CN103556255A - Bamboo charcoal cellulosic fiber and preparation method thereof - Google Patents
Bamboo charcoal cellulosic fiber and preparation method thereof Download PDFInfo
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Abstract
The invention provides a bamboo charcoal cellulosic fiber and a preparation method thereof. The fiber is obtained through the following steps: mixing bamboo charcoal pulp with spinning solution which is prepared by dissolving cellulose with ionic liquid, and spinning through a coagulating bath prepared by ionic liquid aqueous solution, wherein the content of the nano bamboo charcoal is 0.1-10 percent of the weight of the finished product fiber; the bamboo charcoal pulp is prepared from the following raw materials in percentage by weight: 5-25 percent of bamboo charcoal powder, 1-2 percent of bubbleless dispersant, 1-5 percent of a thickening agent, 4-6 percent of sodium hydroxide and the balance of de-ionized water. The preparation method has the characteristics of simple process, no equipment corrosion, small environmental pollution and high production efficiency; the prepared fiber finished product has the characteristics of high strength, good adsorption performance, superior antibacterial effect, uniform and consistent color and strong color fixation; a high-quality bamboo charcoal cellulosic fiber raw material is provided for textiles.
Description
Technical field
The present invention relates to cellulose fibre production technical field, specifically, the present invention relates to a kind of cellulose fibre containing bamboo charcoal and preparation method thereof.
Background technology
The macromolecular polysaccharide that cellulose (cellulose) is comprised of glucose, water insoluble and common organic solvents, is the main component of plant cell wall.That cellulose is that occurring in nature distributes is the widest, content is maximum the more than 50% of a kind of polysaccharide ，Zhan plant kingdom carbon content.Cellulose is also natural polymer ancient, the abundantest on the earth, is inexhaustible, the natural reproducible resource that the mankind are the most valuable.Fiber crops, straw, straw, bagasse etc. are all cellulosic abundant sources.
Bamboo charcoal is that to take 3 years above high mountain mao bamboons of life be raw material, a kind of charcoal forming through nearly thousand degree high-temperature firings.Bamboo charcoal has loose structure, the fine and closely woven porous of its molecule, and quality is hard.There is very strong adsorption capacity, can purify air, eliminate peculiar smell, moisture absorption mildew-resistant, antibacterial expelling parasite.Contact the absorbing sweat that can dry with human body, promote blood circulation of human body and metabolism, fatigue-relieving.After science is refined processing, be widely used in daily life.As the textile fiber cellulose fiber that is added with active carbon is more and more subject to people's favor.
The patent application of the current bamboo charcoal cellulose fiber with regard to field of textiles has:
The patent of invention of application number 200310110113.9, a kind of bamboo-carbon viscose fibre and manufacture method thereof are disclosed, the content of bamboo charcoal is in fiber weight percentage, its ratio is X, 3% ﹤ X≤20%, include glue operation and spinning process, it is characterized in that: to bamboo charcoal, carry out selected, coarse crushing, dedusting, after removal of impurities, be crushed to the bamboo charcoal micropowder preparation section of fineness≤0.5 micron, bamboo charcoal micropowder and dispersant S are put into water and make bamboo charcoal water and milk slurry operation, in glue operation, in alkali cellulose yellow course of dissolution at the end, above-mentioned bamboo charcoal micropowder water and milk slurry is added in viscose glue, through 2-4 hour be fully uniformly mixed after grinding, making viscosity is 25-35 second, the percentage by weight of first fibre is 7.5-9.5%, ripe degree is the bamboo charcoal long fiber viscose glue of 9.2 ± 2ml, in alkali cellulose yellow course of dissolution at the end, above-mentioned bamboo charcoal micropowder water and milk slurry is added in viscose glue, through 2-4 hour be fully uniformly mixed after grinding, the bamboo charcoal staple fibre viscose glue that make viscosity and be 35 ± 3 seconds, the percentage by weight of first fibre and be 8.8 ± 0.2%, ripe degree is 10 ± 0.5ml, above-mentioned two kinds of bamboo charcoals are carried out respectively can obtaining after spinning the viscose filament yarn and the short silk that contain bamboo charcoal.
