CN100558954C - The bamboo charcoal cellulose fiber manufacture method - Google Patents
The bamboo charcoal cellulose fiber manufacture method Download PDFInfo
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- CN100558954C CN100558954C CNB2007100150367A CN200710015036A CN100558954C CN 100558954 C CN100558954 C CN 100558954C CN B2007100150367 A CNB2007100150367 A CN B2007100150367A CN 200710015036 A CN200710015036 A CN 200710015036A CN 100558954 C CN100558954 C CN 100558954C
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- 235000017166 Bambusa arundinacea Nutrition 0.000 title claims abstract description 122
- 235000017491 Bambusa tulda Nutrition 0.000 title claims abstract description 122
- 241001330002 Bambuseae Species 0.000 title claims abstract description 122
- 235000015334 Phyllostachys viridis Nutrition 0.000 title claims abstract description 122
- 239000011425 bamboo Substances 0.000 title claims abstract description 122
- 239000003610 charcoal Substances 0.000 title claims abstract description 119
- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 238000009987 spinning Methods 0.000 claims abstract description 71
- 239000000835 fiber Substances 0.000 claims abstract description 18
- 239000002608 ionic liquid Substances 0.000 claims abstract description 16
- 229920002678 cellulose Polymers 0.000 claims abstract description 10
- 239000001913 cellulose Substances 0.000 claims abstract description 8
- 230000001112 coagulating effect Effects 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims description 36
- 238000000465 moulding Methods 0.000 claims description 12
- 235000019270 ammonium chloride Nutrition 0.000 claims description 9
- OCBHHZMJRVXXQK-UHFFFAOYSA-M benzyl-dimethyl-tetradecylazanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 OCBHHZMJRVXXQK-UHFFFAOYSA-M 0.000 claims description 9
- -1 polysiloxane Polymers 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- ANTRPGYRFWBOCY-UHFFFAOYSA-N 1-ethoxy-3-methyl-2h-imidazole Chemical compound CCON1CN(C)C=C1 ANTRPGYRFWBOCY-UHFFFAOYSA-N 0.000 claims description 7
- 238000005660 chlorination reaction Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- IAERQFQHENCECY-UHFFFAOYSA-N 1-butyl-2-chloro-3-methyl-2H-pyridine Chemical compound CC=1C(N(C=CC=1)CCCC)Cl IAERQFQHENCECY-UHFFFAOYSA-N 0.000 claims description 5
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 238000012805 post-processing Methods 0.000 claims description 4
- 238000004061 bleaching Methods 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- 239000013638 trimer Substances 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- NMUUVEZOVUBZNY-UHFFFAOYSA-N chloromethane;1h-imidazole Chemical class ClC.C1=CNC=N1 NMUUVEZOVUBZNY-UHFFFAOYSA-N 0.000 claims 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims 1
- REOJLIXKJWXUGB-UHFFFAOYSA-N mofebutazone Chemical group O=C1C(CCCC)C(=O)NN1C1=CC=CC=C1 REOJLIXKJWXUGB-UHFFFAOYSA-N 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 42
- 239000007864 aqueous solution Substances 0.000 abstract description 8
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 32
- 229940050176 methyl chloride Drugs 0.000 description 16
- 238000006116 polymerization reaction Methods 0.000 description 10
- 229920000742 Cotton Polymers 0.000 description 8
- 241000209094 Oryza Species 0.000 description 6
- 235000007164 Oryza sativa Nutrition 0.000 description 6
- 235000010980 cellulose Nutrition 0.000 description 6
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 6
- 235000009566 rice Nutrition 0.000 description 6
- 238000000498 ball milling Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- 229920001131 Pulp (paper) Polymers 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 238000007380 fibre production Methods 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 2
- 229960001763 zinc sulfate Drugs 0.000 description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 235000014676 Phragmites communis Nutrition 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
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- 239000003292 glue Substances 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000001226 triphosphate Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of bamboo charcoal cellulose fiber manufacture method, for cellulose is made spinning solution by ion liquid dissolving, add the sex change spinning solution of making behind the bamboo charcoal nano again, the coagulating bath spinning of making through ionic liquid aqueous solution forms then, and the content of bamboo charcoal nano is 4%～30% of finished fiber weight.Manufacture method of the present invention is simple to operate, and productivity ratio height, environmental pollution be few, it is little that operating personnel are endangered, and the bamboo charcoal cellulose fiber absorption property that makes, fungi-proofing performance and bacteriostasis property are good.
