CN101104958A - Viscose fiber and its preparing method - Google Patents
Viscose fiber and its preparing method Download PDFInfo
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Abstract
The invention provides viscose fiber made from industrial hemp as raw material and the preparation method thereof. The method comprises material preparation, cutting, flash explosion, pre-hydrolysis, boiling, selection, chlorination, bleaching, acid treatment, refining, paper-making, rolling mill, dipping, squeezing, crushing, curing, yellowing, dissolution, mixing, filtration, debubbling, filtration, spinning, cutting, refining, drying, and packaging steps. The viscose fiber made from industrial hemp as raw material is soft and smooth, has strong moisture-absorbing and wetting abilities and good antibacterial effect, and is easy to dye; and is a novel fiber raw material for textile industry.
Description
Technical field
The present invention relates to the industrial hemp is viscose of raw material production and preparation method thereof, belongs to the chemical fibre technical field.
Technical background
Viscose is as a kind of textile raw material, and its traditional production is raw material with native celluloses such as timber, cotton linters all, a kind of broad-spectrum regenerated celulose fibre that makes through a series of processing procedures such as boiling, acid treatment, bleaching.Along with the worsening shortages of traditional raw materials such as timber, cotton linter, production cost sharply rises, and therefore, it is imperative that new raw material is explored in exploitation.Simultaneously, China's functional fiber content accounts for fiber insufficient total amount 10%, main dependence on import, and it is few especially to have a fiber of natural antibacterial, moisture absorbing and sweat releasing, the noise reduction of suction ripple, uvioresistant, features such as corrosion-resistant, development function chemical fibre dimension is the new direction of fiber development.
Chinese fiber crops are one of China crops the earliest, and archaeological materials show that China is the area of taming plantation the earliest and utilizing Chinese fiber crops, apart from modern about 5000-6000.Chinese fiber crops have long plantation history, mainly comprise fiber Chinese fiber crops, medicinal Chinese fiber crops and wild Chinese fiber crops three major types.Chinese fiber crops have different appellations in China different regions, as hemp, fire fiber crops, cold fiber crops, stalwart fiber crops and hemp etc.In the world tetrahydrocannabinol (THC) content is lower than 0.3% kind and is called industrial hemp (Industrial Hemp), be higher than 0.3% be called medicinal and the drugs hemp.Chinese fiber crops once were one of the fiber wanted of necessary for human and most important source of food in history, be widely used in purposes such as rope, canvas, textile garment, paper, food and oil plant, indelible huge contribution has been made in navigation, military affairs, economy and social development.But viscose that is feedstock production with the industrial hemp and preparation method thereof does not appear in the newspapers as yet.
Summary of the invention
Primary and foremost purpose of the present invention is to provide a kind of viscose.Described viscose not only has the characteristic of common viscose fiber, and has features such as antibacterial and deodorizing, moisture absorbing and sweat releasing, uvioresistant.It is raw material that the present invention adopts industrial hemp, has alleviated the nervous situation of raw materials such as cotton linter, timber, makes full use of fast growing, the abundant industrial hemp resource of fiber content.The performance of prepared viscose is as follows: the dried fracture strength of described viscose: 〉=2.2CN/dtex; Wet breaking strength: 〉=1.3CN/dtex; Dried elongation at break: 〉=18.0%; Line density deviation ratio: ± 7.00%; Length variation rate: ± 9.0%; Overcut fibre :≤1.0%; Over-length fibre :≤20.0mg/100g; Residual sulfur content :≤15.0mg/100g; Fault≤25mg/100g; Do the strong coefficient of variation≤18.00%.
Another object of the present invention is to provide a kind of preparation method of industrial hemp viscose, and this method is carried out the preparation of viscose, the method simple possible at this special regenerated celulose fibre raw material of industrial hemp.