The patent of invention of application number 200610037895.1, discloses the manufacture method of bamboo-carbon viscose fibre and the bamboo-carbon viscose fibre that uses the method to manufacture, and this bamboo-carbon viscose fibre, contains bamboo charcoal micropowder and bamboo vinegar.The manufacture method of this bamboo-carbon viscose fibre, comprises glue operation and spinning process, in its glue operation, carry out the preparation of viscose solution and carry out the preparation of charcoal micro mist emulsion.In spinning process, viscose solution is mixed with described bamboo charcoal micropowder emulsion, then deliver to spinning machine and make fiber.
The patent of invention of application number 201210499127.3, a kind of production technology of bamboo-carbon viscose fibre is disclosed, comprise that step is: bamboo charcoal micropowder and porphines cobalt microparticulate are also stirred in organic solvent, obtain mixing serum, by pulp flood, squeezing and the experienced cellulose that obtains deriving from natural plants: described cellulose is joined and in described mixing serum, is dissolved and deaeration obtains spinning solution, spinning solution is extruded by Spinning pumps, in solidification liquid, solidifies and obtains bamboo-carbon viscose fibre.
Above-mentioned patent information shows, on the one hand, due to factors such as bamboo charcoal self structure, during regenerated celulose fibre that people are contained bamboo charcoal in production, what substantially adopt is the conventional production method of viscose, comprises glue operation and spinning process, take cellulose as raw material, through operations such as alkalization, yellow, aging, sulfonation, make soluble cellulose sulphonic acid ester, then be dissolved in dilute alkaline soln and make viscose glue, through wet spinning, make.Its production process is complicated, and technique is difficult to control, and water, electricity, gas consumption is large, produce a large amount of hydrogen sulfide, carbon disulfide toxic gas and waste water, not only to environment, equipment is also had to very large corrosivity simultaneously, and above-mentioned chemical reagent is also difficult for reclaiming, cost recovery is high.On the other hand, adopt the mode that adds bamboo charcoal micropowder, the contact time of bamboo charcoal micropowder and viscose glue is long, and the aggegation of dispersed particle easily occurs, and makes viscose glue be difficult for filtering, and the spinnability of viscose glue reduces, thereby the quality of fiber and performance are exerted an influence.
Summary of the invention
The present invention is intended to solve the problems of the technologies described above and bamboo charcoal cellulose fiber of a kind of good adsorption performance and preparation method thereof is provided.The method technique is simple, and to equipment non-corrosiveness, environmental pollution is little.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of bamboo charcoal cellulose fiber, it is characterized in that: this fiber is to be mixed and to obtain by spinning with the spinning solution that adopts ion liquid dissolving cellulose to make by bamboo charcoal slurry, the content of its bamboo charcoal nano is 0.1%～10% of finished fiber weight, the specific targets of described bamboo charcoal cellulose fiber finished product comprise: dry fracture strength >=2.4cN/dtex, dry elongation at break is 16～20%, dry fracture strength coefficient of variation CV≤15%, fault≤1mg/100, bamboo charcoal content 0.1～10%, antibiotic rate > 99.9%, ammonia absorption > 50%, water-fastness COLOR FASTNESS 4-5 level.
Described ionic liquid is chlorination 1-butyl-methylimidazole, 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite, 1-(2-ethoxy)-3-methylimidazole villaumite, 1-ethyl-3-methylimidazole acetate, 1-ethyl-3-methylimidazole phosphate ester salt or N-methyl-N-allyl morpholine chloride salt solvent, or the ionic liquid that is mixed of N-methyl-N-allyl morpholine villaumite and 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite.
Described bamboo charcoal slurry is made by the raw material of following weight percentage:
Bamboo charcoal powder 5～25%
Still dispersant 1～2%
Thickener 1～5%
Alkali 4～6%
Surplus is deionized water.
Described still dispersant is polyacrylic acid sodium salt; Described thickener is cellulose thickener; Described alkali is NaOH.
Described cellulose thickener is selected from hydroxyethylcellulose (HEC), hydroxypropyl methylcellulose (HPMC), carboxymethyl cellulose (CMC) or ethylhydroxyethylcellulose (EHEC).