Description
Technical field
The present invention relates to a kind of cellulose fibre technology, especially relate to a kind of manufacture method of bamboo charcoal cellulose fiber.
Background technology
Cellulose is a kind of renewable resource, is prevalent in the Nature, all contains a large amount of celluloses in the secretion of plant such as trees, cotton, rice bar, corn and some bacteriums, and becomes the renewable resource that replaces the petroleum cracking fiber product.And in cellulose fibre, have the cellulose fibre of the active carbon of adsorbable peculiar smell, also more and more obtain people's favor.And contain the cellulose fibre of bamboo charcoal particle, and it not only has the function of absorption peculiar smell, and it can also distribute simple and elegant delicate fragrance, has the function of antibacterial and bacteriostatic simultaneously.But the cellulose fibre that contains bamboo charcoal of people's production at present, because of the bamboo charcoal reasons in structure, its absorption property and fungi-proofing poor-performing, and people produce when containing the cellulose fibre of bamboo charcoal, still adopt the conventional production method of present cellulose fibre to come production spinning viscose glue, the promptly main NaOH that adopts, carbon disulfide etc. are as solvent and auxiliary agent, and need carry out yellow to used cellulose, experienced and maturation, relate to sulfate simultaneously, chemical reagent such as sulfuric acid and zinc sulfate, but all above-mentioned organic reagents all have volatility, the health that environment is caused serious pollution and jeopardizing operating personnel; And inorganic reagent all has severe corrosive, and is very big to the corrosion of equipment.In addition, not only technological process is loaded down with trivial details, cost recovery is high to the recovery process of these chemical reagent, and can produce a large amount of waste gas and waste water, again environment is caused severe contamination.
Summary of the invention
Technical problem to be solved by this invention has provided a kind of bamboo charcoal cellulose fiber with good absorption property, fungi-proofing performance and bacteriostasis property.
This bamboo charcoal cellulose fiber is for after making spinning solution with cellulose by ion liquid dissolving, adding the sex change spinning solution spinning of making behind the bamboo charcoal nano again forms, wherein the content of bamboo charcoal nano is 4%～30% of finished fiber weight in the fiber, doing of this bamboo charcoal cellulose fiber then is by force 1.0～3cN/dtex, and dried stretching is 5～18%.
Wherein ionic liquid can adopt the 1-allyl, 3-methyl chloride imidazole salts ([AMIM] Cl), 1-butyl, the ionic liquid of 3-methyl chloride imidazole salts ([BMIM] Cl), chlorination 1-(2-ethoxy)-3-methylimidazole ([HeMIM] Cl), 3-methyl-N-butyl chloro-pyridine ([BMPy] Cl) or benzyl dimethyl tetradecyl ammonium chloride (BDTAC).
And it is corresponding, spinning coagulation bath can adopt the 1-allyl when spinning, 3-methyl chloride imidazole salts ([AMIM] Cl), 1-butyl, the temperature that 3-methyl chloride imidazole salts ([BMIM] Cl), chlorination 1-(2-ethoxy)-3-methylimidazole ([HeMIM] Cl), 3-methyl-N-butyl chloro-pyridine ([BMPy] Cl) or benzyl dimethyl tetradecyl ammonium chloride (BDTAC) are made are that 0～90 ℃, concentration then are≤30% ionic liquid aqueous solution.
