (mixture of Afilan CVS and Leomin PN of the chemical Co., Ltd., mass ratio of the Afilan CVS to the Leomin PN is 7: 1), and H2O21.0-3.0 g/L at 50-65 ℃.
The drying process comprises the following steps: the temperature is 105-120 ℃, and the time is 35-55 min.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
(1) the technology of the patent is innovated on the basis of the forming process of viscose and alginate fibers, and achieves better effect. By adjusting the production process and adopting a twice coagulation bath forming method, the gradual forming of the alginate and the cellulose is realized, the formation of alginic acid is avoided, the forming of the alginate is ensured, and the alginate and the cellulose exist in an interpenetrating copolymer network structure form. The prepared fiber has good biocompatibility, flame retardance, antibacterial activity and degradability, the dry breaking strength of the fiber is 2.36-2.58 cN/dtex, the moisture regain is 13.9-17.2%, the limiting oxygen index is 29.6-35.1%, the antibacterial rate to escherichia coli is more than or equal to 86.3%, 86.3-93.2%, the antibacterial rate to candida albicans is more than or equal to 83.1%, and 83.1-89.7%, the fiber obtained by adopting a soil burying method cannot be sampled after 60 days, and the degradation rate can reach 91.6-95.3%.
The alginate in the finally prepared fiber exists in the forms of calcium alginate and zinc alginate, and the prepared fiber forms an interpenetrating copolymer network structure with cellulose fiber in the form of macromolecular chains of an eggshell structure (metal ions are equivalent to an egg core).
(2) The invention innovates the refining process of the prepared alginate/cellulose composite fiber with the flame retardant function. The stability of the fiber structure and the washing fastness of the fiber are ensured by carrying out cross-linking finishing and calcium chloride finishing on the alginate. After 50 times of washing, the composite fiber has the dry breaking strength of 2.25-2.39 cN/dtex, the moisture regain of 13.5-17.3%, the limiting oxygen index of 29.5-34.2%, the Escherichia coli inhibition rate of more than or equal to 83.5% and up to 83.5-91.2%, and the Candida albicans inhibition rate of more than or equal to 80.2% and up to 80.2-87.9%.
Detailed Description
Example 1:
the preparation method of the flame-retardant functional alginate/cellulose composite fiber with the specification of 1.33dtex 38mm comprises the following steps:
1. preparation of blended spinning dope
Cellulose pulp is taken as a raw material, and a cellulose fiber spinning solution is prepared by the following known viscose preparation process, wherein the cellulose fiber spinning solution comprises 8.2 percent of alpha cellulose and 4.3 percent of sodium hydroxide (mass fraction); dissolving a proper amount of sodium alginate with the polymerization degree of 600 in water, and preparing a sodium alginate spinning solution with the mass fraction of 5.2% through the processes of filtering, defoaming and the like;
adding the prepared sodium alginate spinning solution into the cellulose fiber spinning stock solution by using a pre-spinning injection process according to the mass ratio of the sodium alginate to the alpha cellulose of 20:80 to prepare a blended spinning stock solution.
Spinning of alginate/cellulose composite fiber with flame retardant function
(1) First coagulation bath forming
And spinning the prepared blended spinning solution by a spinning device and an adjusted first coagulating bath. The first coagulation bath consists of: 35g/L hydrochloric acid, 30g/L calcium chloride and 10.5g/L zinc chloride, the coagulation bath temperature is 45 ℃, and the bath immersion time is 1.1 s. After the first coagulation bath, the sodium alginate in the blended spinning solution is formed and converted into calcium alginate and zinc alginate, so that the formation of alginic acid is avoided, and the primary forming of cellulose in the blended spinning solution is realized.
(2) Second coagulation bath forming
And (4) carrying out a second coagulation bath on the tows after passing through the first coagulation bath, so that the cellulose is completely molded. The composition of the second coagulation bath is as follows: 35g/L hydrochloric acid and 15.5g/L zinc chloride, the coagulation bath temperature is 35 ℃, and the dipping bath time is 0.2 s. After two times of coagulating bath, the formation of calcium alginate, zinc alginate and cellulose in the fiber is realized.
(3) Inter-disc drawing and plastification drawing
The fiber tows which pass through the coagulation bath twice are firstly subjected to disc-to-disc drafting, and the drafting rate is 52%. And (3) feeding the tows drafted between the discs into a plasticizing bath, wherein the plasticizing bath comprises: 10g/L hydrochloric acid and 6.0g/L calcium chloride, the temperature is 95 ℃, the plasticizing drafting is 15%, and the tow subjected to the plasticizing drafting is cut off.