To achieve these goals, the technical solution used in the present invention is:
A kind of viscose, described viscose are feedstock production with the industrial hemp, the dried fracture strength of described viscose: 〉=2.2CN/dtex; Wet breaking strength: 〉=1.3CN/dtex; Dried elongation at break: 〉=18.0%; Line density deviation ratio: ± 7.00%; Length variation rate: ± 9.0%; Overcut fibre :≤1.0%; Over-length fibre :≤20.0mg/100g; Residual sulfur content :≤15.0mg/100g; Fault≤25mg/100g; Do the strong coefficient of variation≤18.00%.
Described raw material is the bast part through the industrial hemp stalk that comes unstuck or do not come unstuck, and perhaps the full stalk of industrial hemp perhaps removes bast industrial hemp stalk partly.
The preparation method of described viscose, comprise get the raw materials ready, blank, boiling, selected, chlorination, bleaching, acid treatment, alkali refining, manufacture paper with pulp, flood, squeezing, pulverizing, experienced, yellow, dissolving, spinning, refining, drying, packing, before boiling, also process is dodged quick-fried process after carrying out blank.
Described sudden strain of a muscle is quick-fried to be specially: the material of chopping is placed on dodges in the quick-fried machine, adopt the steam humidification pressurization, when pressure reaches 0.6-1.2Mpa, keep after 8-15 minute the moment release of pressure.
In the method for the present invention, before the dipping, utilize kneading or grinding leaser to rub pulp with the hands mill and divide silk after manufacturing paper with pulp, the constant volume Weight control that makes raw material is at 120～150g/l, and wherein the rotating speed of kneading or grinding leaser is 250-500r/min.
The method of prehydrolysis-kraft cooking that the present invention adopts is specially: earlier in liquor ratio 1: 4～6, under the condition that holding temperature is 150～175 ℃ with the raw material prehydrolysis temperature retention time got ready 60～120 minutes; Be 1: 3～5 in liquor ratio then, alkali charge is with Na
2The O meter under the condition of sulphidity 5～25%, is warming up to 130～150 ℃, temperature retention time 60～90 minutes to over dry material quantity 20～40%; Be warming up to 155～170 ℃ afterwards again, temperature retention time 90～180 minutes.
The present invention also can adopt alkaline cooking, and its concrete grammar is: in liquor ratio is 1: 3.5～5.5, and alkali charge is with Na
2Under O meter 18～25% the condition to the over dry material quantity, be warming up to 160～175 ℃ after temperature retention time 120～180 minutes.
The quality of the pulp of gained is after described manufacturing paper with pulp: alpha cellulose 〉=90%, viscosity 〉=8.0mPas, whiteness 〉=60%, moisture 9.0 ± 0.5%, iron branch≤140ppm.
Described dipping is specially: the industrial hemp pulp that will carry out after the branch silk through kneading or grinding leaser is 220-260g/l in concentration, and temperature is dipping 10-25 minute in 40-60 ℃ the NaOH solution.
In the method for the present invention, before after selected, manufacturing paper with pulp, also comprise the process of alkali refining; Described alkali refining is specially: the concentration of NaOH is 130-200g/l, and the time is 60-120 minute, and alkali refining is starched dense 6-12%, and the temperature of alkali refining is 20-35 ℃.
Bleaching described in the present invention and acid treatment are:
Once bleach in bleaching machine earlier, the oven dry stock chlorine dosage is 1-3% relatively, the dense 4-6% of bleached pulp, temperature 39-50 ℃, the time is 40-90 minute, and bleaching is carried out acid treatment after finishing, the hydrochloric acid consumption is 2-5% to oven dry stock in the acid treatment, and the time is 20-60 minute, and temperature is a normal temperature; Carry out the secondary bleaching afterwards, the oven dry stock chlorine dosage is 0.2%-0.5% relatively, and the time is 20-40 minute, and temperature is a normal temperature, and bleaching is carried out acid treatment after finishing, and the hydrochloric acid consumption is 1-3% to oven dry stock in the acid treatment, and the time is 10-30 minute.