The viscosity of described bamboo charcoal slurry is 30～70s, and alkalinity is 4～6%, the particle diameter≤0.8 μ m of bamboo carbon powder particle.
The preparation method of described bamboo charcoal cellulose fiber comprises following processing step:
The preparation of A bamboo charcoal slurry
In deionized water, add after still dispersant, bamboo charcoal powder, thickener, alkali, through stirring, grinding evenly and get final product;
The preparation of B spinning solution
Cellulose powder is broken into the micro mist of particle diameter≤0.1 μ m, dissolves the spinning solution of making stable homogeneous with ionic liquid at 80～150 ℃ of temperature, the spinning solution inner cellulose concentration of making is 8～12%; Described cellulose is selected from a kind of or its combination in bamboo pulp, Cotton Pulp, hemp dissolving pulp, straw pulp, wood pulps;
C spinning
The ratio that the bamboo charcoal slurry that steps A is made accounts for finished fiber weight 0.1%～10% in bamboo charcoal is added in the spinning solution that step B makes, and carries out deaeration, filtration after mixing, then through coagulating bath spinning moulding; Fiber strand silk after moulding makes bamboo charcoal cellulose fiber finished product through drawing-off, post processing and oven dry.
Described coagulating bath is for adopting chlorination 1-butyl-methylimidazole, 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite, 1-(2-ethoxy)-3-methylimidazole villaumite, 1-ethyl-3-methylimidazole acetate, 1-ethyl-3-methylimidazole phosphate ester salt or N-methyl-N-allyl morpholine villaumite, or the ionic liquid that is mixed of N-methyl-N-allyl morpholine villaumite and 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite, the temperature of making is the ionic liquid aqueous solution that 0～90 ℃, concentration are≤30%.
In described spinning moulding process, coagulation bath temperature is controlled at 40～50 ℃, spins speed control built in 40～70m/mim.
The drawing-off flow process of the fiber strand silk after described moulding is: the drawing-off of organizine mouth, 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%, first plasticizing-bath drawing-off the 5%～100%, second plasticizing-bath drawing-off 5%～100%.
The invention has the advantages that:
1, adopt ionic liquid to dissolve and make spinning solution cellulose, its production process is polluted minimum, in production process, do not produce chemical change, toxicity is little, solvent is recyclable uses again, have that production process is short, energy consumption is low, without remarkable advantages such as waste water and gas environmental pollutions, solved to a great extent the pollution problem producing in traditional production process of viscose fiber.
2, adopting viscosity is 30～70s, and alkalinity is 4～6%, the bamboo charcoal slurry of the particle diameter≤0.8 μ m of bamboo carbon powder particle, and spinnability is high, has fully guaranteed quality and the performance requirement of bamboo-carbon fibre.
3, by bamboo charcoal slurry with through ionic liquid, cellulose is dissolved to the spinning solution of the making spinning that is mixed, can greatly improve the production efficiency of fiber, in aftertreatment technology, reduced the bleaching process in traditional adhering process simultaneously, avoided the destruction of antibacterial substance in bamboo charcoal, guaranteed the desired function of bamboo-carbon fibre finished product, there is natural antibacterial bacteriostatic, the absorbing sweat that dries, the function that eliminates the unusual smell, for making textiles, provide colory bamboo charcoal cellulose fiber raw material.
4, in spinning moulding process, coagulation bath temperature is controlled to 40～50 ℃, spin speed control built in 40～70m/mim, can effectively prevent the decline of bath surface viscosity, improve the rheological property of melt, thereby fully improved the uniformity that bamboo-carbon powder distributes.
5, the dry fracture strength >=2.4cN/dtex of bamboo charcoal cellulose fiber finished product of the present invention, dry elongation at break is 16～20%, dry fracture strength coefficient of variation CV≤15%, fault≤1mg/100, bamboo charcoal content 0.1～10%, antibiotic rate > 99.9%, ammonia absorption > 50%, water-fastness COLOR FASTNESS 4-5 level, have that intensity is high, absorption property good, antibacterial effect is excellent, color and luster uniformity, speciality that fixation is strong, thereby the dyeing in later stage and textile process performance good.