Refining treatment of alginate/cellulose composite fiber with flame retardant function
And (3) washing, cross-linking and finishing, desulfurizing, calcium chloride finishing, oiling, bleaching, drying and the like are carried out on the cut fiber, so as to prepare the alginate/cellulose composite fiber with the flame retardant function. Washing with deionized water at 65 deg.C; the bath liquid used for the crosslinking finishing is as follows: 0.5g/L of boric acid, 1.0g/L of sodium tetraborate,the temperature is 50 ℃, and the treatment time of each bath station is 5.0 min; the bath liquid used in the desulfurization procedure is as follows: 8.0g/L of sodium sulfide at 65 ℃; the bath solution used in the calcium chloride finishing procedure is as follows: calcium chloride 4.0g/L, pH 8.0, temperature 40 deg.C, and treatment time 5.0 min; the oiling and bleaching process is a bath station, and the bath solution comprises the following components: 6.0g/L of oil agent (mixture of Afilan CVS and Leomin PN of the chemical Co., Ltd., mass ratio of the Afilan CVS to the Leomin PN is 7: 1), H2O21.0g/L and the temperature is 65 ℃; and (3) drying: the temperature was 105 ℃ and the time 55 min.
The index of the prepared flame-retardant functional alginate/cellulose composite fiber with the specification of 1.33dtex 38mm is shown in table 1.
Comparative example 1:
on the basis of example 1, only one coagulation bath molding was carried out, the coagulation bath composition: 35g/L hydrochloric acid, 30g/L calcium chloride and 10.5g/L zinc chloride, the coagulation bath temperature is 45 ℃, and the bath immersion time is 1.1 s. Under the condition that other technical schemes are not changed, the indexes of the prepared composite fiber are shown in the table 1.
Comparative example 2:
the indexes of the prepared fibers are shown in table 1 without the calcium chloride finishing step and other technical schemes being changed on the basis of example 1.
Example 2:
the preparation method of the flame-retardant functional alginate/cellulose composite fiber with the specification of 1.56dtex 38mm comprises the following steps:
1. preparation of blended spinning dope
Cellulose pulp is taken as a raw material, and a cellulose fiber spinning solution is prepared by the following known viscose preparation process, wherein the cellulose fiber spinning solution comprises 8.9 percent of alpha cellulose and 5.2 percent of sodium hydroxide (mass fraction); dissolving a proper amount of sodium alginate with the polymerization degree of 715 in water, and preparing a sodium alginate spinning solution with the mass fraction of 6.8% through the working procedures of filtering, defoaming and the like;
adding the prepared sodium alginate spinning solution into the cellulose fiber spinning stock solution by using a pre-spinning injection process according to the mass ratio of the sodium alginate to the alpha cellulose of 30:70 to prepare a blended spinning stock solution.
Spinning of alginate/cellulose composite fiber with flame retardant function
(1) First coagulation bath forming
And spinning the prepared blended spinning solution by a spinning device and an adjusted first coagulating bath. The first coagulation bath consists of: 27.6g/L hydrochloric acid, 46g/L calcium chloride and 7.9g/L zinc chloride, the coagulation bath temperature is 39 ℃, and the bath immersion time is 0.8 s. After the first coagulation bath, the sodium alginate in the blended spinning solution is formed and converted into calcium alginate and zinc alginate, so that the formation of alginic acid is avoided, and the primary forming of cellulose in the blended spinning solution is realized.
(2) Second coagulation bath forming
And (4) carrying out a second coagulation bath on the tows after passing through the first coagulation bath, so that the cellulose is completely molded. The composition of the second coagulation bath is as follows: 31g/L hydrochloric acid and 12.8g/L zinc chloride, the coagulation bath temperature is 39.5 ℃, and the bath immersion time is 0.5 s. After two times of coagulating bath, the formation of calcium alginate, zinc alginate and cellulose in the fiber is realized.
(3) Inter-disc drawing and plastification drawing
The fiber tow subjected to the coagulation bath twice was first subjected to inter-tray drawing at a draw ratio of 49%. And (3) feeding the tows drafted between the discs into a plasticizing bath, wherein the plasticizing bath comprises: 7.8g/L hydrochloric acid and 12.5g/L calcium chloride, the temperature is 93 ℃, the plasticizing drafting is 11.6 percent, and the tow subjected to the plasticizing drafting is cut off.