It is a kind of simple to operate that the present invention also provides, and the productivity ratio height, environmental pollution is few and the manufacture method that operating personnel endangered little bamboo charcoal cellulose fiber.
This manufacture method comprises production stage
1) bamboo charcoal slurry configuration, it is the bamboo charcoal nano of 75～350nm that bamboo charcoal adopts particle diameter, in bamboo charcoal, add dispersant, adding deionized water again, to be configured to bamboo charcoal concentration be 18%～28% uniform bamboo charcoal slurry, then the bamboo charcoal slurry is ground 90～120min and make uniform bamboo charcoal nano slurry, for the convenience of producing, the bamboo charcoal slurry can adopt disposable configuration to use, and can adopt ball mill that the bamboo charcoal slurry is carried out ball milling, to improve grinding effect;
2) spinning solution preparation is adopted the cellulose after pulverizing evenly to mix with ionic liquid, and dissolve the spinning solution of making stable homogeneous under 40～120 ℃ of temperature, and the concentration of spinning solution can be 3～15%; It is raw material that cellulose can adopt the degree of polymerization one or more in 300～1500 the cotton pulp dregs of rice, wood pulps, bamboo pulp, reed pulp, cotton stalk bark pulp, the livings poplar pulp of speed;
3) spinning, the ratio that the bamboo charcoal nano slurry that step 1 is made accounts for finished fiber weight 4%～30% in bamboo charcoal be added into the spinning solution that step 2 makes and mix after make the sex change spinning solution, spinning moulding after coagulating bath afterwards, can carry out deaeration, filtration to it, to improve its spinnability;
Fiber strand silk behind the spinning moulding is made the finished product bamboo charcoal cellulose fiber through drawing-off, post processing and oven dry, the content that makes bamboo charcoal nano in the finished product bamboo charcoal cellulose fiber is 4%～30% of finished fiber weight, and doing of this bamboo charcoal cellulose fiber is by force 1.0～3cN/dtex, and dried stretching is 5～18%.
In order to improve the convenience of bamboo charcoal nano slurry configuration, when carrying out the configuration of bamboo charcoal nano slurry, add amine cation type surfactant, as two alkyl-dimethyl ammonium chlorides, many alkyl trimethyl ammonium chlorides, addition is that 0.01%～0.6% of bamboo charcoal weight is added; It is the cationoid surfactant that dispersant then can adopt silicon, and as polysiloxane quaternary ammonium, dialkoxy silicane quaternary ammonium salt or sodium phosphate trimer, it is pressed 0.1%～1.5% of bamboo charcoal weight and adds.
In the spinning solution preparation, adopt the ionic liquid of dissolving cellulos can adopt the 1-allyl, ionic liquid, the 1-butyl of 3-methyl chloride imidazole salts ([AMIM] Cl), the ionic liquid of the ionic liquid of 3-methyl chloride imidazole salts ([BMIM] Cl), chlorination 1-(2-ethoxy)-3-methylimidazole ([HeMIM] Cl), the ionic liquid of 3-methyl-N-butyl chloro-pyridine ([BMPy] Cl) or the ionic liquid of benzyl dimethyl tetradecyl ammonium chloride (BDTAC).
And spinning coagulation bath can adopt the 1-allyl when spinning, to be 0～90 ℃, concentration be≤30% ionic liquid aqueous solution for 3-methyl chloride imidazole salts ([AMIM] Cl), 1-butyl, the temperature that 3-methyl chloride imidazole salts ([BMIM] Cl), chlorination 1-(2-ethoxy)-3-methylimidazole ([HeMIM] Cl), 3-methyl-N-butyl chloro-pyridine ([BMPy] Cl) or benzyl dimethyl tetradecyl ammonium chloride (BDTAC) are made.
In order to guarantee the excellent properties of this bamboo charcoal cellulose fiber, when being carried out post processing, it does not carry out the bleaching process post processing, to prevent the loss of its active ingredient, prevent from bamboo charcoal and antibacterial substance are wherein damaged, reduce the performance of finished fiber.