The specific embodiment
embodiment 1
A kind of bamboo charcoal cellulose fiber, this fiber is to be mixed and to obtain by spinning with the spinning solution that adopts ion liquid dissolving cellulose to make by bamboo charcoal slurry, the content of its bamboo charcoal nano is 5% of finished fiber weight, the specific targets of described bamboo charcoal cellulose fiber finished product comprise: dry fracture strength 2.5cN/dtex, dry elongation at break 18%, dry fracture strength coefficient of variation CV 13%, fault≤1mg/100, bamboo charcoal content 5%, antibiotic rate > 99.9%, ammonia absorption > 50%, water-fastness COLOR FASTNESS 4-5 level.
Described ionic liquid is the ionic liquid that is mixed of chlorination 1-butyl-methylimidazole and 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite.
Described bamboo charcoal slurry is made by the raw material of following weight percentage:
Bamboo charcoal powder 15%
Still dispersant 1%
Thickener 3%
Alkali 5%
Surplus is deionized water.
Described still dispersant is polyacrylic acid sodium salt; Described thickener is hydroxyethylcellulose (HEC); Described alkali is NaOH.
The viscosity of described bamboo charcoal slurry is 45s, and alkalinity is 5%, the particle diameter≤0.8 μ m of bamboo carbon powder particle.
The preparation method of described bamboo charcoal cellulose fiber comprises following processing step:
The preparation of A bamboo charcoal slurry
In deionized water, add after still dispersant, bamboo charcoal powder, thickener, alkali, through stirring, grinding evenly and get final product;
The preparation of B spinning solution
Cellulose powder is broken into the micro mist of particle diameter≤0.1 μ m, dissolves the spinning solution of making stable homogeneous with ionic liquid at 100 ℃ of temperature, the spinning solution inner cellulose concentration of making is 10%; Described cellulose is comprised of by the weight ratio of 5:1 bamboo pulp and Cotton Pulp;
C spinning
The ratio that the bamboo charcoal slurry that steps A is made accounts for finished fiber weight 5% in bamboo charcoal is added in the spinning solution that step B makes, and carries out deaeration, filtration after mixing, then through coagulating bath spinning moulding; Fiber strand silk after moulding makes bamboo charcoal cellulose fiber finished product through drawing-off, post processing and oven dry.
Described coagulating bath for the temperature that adopts chlorination 1-butyl-methylimidazole and 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite to make be the ionic liquid aqueous solution that 60 ℃, concentration are 10%.
In described spinning moulding process, coagulation bath temperature is controlled at 40 ℃, spins speed control built in 50m/mim.
The drawing-off flow process of the fiber strand silk after described moulding is: the drawing-off of organizine mouth, 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%, air bath drawing-off 10%, the first plasticizing-bath drawing-off 20%, the second plasticizing-bath drawing-off 45%.
embodiment 2
A kind of bamboo charcoal cellulose fiber, this fiber is to be mixed and to obtain by spinning with the spinning solution that adopts ion liquid dissolving cellulose to make by bamboo charcoal slurry, the content of its bamboo charcoal nano is 0.1% of finished fiber weight, the specific targets of described bamboo charcoal cellulose fiber finished product comprise: dry fracture strength 2.4cN/dtex, dry elongation at break 20%, dry fracture strength coefficient of variation CV 14.5%, fault≤1mg/100, bamboo charcoal content 0.1%, antibiotic rate > 99.9%, ammonia absorption > 50%, water-fastness COLOR FASTNESS 4-5 level.
Described ionic liquid is 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite and 1-(2-ethoxy) ionic liquid that is mixed of-3-methylimidazole villaumite.
Described bamboo charcoal slurry is made by the raw material of following weight percentage:
Bamboo charcoal powder 5%
Still dispersant 1%
Thickener 1%
Alkali 4%
Surplus is deionized water.
Described still dispersant is polyacrylic acid sodium salt; Described thickener is hydroxypropyl methylcellulose (HPMC); Described alkali is NaOH.
The viscosity of described bamboo charcoal slurry is 30s, and alkalinity is 4%, the particle diameter≤0.8 μ m of bamboo carbon powder particle.