Refining treatment of alginate/cellulose composite fiber with flame retardant function
And (3) washing, cross-linking and finishing, desulfurizing, calcium chloride finishing, oiling, bleaching, drying and the like are carried out on the cut fiber, so as to prepare the alginate/cellulose composite fiber with the flame retardant function. Washing with deionized water at the temperature of 69 ℃; the bath liquid used for the crosslinking finishing is as follows: boric acid of 0.8g/L and sodium tetraborate of 1.9g/L at 59 ℃, and two bath stations, wherein the treatment time of each bath station is 7.0 min; the bath liquid used in the desulfurization procedure is as follows: 5.0g/L of sodium sulfide at 76 ℃; the bath solution used in the calcium chloride finishing procedure is as follows: chlorination ofCalcium 7.8g/L, pH 8.5, temperature 52 deg.C, and treatment time 3.5 min; the oiling and bleaching process is a bath station, and the bath solution comprises the following components: oil solution 4.6g/L (mixture of Afilan CVS and Leomin PN of Clarian chemical Co., Ltd., mass ratio of Afilan CVS to Leomin PN is 7: 1), H2O22.5g/L and 56 ℃ of temperature; and (3) drying: the temperature was 115 ℃ and the time was 45 min.
The index of the prepared flame-retardant functional alginate/cellulose composite fiber with the specification of 1.56dtex 38mm is shown in table 1.
Example 3:
the preparation method of the flame-retardant functional alginate/cellulose composite fiber with the specification of 1.67dtex 38mm comprises the following steps:
1. preparation of blended spinning dope
Cellulose pulp is taken as a raw material, and a cellulose fiber spinning solution is prepared by the following known viscose preparation process, wherein the cellulose fiber spinning solution comprises 9.5 percent of alpha cellulose and 5.8 percent of sodium hydroxide (mass fraction); dissolving a proper amount of sodium alginate with the polymerization degree of 800 in water, and preparing a sodium alginate spinning solution with the mass fraction of 8.5 percent through the working procedures of filtering, defoaming and the like;
adding the prepared sodium alginate spinning solution into the cellulose fiber spinning solution by using a pre-spinning injection process according to the mass ratio of the sodium alginate to the alpha cellulose of 40:60 to prepare a blended spinning solution.
Spinning of alginate/cellulose composite fiber with flame retardant function
(1) First coagulation bath forming
And spinning the prepared blended spinning solution by a spinning device and an adjusted first coagulating bath. The first coagulation bath consists of: 20g/L hydrochloric acid, 60g/L calcium chloride and 5.5g/L zinc chloride, the coagulation bath temperature is 35 ℃, and the bath immersion time is 0.5 s. After the first coagulation bath, the sodium alginate in the blended spinning solution is formed and converted into calcium alginate and zinc alginate, so that the formation of alginic acid is avoided, and the primary forming of cellulose in the blended spinning solution is realized.
(2) Second coagulation bath forming
And (4) carrying out a second coagulation bath on the tows after passing through the first coagulation bath, so that the cellulose is completely molded. The composition of the second coagulation bath is as follows: 30g/L hydrochloric acid and 10.5g/L zinc chloride, the coagulation bath temperature is 45 ℃, and the dipping bath time is 0.8 s. After two times of coagulating bath, the formation of calcium alginate, zinc alginate and cellulose in the fiber is realized.
(3) Inter-disc drawing and plastification drawing
The fiber tow subjected to the coagulation bath twice was first subjected to inter-tray drawing at a draw ratio of 43%. And (3) feeding the tows drafted between the discs into a plasticizing bath, wherein the plasticizing bath comprises: 5.0g/L hydrochloric acid and 6.0g/L calcium chloride, the temperature is 90 ℃, the plasticizing drafting is 8.0 percent, and the tow subjected to the plasticizing drafting is cut off.
Refining treatment of alginate/cellulose composite fiber with flame retardant function
And (3) washing, cross-linking and finishing, desulfurizing, calcium chloride finishing, oiling, bleaching, drying and the like are carried out on the cut fiber, so as to prepare the alginate/cellulose composite fiber with the flame retardant function. Washing with deionized water at 75 deg.C; the bath liquid used for the crosslinking finishing is as follows: boric acid 1.0g/L and sodium tetraborate 2.5g/L at 65 deg.C, and two bath stations, each bath station for 8.0 min; the bath liquid used in the desulfurization procedure is as follows: 3.0g/L of sodium sulfide at 85 ℃; the bath solution used in the calcium chloride finishing procedure is as follows: calcium chloride 10.0g/L, pH 9.0, temperature 60 deg.C, and treatment time 2.0 min; the oiling and bleaching process is a bath station, and the bath solution comprises the following components: oil solution 3.0g/L (mixture of Afilan CVS and Leomin PN of Clarian chemical Co., Ltd., mass ratio of Afilan CVS to Leomin PN is 7: 1), H2O23.0g/L at 50 ℃; and (3) drying: the temperature is 120 deg.C, and the time is 35 min.
The index of the prepared flame-retardant functional alginate/cellulose composite fiber with the specification of 1.67dtex 38mm is shown in table 1.
The physical and mechanical properties of the alginate/cellulose composite fibers with the flame retardant function prepared in the embodiments 1-3 and the comparative examples 1-2 are detected according to GB/T14463-.