Drawing-off behind the fiberizing can the drawing-off of organizine mouth, air bath drawing-off, the first plasticizing-bath drawing-off, the second plasticizing-bath drawing-off, and its process conditions are silk mouthful drawing-off-10%～0%, air bath drawing-off 0%～60%, the first plasticizing-bath drawing-off, 5%～100%, the second plasticizing-bath drawing-off 5%～100%.
Bamboo charcoal cellulose fiber disclosed in this invention and manufacture method thereof, because ionic liquid has the boiling point height, non-volatile, in wider temperature range, exist with liquid state, and good heat endurance characteristics are arranged, and are the good solvents of many organic matters, inorganic matter and macromolecular material, and it is very big to cellulosic solubility, some in addition can reach more than 35% (mass percent), so adopt the ion liquid dissolving spinning to enhance productivity greatly.And adopt the ion liquid dissolving spining technology, cancelled in the manufacture process that human environment is polluted industrial chemicals such as big carbon disulfide, sulfuric acid, sulfate such as zinc sulfate, reduced the environmental hazard of fiber production process, and to operating personnel's harm.Cancel the bleaching process of conventional dope fiber production process equally at aftertreatment technology, prevent from bamboo charcoal and antibacterial substance are wherein damaged, influence the outward appearance of the functional and product of product.Product of the present invention has natural antibiotic fungi-proofing, generating negative ions, far infrared health care and removes peculiar smell, delicate fragrance function, and its textiles of making has characteristics smooth, fine and smooth, that feel nice and cool simultaneously, is specially adapted to summer clothes apparel product field.
The specific embodiment
Following examples explanation embodiment of the present invention, but the present invention is not limited to following examples.
Embodiment 1:
The configuration of bamboo charcoal slurry: adopting particle diameter is the bamboo charcoal of 125nm, in bamboo charcoal, press 0.3% of bamboo charcoal weight and add two alkyl-dimethyl ammonium chlorides, press 0.5% of bamboo charcoal weight and add polysiloxane quaternary ammonium, add deionized water again, be configured to 25% bamboo charcoal slurry, place ball mill, ball milling 100min makes uniform bamboo charcoal nano slurry;
The preparation of spinning solution: the degree of polymerization is about 330 cotton pulp dregs of rice pulverizing back and 1-allyl, and 3-methyl chloride imidazole salts solution evenly mixes, and at the spinning solutions of 90 ℃ of dissolving formation stable homogeneous, the concentration of spinning solution is 5%;
Spinning: the bamboo charcoal nano slurry of configuration is accounted for the ratio of finished fiber weight 5% in bamboo charcoal wherein, be blended in the spinning solution and stir, the above-mentioned spinning solution that mixes obtains containing the sex change spinning solution of bamboo charcoal through deaeration, filtration; Via the 1-allyl, the concentration that the 3-methyl chloride imidazole salts aqueous solution is made is 10%, and temperature is 50 ℃ a coagulating bath spinning moulding.The shaping fiber strand through the drawing-off flow process is: silk mouthful drawing-off → air bath drawing-off → first plasticizing-bath drawing-off → second plasticizing-bath drawing-off, its process conditions are: silk mouthful drawing-off-10%, air bath drawing-off 5%, the first plasticizing-bath drawing-off 10%, the second plasticizing-bath drawing-off 55% obtains the 1.33dtex*38mm bamboo charcoal cellulose fiber.The dried strong 2.35cN/dtex of finished product bamboo charcoal cellulose fiber driedly stretches 16.5%.