Yellow condition described in the present invention is: CS
2The 25-40% of the relative methylcellulose content of addition, the time is 90-130 minute, the yellow initial temperature is 19-20 ℃, warm 25-32 ℃ eventually of yellow, vacuum :≤-0.08Mpa.
Spinning described in the present invention is specially: carry out the consisting of of acid bath liquid at the spinning machine: sulfuric acid 110-130g/l, and sodium sulphate 280-310g/l, zinc sulfate 10-15g/l, acid bath drop＜5g/l, temperature is 45-55 ℃.
Hemp is the annual herb plant, and China's annual production ranks first in the world, and its content of cellulose reaches 50-60%, is a kind of desirable novel pulping raw material.Industrial hemp used in the present invention can be through bast part that come unstuck or that do not come unstuck, can be big whole hemp stalk also, or removes the hemp stalk of bast part, to require it be normal mature, do not have go mouldy, do not have rotten.Adopting industrial hemp is that to prepare viscose be one of key of the present invention to raw material.
Specifically, preparation method of the present invention is:
(1) get the raw materials ready, blank:
Raw material is got the raw materials ready, blank, is washed material etc., removing impurity such as silt, chip, for after the boiling step prepare these conventional steps that all are absolutely necessary, and this also is known to those skilled in the art.
(2) sudden strain of a muscle is quick-fried
Sudden strain of a muscle of the present invention is quick-fried to be specially: the material of chopping is dodged in the quick-fried machine, adopt the steam humidification pressurization, when pressure reaches 0.6-1.2Mpa, keep after 10 minutes the moment release of pressure.Adopted and dodged quick-fried method, cellulosic percentage composition contained in the industrial hemp is improved, make industrial hemp through the quick-fried processing of sudden strain of a muscle the time, play expanded effect, and impurity such as some lignin have tentatively been removed, for sufficient preparation has been carried out in the infiltration of cooking liquor in the boiling afterwards.
(3) boiling:
Boiling of the present invention can be adopted the prehydrolytic sulfate process boiling, also can adopt alkaline cooking.
When adopting the prehydrolytic sulfate process boiling, be 1 in liquor ratio earlier: 4-6, holding temperature is under 150-175 ℃ the condition, to carry out prehydrolysis 60-120 branch; After hydrolysis finished, at liquor ratio 1: 3-5, total alkali content was (with Na
2The O meter) to over dry raw material 20-40%, carry out kraft cooking under the condition of sulphidity 5-25%, boiling is incubated 130-150 ℃ for the first time, and temperature retention time 60-90 minute, holding temperature was 155-170 ℃ for the second time, temperature retention time 90-180 minute.
When adopting alkaline cooking, be 1 in liquor ratio: 3.5-5.5, total alkali content is (with Na
2O meter) is warming up to 160-175 ℃, insulation 120-180 branch under the condition to the 20-40% of over dry raw material.
(4) selected:
This step comprises that the slurry to the boiling gained washs, desanding, concentrate etc., removing foreign material such as silt, irony, and is concentrated into technological requirement by thickener, is those skilled in the art's technology in common knowledge.
(5) chlorination, bleaching, acid treatment:
Once bleach in bleaching machine earlier, the oven dry stock chlorine dosage is 1-3% relatively, the dense 4-6% of bleached pulp, temperature 39-50 ℃, the time is 40-90 minute, and bleaching is carried out acid treatment after finishing, the hydrochloric acid consumption is 2-5% to oven dry stock in the acid treatment, and the time is 20-60 minute, and temperature is a normal temperature; Carry out the secondary bleaching afterwards, the oven dry stock chlorine dosage is 0.2%-0.5% relatively, and the time is 20-40 minute, and temperature is a normal temperature, and bleaching is carried out acid treatment after finishing, and the hydrochloric acid consumption is 1-3% to oven dry stock in the acid treatment, and the time is 10-30 minute.