The preparation method of described bamboo charcoal cellulose fiber comprises following processing step:
The preparation of A bamboo charcoal slurry
In deionized water, add after still dispersant, bamboo charcoal powder, thickener, alkali, through stirring, grinding evenly and get final product;
The preparation of B spinning solution
Cellulose powder is broken into the micro mist of particle diameter≤0.1 μ m, dissolves the spinning solution of making stable homogeneous with ionic liquid at 80 ℃ of temperature, the spinning solution inner cellulose concentration of making is 8%; Described cellulose is comprised of by weight 2:5 hemp dissolving pulp and wood pulps;
C spinning
The ratio that the bamboo charcoal slurry that steps A is made accounts for finished fiber weight 0.1% in bamboo charcoal is added in the spinning solution that step B makes, and carries out deaeration, filtration after mixing, then through coagulating bath spinning moulding; Fiber strand silk after moulding makes bamboo charcoal cellulose fiber finished product through drawing-off, post processing and oven dry.
Described coagulating bath is for adopting chlorination 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite and 1-(2-ethoxy)-temperature that 3-methylimidazole villaumite is made is the ionic liquid aqueous solution that 30 ℃, concentration are 15%.
In described spinning moulding process, coagulation bath temperature is controlled at 50 ℃, spins speed control built in 70m/mim.
The drawing-off flow process of the fiber strand silk after described moulding is: the drawing-off of organizine mouth, air bath drawing-off, the first plasticizing-bath drawing-off, the second plasticizing-bath drawing-off; Its process conditions are silk mouthful drawing-off-5%, air bath drawing-off 30%, the first plasticizing-bath drawing-off 18%, the second plasticizing-bath drawing-off 50%.
embodiment 3
A kind of bamboo charcoal cellulose fiber, this fiber is to be mixed and to obtain by spinning with the spinning solution that adopts ion liquid dissolving cellulose to make by bamboo charcoal slurry, the content of its bamboo charcoal nano is 10% of finished fiber weight, the specific targets of described bamboo charcoal cellulose fiber finished product comprise: dry fracture strength 2.42cN/dtex, dry elongation at break 16%, dry fracture strength coefficient of variation CV 15%, fault≤1mg/100, bamboo charcoal content 10%, antibiotic rate > 99.9%, ammonia absorption > 50%, water-fastness COLOR FASTNESS 4-5 level.
Described ionic liquid is the ionic liquid that is mixed of N-methyl-N-allyl morpholine villaumite and 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite.
Described bamboo charcoal slurry is made by the raw material of following weight percentage:
Bamboo charcoal powder 25%
Still dispersant 2%
Thickener 5%
Alkali 4%
Surplus is deionized water.
Described still dispersant is polyacrylic acid sodium salt; Described thickener is carboxymethyl cellulose (CMC); Described alkali is NaOH.
The viscosity of described bamboo charcoal slurry is 70s, and alkalinity is 4%, the particle diameter≤0.8 μ m of bamboo carbon powder particle.
The preparation method of described bamboo charcoal cellulose fiber comprises following processing step:
The preparation of A bamboo charcoal slurry
In deionized water, add after still dispersant, bamboo charcoal powder, thickener, alkali, through stirring, grinding evenly and get final product;
The preparation of B spinning solution
Cellulose powder is broken into the micro mist of particle diameter≤0.1 μ m, dissolves the spinning solution of making stable homogeneous with ionic liquid at 150 ℃ of temperature, the spinning solution inner cellulose concentration of making is 12%; Described cellulose is comprised of by the weight ratio of 1:4 bamboo pulp and wood pulps;
C spinning
The ratio that the bamboo charcoal slurry that steps A is made accounts for finished fiber weight 10% in bamboo charcoal is added in the spinning solution that step B makes, and carries out deaeration, filtration after mixing, then through coagulating bath spinning moulding; Fiber strand silk after moulding makes bamboo charcoal cellulose fiber finished product through drawing-off, post processing and oven dry.
Described coagulating bath for the temperature that adopts the ionic liquid that is mixed of N-methyl-N-allyl morpholine villaumite and 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite to make be the ionic liquid aqueous solution that 90 ℃, concentration are 30%.