Embodiment 2:
The configuration of bamboo charcoal slurry: adopting particle diameter is the bamboo charcoal of 80nm, in bamboo charcoal, press 0.5% of bamboo charcoal weight and add two alkyl-dimethyl ammonium chlorides, press 1.5% of bamboo charcoal weight and add sodium phosphate trimer, add deionized water again, be configured to 22% bamboo charcoal slurry, make uniform bamboo charcoal nano slurry behind the grinding 120min;
The preparation of spinning solution: the degree of polymerization is about 800 wood pulps: the degree of polymerization is that the 700 cotton pulp dregs of rice mixed pulverizing back and 1-butyl by weight 1: 3,3-methyl chloride imidazole salts solution evenly mixes, at the spinning solution of 110 ℃ of dissolving formation stable homogeneous, the concentration of spinning solution is 8%;
Spinning: the bamboo charcoal slurry of configuration is accounted for the ratio of finished fiber weight 15% in bamboo charcoal wherein, be blended in the spinning solution and stir, the above-mentioned spinning solution that mixes obtains containing the sex change spinning solution of bamboo charcoal through deaeration, filtration; Via the 1-butyl, the concentration that the 3-methyl chloride imidazole salts aqueous solution is made is 20%, and temperature is 20 ℃ a coagulating bath spinning moulding.The fiber strand silk of spinning moulding through the drawing-off flow process is: silk mouthful drawing-off → air bath drawing-off → first plasticizing-bath drawing-off → second plasticizing-bath drawing-off, its draft process condition is: silk mouthful drawing-off-10%, air bath drawing-off 8%, the first plasticizing-bath drawing-off 15%, the second plasticizing-bath drawing-off 35%, obtain the 2.78dtex*51mm bamboo charcoal cellulose fiber, this bamboo charcoal cellulose fiber to do by force be 2.15cN/dtex, driedly stretch 13%.
Embodiment 3
The configuration of bamboo charcoal slurry: with particle diameter is the bamboo charcoal of 160nm, presses 0.6% of bamboo charcoal weight and add many alkyl trimethyl ammonium chlorides in bamboo charcoal, presses 0.9% of bamboo charcoal weight and adds pentasodium triphosphate of dispersing agent, adds deionized water again, is configured to 26% bamboo charcoal slurry; Place ball mill, ball milling 100min makes uniform bamboo charcoal nano slurry;
The preparation of spinning solution: with the degree of polymerization is that 1000 wood pulps, the degree of polymerization are evenly to mix with chlorination 1-(2-ethoxy)-3-methylimidazole solution after 900 bamboo pulps mixed pulverizing by weight 5: 1, at the spinning solution of 80 ℃ of dissolving formation stable homogeneous, the concentration of spinning solution is 15%;
Spinning: the bamboo charcoal slurry of configuration is accounted for the ratio of finished fiber weight 25% in bamboo charcoal wherein, be blended in the spinning solution and stir, the above-mentioned spinning solution that mixes obtains containing the sex change spinning solution of bamboo charcoal through deaeration, filtration; Make via chlorination 1-(2-ethoxy)-3-methylimidazole aqueous solution, concentration is 3%, and temperature is 60 ℃ a coagulating bath spinning moulding.The strand of spinning moulding through the drawing-off flow process is: silk mouthful drawing-off → air bath drawing-off → first plasticizing-bath drawing-off → second plasticizing-bath drawing-off, its draft process condition is: silk mouthful drawing-off-5%, air bath drawing-off 10%, the first plasticizing-bath drawing-off 9%, the second plasticizing-bath drawing-off 65%, obtain the 2.22dtex*51mm bamboo charcoal cellulose fiber, it is 2.05cN/dtex that this bamboo charcoal cellulose fiber is done by force, driedly stretches 11%.