The invention is according to GB/T20944.3-2008 evaluation of textile antibacterial performance, part 3: the inhibition rates of the flame-retardant alginate/cellulose composite fibers prepared in examples 1 to 3 and comparative examples 1 to 2 on escherichia coli and candida albicans were determined by an oscillation method, and the results are shown in table 1.
The limit oxygen index of the alginate/cellulose composite fiber with the flame retardant function is detected according to FZ/T50016, and the result is shown in Table 1.
TABLE 1 Performance index Condition of flame retardant alginate/cellulose composite fiber
As can be seen, the comparative example 1 adopts one-step solidification molding, and the dry breaking strength, the inhibition rate on escherichia coli, the inhibition rate on candida albicans and the limiting oxygen index of the composite material are all obviously lower than those of the example 1; comparative example 2 the calcium chloride finishing step was omitted and the fiber produced had a lower index than example 1.
After the flame-retardant alginate/cellulose composite fibers prepared in the examples 1-3 and the comparative examples 1-2 are washed for 50 times according to the standard FZ/T73023 appendix C4. simplified washing conditions and the washing method in the procedure, the physical and mechanical properties, the bacteriostatic property and the limiting oxygen index after 50 times of washing are detected according to GB/T14463-.
TABLE 2 Performance index of alginate/cellulose composite fiber with flame retardant function after washing for 50 times
After 50 times of washing, the inhibition rate of the fibers of comparative examples 1 and 2 on escherichia coli, the inhibition rate on candida albicans and the limiting oxygen index are all obviously lower than those of example 1.
It can be known from tables 1 and 2 that the alginate/cellulose composite fiber with flame retardant function provided by the invention still has higher physical and mechanical properties, antibacterial activity and limiting oxygen index after being washed for 50 times, and the composite fiber provided by the invention is proved to have better washing resistance.
Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and the embodiments are within the scope of the present invention.
Claims (10)
1. The alginate/cellulose composite fiber with the flame retardant function is characterized in that: the alginate is zinc alginate and calcium alginate.
2. The alginate/cellulose composite fiber with flame retardant function of claim 1, wherein: the limiting oxygen index of the composite fiber is not less than 29%.
3. A preparation method of alginate/cellulose composite fiber with flame retardant function is characterized in that: the preparation method comprises the steps of preparation of blended spinning stock solution, spinning and refining treatment; and the spinning comprises first coagulation bath forming, second coagulation bath forming, inter-disc drawing and plasticizing drawing.
4. The preparation method of the alginate/cellulose composite fiber with the flame retardant function according to claim 3, which is characterized in that: the first coagulation bath is formed, the bath immersion time is 0.5-1.1 s, and the first coagulation bath comprises the following components: 20-35 g/L hydrochloric acid, 30-60 g/L calcium chloride and 5.5-10.5 g/L zinc chloride.
5. The preparation method of the alginate/cellulose composite fiber with the flame retardant function according to claim 3, which is characterized in that: and (3) forming by the second coagulation bath, wherein the bath soaking time is 0.2-0.8 s, and the composition of the second coagulation bath is as follows: 30-35 g/L hydrochloric acid and 10.5-15.5 g/L zinc chloride.
6. The preparation method of the alginate/cellulose composite fiber with the flame retardant function according to claim 3, which is characterized in that: inter-disc drafting and plasticizing drafting, and a plasticizing bath: 5.0-10.0 g/L hydrochloric acid, 6.0-15.0 g/L calcium chloride.
7. The preparation method of the alginate/cellulose composite fiber with the flame retardant function according to claim 3, which is characterized in that: in the refining, cross-linking finishing is added before the desulfurization procedure, and calcium chloride finishing is added after the desulfurization procedure.
8. The preparation method of the alginate/cellulose composite fiber with the flame retardant function according to claim 7, which is characterized in that: the cross-linking finishing is carried out by using the following bath liquids: 0.5-1.0 g/L of boric acid, 1.0-2.5 g/L of sodium tetraborate and at the temperature of 50-65 ℃; the calcium chloride is finished, and the used bath liquid is as follows: calcium chloride 4.0-10.0 g/L, pH 8.0-9.0, and temperature 40-60 deg.C.
9. The preparation method of the alginate/cellulose composite fiber with the flame retardant function according to claim 3, which is characterized in that: preparing the blended spinning solution, namely blending the cellulose fiber spinning solution and the sodium alginate spinning solution to obtain the blended spinning solution; the mass ratio of the sodium alginate in the sodium alginate spinning solution to the alpha cellulose in the cellulose fiber spinning solution is 20-40: 80-60.
10. The preparation method of the alginate/cellulose composite fiber with the flame retardant function according to claim 9, which is characterized in that: the mass fraction of the sodium alginate spinning solution is 5.2-8.5%, and the polymerization degree of the sodium alginate is 600-800.
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Application publication date: 20201229 |