In described spinning moulding process, coagulation bath temperature is controlled at 50 ℃, spins speed control built in 40m/mim.
The drawing-off flow process of the fiber strand silk after described moulding is: the drawing-off of organizine mouth, air bath drawing-off, the first plasticizing-bath drawing-off, the second plasticizing-bath drawing-off; Its process conditions are silk mouthful drawing-off 0%, air bath drawing-off 60%, the first plasticizing-bath drawing-off 30%, the second plasticizing-bath drawing-off 70%.
embodiment 4
A kind of bamboo charcoal cellulose fiber, this fiber is to be mixed and to obtain by spinning with the spinning solution that adopts ion liquid dissolving cellulose to make by bamboo charcoal slurry, the content of its bamboo charcoal nano is 0.5% of finished fiber weight, the specific targets of described bamboo charcoal cellulose fiber finished product comprise: dry fracture strength 2.55cN/dtex, dry elongation at break 18.5%, dry fracture strength coefficient of variation CV 14.1%, fault≤1mg/100, bamboo charcoal content 0.5%, antibiotic rate > 99.9%, ammonia absorption > 50%, water-fastness COLOR FASTNESS 4-5 level.
Described ionic liquid is chlorination 1-butyl-methylimidazole and 1-(2-ethoxy)-3-methylimidazole villaumite, the ionic liquid that is mixed.
Described bamboo charcoal slurry is made by the raw material of following weight percentage:
Bamboo charcoal powder 10%
Still dispersant 1.5%
Thickener 2.5%
Alkali 6%
Surplus is deionized water.
Described still dispersant is polyacrylic acid sodium salt; Described thickener is ethylhydroxyethylcellulose (EHEC); Described alkali is NaOH.
The viscosity of described bamboo charcoal slurry is 50s, and alkalinity is 6%, the particle diameter≤0.8 μ m of bamboo carbon powder particle.
The preparation method of described bamboo charcoal cellulose fiber comprises following processing step:
The preparation of A bamboo charcoal slurry
In deionized water, add after still dispersant, bamboo charcoal powder, thickener, alkali, through stirring, grinding evenly and get final product;
The preparation of B spinning solution
Cellulose powder is broken into the micro mist of particle diameter≤0.1 μ m, dissolves the spinning solution of making stable homogeneous with ionic liquid at 120 ℃ of temperature, the spinning solution inner cellulose concentration of making is 9%; Described cellulose is comprised of by the weight ratio of 1:2:3 wood pulps, Cotton Pulp, straw pulp;
C spinning
The ratio that the bamboo charcoal slurry that steps A is made accounts for finished fiber weight 0.5% in bamboo charcoal is added in the spinning solution that step B makes, and carries out deaeration, filtration after mixing, then through coagulating bath spinning moulding; Fiber strand silk after moulding makes bamboo charcoal cellulose fiber finished product through drawing-off, post processing and oven dry.
Described coagulating bath is for adopting chlorination 1-butyl-methylimidazole and 1-(2-ethoxy)-temperature that 3-methylimidazole villaumite is made is the ionic liquid aqueous solution that 10 ℃, concentration are 10%.
In described spinning moulding process, coagulation bath temperature is controlled at 45 ℃, spins speed control built in 65m/mim.
The drawing-off flow process of the fiber strand silk after described moulding is: the drawing-off of organizine mouth, air bath drawing-off, the first plasticizing-bath drawing-off, the second plasticizing-bath drawing-off; Its process conditions are silk mouthful drawing-off-1%, air bath drawing-off 8%, the first plasticizing-bath drawing-off 15%, the second plasticizing-bath drawing-off 45%.
embodiment 5
A kind of bamboo charcoal cellulose fiber, this fiber is to be mixed and to obtain by spinning with the spinning solution that adopts ion liquid dissolving cellulose to make by bamboo charcoal slurry, the content of its bamboo charcoal nano is 1% of finished fiber weight, the specific targets of described bamboo charcoal cellulose fiber finished product comprise: dry fracture strength 2.47cN/dtex, dry elongation at break 18.5%, dry fracture strength coefficient of variation CV≤13.8%, fault≤1mg/100, bamboo charcoal content 1%, antibiotic rate > 99.9%, ammonia absorption > 50%, water-fastness COLOR FASTNESS 4-5 level.