Embodiment 4
The configuration of bamboo charcoal slurry: with particle diameter is the bamboo charcoal of 75nm, in bamboo charcoal, press 0.5% of bamboo charcoal weight and add many alkyl trimethyl ammonium chlorides, press 0.5% of bamboo charcoal weight and add dispersant dialkoxy silicane quaternary ammonium salt, add deionized water again, be configured to 18% bamboo charcoal slurry, place ball mill, ball milling 120min makes uniform bamboo charcoal nano slurry;
The preparation of spinning solution: with the degree of polymerization is that 1300 cotton stalk bark pulps, the degree of polymerization are that the 1200 cotton pulp dregs of rice are pulverized back and 1-allyl by weight 1: 8 mixing, 3-methyl chloride imidazole salts solution evenly mixes, at the spinning solution of 115 ℃ of dissolving formation stable homogeneous, the concentration of spinning solution is 10%;
Spinning: the ratio that the bamboo charcoal slurry of configuration is accounted for finished fiber weight 12% in bamboo charcoal wherein, be blended in the spinning solution and stir and obtain containing the sex change spinning solution of bamboo charcoal, via the 1-allyl, the concentration that the 3-methyl chloride imidazole salts aqueous solution is made is 15%, and temperature is 30 ℃ a coagulating bath spinning moulding.The spinning moulding strand through the drawing-off flow process is: silk mouthful drawing-off → air bath drawing-off → first plasticizing-bath drawing-off → second plasticizing-bath drawing-off, its process conditions are: silk mouthful drawing-off-1%, air bath drawing-off 5%, the first plasticizing-bath drawing-off 11%, the second plasticizing-bath drawing-off 65%, obtain the 2.22dtex*51mm bamboo charcoal cellulose fiber, this fiber to do by force be 2.65cN/dtex, driedly stretch 10%.
Embodiment 5
The configuration of bamboo charcoal slurry: with particle diameter is the bamboo charcoal of 105nm, in bamboo charcoal, press 0.1% of bamboo charcoal weight and add many alkyl trimethyl ammonium chlorides, press 0.8% of bamboo charcoal weight and add dispersant dialkoxy silicane quaternary ammonium salt, add deionized water again, be configured to 20% bamboo charcoal slurry, place ball mill, ball milling 120min makes uniform bamboo charcoal nano slurry;
The preparation of spinning solution: with the degree of polymerization is that the 800 cotton pulp dregs of rice, the degree of polymerization are that 700 bamboo pulps are pulverized back and 1-allyl by weight 5: 1 mixing, 3-methyl chloride imidazole salts is evenly mixed, at the spinning solution of 90 ℃ of dissolving formation stable homogeneous, the concentration of spinning solution is 8%;
Spinning: the ratio that the bamboo charcoal slurry of configuration is accounted for finished fiber weight 6% in bamboo charcoal wherein, be blended in the spinning solution and stir and obtain containing the sex change spinning solution of bamboo charcoal, via the 1-allyl, the concentration that the 3-methyl chloride imidazole salts aqueous solution is made is 13%, temperature is 40 ℃ a coagulating bath spinning moulding, spinning moulding through strand drawing-off flow process is: silk mouthful drawing-off → air bath drawing-off → first plasticizing-bath drawing-off → second plasticizing-bath drawing-off, its process conditions are: silk mouthful drawing-off-2%, air bath drawing-off 8%, the first plasticizing-bath drawing-off 16%, the second plasticizing-bath drawing-off 58%, obtain the 1.33dtex*38mm bamboo charcoal cellulose fiber, this fiber to do by force be 2.55cN/dtex, driedly stretch 12%.
Claims (6)
1, the manufacture method of bamboo charcoal cellulose fiber is characterized in that it comprises step:
1) bamboo charcoal slurry configuration bamboo charcoal employing particle diameter is the bamboo charcoal nano of 75～350nm, in bamboo charcoal, add dispersant, adding deionized water again, to be configured to concentration be 18%～28% uniform bamboo charcoal slurry, the bamboo charcoal slurry placed grind 90～120min and make uniform bamboo charcoal nano slurry;
2) the spinning solution preparation adopts the cellulose after pulverizing evenly to mix with ionic liquid, and dissolves the spinning solution of making stable homogeneous under 40～120 ℃ of temperature, and the spinning solution inner cellulose concentration of making is 3～15%;
3) spinning bamboo charcoal nano slurry that step 1 the is made ratio that accounts for finished fiber weight 4%～30% in bamboo charcoal be added into the spinning solution that step 2 makes and mix after make the sex change spinning solution, afterwards through the coagulating bath spinning moulding.
2, the manufacture method of bamboo charcoal cellulose fiber as claimed in claim 1 is characterized in that: add two alkyl-dimethyl ammonium chlorides or many alkyl trimethyl ammonium chlorides when described bamboo charcoal slurry disposes, addition is that 0.01%～0.6% of bamboo charcoal weight is added.
3, the manufacture method of bamboo charcoal cellulose fiber as claimed in claim 1, it is characterized in that: dispersant is polysiloxane quaternary ammonium, dialkoxy silicane quaternary ammonium salt or sodium phosphate trimer in the described bamboo charcoal slurry configuration, presses 0.1%～1.5% of bamboo charcoal weight and adds.
4, the manufacture method of bamboo charcoal cellulose fiber as claimed in claim 1, it is characterized in that: it is 1 one allyls that ionic liquid is adopted in described spinning solution preparation, 3 monomethyl chlorine imidazole salts, 1 monobutyl, the ionic liquid of 3 monomethyl chlorine imidazole salts, chlorination 1-(2-ethoxy)-3-methylimidazole, 3-methyl-N-butyl chloro-pyridine or benzyl dimethyl tetradecyl ammonium chloride.
5, the manufacture method of bamboo charcoal cellulose fiber as claimed in claim 4 is characterized in that: this bamboo charcoal cellulose fiber does not carry out the bleaching process post processing.
6, as the manufacture method of each described bamboo charcoal cellulose fiber in the claim 1 to 5, it is characterized in that: organizine mouth drawing-off behind the fiberizing, air bath drawing-off, the first plasticizing-bath drawing-off, the second plasticizing-bath drawing-off; Its process conditions are silk mouthful drawing-off-10%～0%, air bath drawing-off 0%～60%, the first plasticizing-bath drawing-off 5%～100%, the second plasticizing-bath drawing-off 5%～100%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100150367A CN100558954C (en) | 2007-06-14 | 2007-06-14 | The bamboo charcoal cellulose fiber manufacture method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100150367A CN100558954C (en) | 2007-06-14 | 2007-06-14 | The bamboo charcoal cellulose fiber manufacture method |
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| CN101270507B (en) * | 2008-05-13 | 2010-06-09 | 东华大学 | Plasticization method for cellulose |
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| CN101985781B (en) * | 2010-10-19 | 2012-03-28 | 山东海龙股份有限公司 | Preparation method of calamine cellulose fiber |
| JP5971340B2 (en) * | 2012-08-07 | 2016-08-17 | 日東紡績株式会社 | Method for producing cellulose fiber |
| CN103556274B (en) * | 2013-10-31 | 2016-04-06 | 宜宾海丝特纤维有限责任公司 | A kind of bamboo charcoal, charcoal composite viscose |
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| CN103556256B (en) * | 2013-10-31 | 2015-08-19 | 宜宾海丝特纤维有限责任公司 | A kind of bamboo charcoal, hemp stalk carbon composite viscose |
| CN103556260B (en) * | 2013-10-31 | 2015-09-16 | 宜宾海丝特纤维有限责任公司 | A kind of bamboo-carbon viscose fibre and preparation method thereof |
| CN103556263B (en) * | 2013-10-31 | 2015-09-16 | 宜宾海丝特纤维有限责任公司 | A kind of hollow bamboo charcoal viscose fiber and production technology thereof |
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| CN103556257B (en) * | 2013-10-31 | 2016-05-25 | 宜宾海丝特纤维有限责任公司 | A kind of bamboo charcoal, fruit shell carbon composite viscose fiber |
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