Described ionic liquid is chlorination 1-butyl-methylimidazole.
Described bamboo charcoal slurry is made by the raw material of following weight percentage:
Bamboo charcoal powder 12%
Still dispersant 2%
Thickener 3.5%
Alkali 5%
Surplus is deionized water.
Described still dispersant is polyacrylic acid sodium salt; Described thickener is carboxymethyl cellulose (CMC); Described alkali is NaOH.
The viscosity of described bamboo charcoal slurry is 40s, and alkalinity is 5%, the particle diameter≤0.8 μ m of bamboo carbon powder particle.
The preparation method of described bamboo charcoal cellulose fiber comprises following processing step:
The preparation of A bamboo charcoal slurry
In deionized water, add after still dispersant, bamboo charcoal powder, thickener, alkali, through stirring, grinding evenly and get final product;
The preparation of B spinning solution
Cellulose powder is broken into the micro mist of particle diameter≤0.1 μ m, dissolves the spinning solution of making stable homogeneous with ionic liquid at 110 ℃ of temperature, the spinning solution inner cellulose concentration of making is 11.5%; Described cellulose is comprised of by weight 1:1 Cotton Pulp and wood pulps;
C spinning
The ratio that the bamboo charcoal slurry that steps A is made accounts for finished fiber weight 1% in bamboo charcoal is added in the spinning solution that step B makes, and carries out deaeration, filtration after mixing, then through coagulating bath spinning moulding; Fiber strand silk after moulding makes bamboo charcoal cellulose fiber finished product through drawing-off, post processing and oven dry.
Described coagulating bath for the temperature that adopts chlorination 1-butyl-methylimidazole to make be the ionic liquid aqueous solution that 0 ℃, concentration are 15%.
In described spinning moulding process, coagulation bath temperature is controlled at 47 ℃, spins speed control built in 58m/mim.
The drawing-off flow process of the fiber strand silk after described moulding is: the drawing-off of organizine mouth, air bath drawing-off, the first plasticizing-bath drawing-off, the second plasticizing-bath drawing-off; Its process conditions are silk mouthful drawing-off-2%, air bath drawing-off 20%, the first plasticizing-bath drawing-off 17%, the second plasticizing-bath drawing-off 55%.
Claims (10)
1. a bamboo charcoal cellulose fiber, it is characterized in that: this fiber is to be mixed and to obtain by spinning with the spinning solution that adopts ion liquid dissolving cellulose to make by bamboo charcoal slurry, the content of its bamboo charcoal nano is 0.1%～10% of finished fiber weight, the specific targets of described bamboo charcoal cellulose fiber finished product comprise: dry fracture strength >=2.4cN/dtex, dry elongation at break is 16～20%, dry fracture strength coefficient of variation CV≤15%, fault≤1mg/100, bamboo charcoal content 0.1～10%, antibiotic rate > 99.9%, ammonia absorption > 50%, water-fastness COLOR FASTNESS 4-5 level.
2. bamboo charcoal cellulose fiber according to claim 1, it is characterized in that: described ionic liquid is chlorination 1-butyl-methylimidazole, 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite, 1-(2-ethoxy)-3-methylimidazole villaumite, 1-ethyl-3-methylimidazole acetate, 1-ethyl-3-methylimidazole phosphate ester salt or N-methyl-N-allyl morpholine chloride salt solvent, or the ionic liquid that is mixed of N-methyl-N-allyl morpholine villaumite and 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite.
3. bamboo charcoal cellulose fiber according to claim 1, is characterized in that: described bamboo charcoal slurry is made by the raw material of following weight percentage:
Bamboo charcoal powder 5～25%
Still dispersant 1～2%
Thickener 1～5%
Alkali 4～6%
Surplus is deionized water.
4. bamboo charcoal cellulose fiber according to claim 3, is characterized in that: described still dispersant is polyacrylic acid sodium salt; Described thickener is cellulose thickener; Described alkali is NaOH.
5. bamboo charcoal cellulose fiber according to claim 4, is characterized in that: described cellulose thickener is selected from hydroxyethylcellulose, hydroxypropyl methylcellulose, carboxymethyl cellulose or ethylhydroxyethylcellulose.
6. according to the bamboo charcoal cellulose fiber described in claim 1 or 3, it is characterized in that: the viscosity of described bamboo charcoal slurry is 30～70s, and alkalinity is 4～6%, the particle diameter≤0.8 μ m of bamboo carbon powder particle.
7. the preparation method of bamboo charcoal cellulose fiber according to claim 1, is characterized in that processing step is as follows:
The preparation of A bamboo charcoal slurry
In deionized water, add after still dispersant, bamboo charcoal powder, thickener, alkali, through stirring, grinding evenly and get final product;
The preparation of B spinning solution
Cellulose powder is broken into the micro mist of particle diameter≤0.1 μ m, dissolves the spinning solution of making stable homogeneous with ionic liquid at 80～150 ℃ of temperature, the spinning solution inner cellulose concentration of making is 8～12%; Described cellulose is selected from a kind of or its combination in bamboo pulp, Cotton Pulp, hemp dissolving pulp, straw pulp, wood pulps;
C spinning
The ratio that the bamboo charcoal slurry that steps A is made accounts for finished fiber weight 0.1%～10% in bamboo charcoal is added in the spinning solution that step B makes, and carries out deaeration, filtration after mixing, then through coagulating bath spinning moulding; Fiber strand silk after moulding makes bamboo charcoal cellulose fiber finished product through drawing-off, post processing and oven dry.
8. the preparation method of bamboo charcoal cellulose fiber according to claim 7, it is characterized in that: described coagulating bath is for adopting chlorination 1-butyl-methylimidazole, 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite, 1-(2-ethoxy)-3-methylimidazole villaumite, 1-ethyl-3-methylimidazole acetate, 1-ethyl-3-methylimidazole phosphate ester salt or N-methyl-N-allyl morpholine villaumite, or the temperature made of the ionic liquid that is mixed of N-methyl-N-allyl morpholine villaumite and 3-methyl isophthalic acid-alkene phenyl imidazoles villaumite is the ionic liquid aqueous solution that 0～90 ℃, concentration are≤30%.
9. according to the preparation method of the bamboo charcoal cellulose fiber described in claim 7 or 8, it is characterized in that: in described spinning moulding process, coagulation bath temperature is controlled at 40～50 ℃, spins speed control built in 40～70m/mim.
10. the preparation method of bamboo charcoal cellulose fiber according to claim 7, is characterized in that: the drawing-off flow process of the fiber strand silk after described moulding is: the drawing-off of organizine mouth, 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%, first plasticizing-bath drawing-off the 5%～100%, second plasticizing-bath drawing-off 5%～100%.
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| CN109332177A (en) * | 2018-08-22 | 2019-02-15 | 浦江县顺光科技有限公司 | Chrysanthemum high-efficiency dynamic deashing cleaner |
| CN110219066A (en) * | 2019-05-09 | 2019-09-10 | 海盐县硕创服装研究所 | The antistatic bamboo charcoal fiber of underwear |
| CN115961368A (en) * | 2022-11-30 | 2023-04-14 | 新乡化纤股份有限公司 | Ionic liquid method fungus grass regenerated cellulose fiber and preparation method thereof |
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| CN108754659B (en) * | 2018-06-04 | 2021-02-12 | 汕头市欣和棉麻纺织有限公司 | Artemisinin cellulose fiber and preparation method thereof |
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| CN110219066A (en) * | 2019-05-09 | 2019-09-10 | 海盐县硕创服装研究所 | The antistatic bamboo charcoal fiber of underwear |
| CN115961368A (en) * | 2022-11-30 | 2023-04-14 | 新乡化纤股份有限公司 | Ionic liquid method fungus grass regenerated cellulose fiber and preparation method thereof |
| CN115961368B (en) * | 2022-11-30 | 2023-09-12 | 新乡化纤股份有限公司 | Ionic liquid method fungus grass regenerated cellulose fiber and preparation method thereof |
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