(6) alkali refining:
This step comprises that the slurry to gained after the acid treatment carries out desanding, concentrates, and can carry out desanding in desander, removes sand after thickener makes concentration of slurry be concentrated into 3.0-3.5%.Described alkali refining is specially: concentration sodium hydroxide is 130-200g/l, and the time is 60-120 minute, and alkali refining is starched dense 6-12%, and the temperature of alkali refining is 20-35 ℃.
(7) manufacture paper with pulp:
Carry out in pulp machine, concrete technical conditions can be quantitative 500-800g/m
2, moisture 8.5-11.5%.
(8) rub mill with the hands:
Utilize kneading or grinding leaser to rub hemp dissolving pulp with the hands mill and divide silk, the constant volume Weight control that makes raw material is at 120-150g/l, and wherein the rotating speed of kneading or grinding leaser is 250-500r/min.
(9) dipping:
Carry out in treating tank, the hemp dissolving pulp that will carry out after the branch silk through kneading or grinding leaser is dipping 10-25 minute in 30-50 ℃ the aqueous slkali for the 220-260g/l temperature in concentration.Because pulp has divided silk before slurry is flooded, so alkali lye is penetrated into the inside of pulp soon when flooding in this step, fully react with the cellulose in the pulp, Jin Zi time just shortens like this, the temperature also temperature than dipping in the general viscose preparation is low, thereby has improved production efficiency.
(10) squeezing, pulverizing:
This step is handled according to the method for routine.Squeezing is carried out in squeezer, and concrete technical conditions are: the fine content 34-37% of first, caustic soda content 12-15%.The step of pulverizing after the squeezing.
(11) experienced, yellow:
Experiencedly carry out in experienced drum, actual conditions is: temperature 30-60 ℃, and time 30-90 minute, viscosity 0.005-0.007MPaS.Yellow is carried out in xanthating machine, and actual conditions is: the carbon disulfide consumption is the 26-45% of alkali cellulose weight, and the temperature at end of yellow is 28-33 ℃, and the yellow time is 50-100 minute.
(12) spinning:
Carry out at the spinning machine, spin speed: 55m/min, the consisting of of acid bath liquid: sulfuric acid 110-130g/l, sodium sulphate 280-310g/l, zinc sulfate 10-15g/l, acid bath drop＜5g/l. temperature is 45-55 ℃.Certainly, above-mentioned condition also can be carried out suitable adjustment.
(13) refining,
Carry out in refiner, actual conditions is: a washing temperature: normal temperature; Two washing temperature: 50～55 ℃;
Three washing temperature: 50～55 ℃; Desulfurization bath temperature: 70～75 ℃; Desulfurization bath concentration: 7.0～8.0g/l
Hydrogen peroxide concentration: 0.15～0.18%; Last oil concentration: 5～6g/l, temperature is a normal temperature;
Moisture behind the high pressure bundle car: 50～55%
(14) dry, packing
The dried fracture strength of described viscose: 〉=2.2CN/dtex; Wet breaking strength: 〉=1.3CN/dtex; Dried elongation at break: 〉=18.0%; Line density deviation ratio: ± 11.00%; Length variation rate: ± 9.0%; Overcut fibre :≤1.0%; Over-length fibre :≤20.0mg/100g; Residual sulfur content :≤15.0mg/100g; Fault≤25mg/100g; Do the strong coefficient of variation≤18.00%.
Described viscose finished product is carried out the test of antibiotic property, adopt improvement vibration bottle method (JXUB9-2001 01 stretch socks appendix B) to test by PLA General Hospital first traumatology department of the affiliated hospital research department, test result shows, this big jute viscose can reach 100% to the bacteriostasis rate of golden yellow grape ball (ATCC 26085) and Candida albicans (ATCC 90028), can reach more than 93% respectively and more than 96% to the bacteriostasis rate of Escherichia coli and Pseudomonas aeruginosa.
Beneficial effect of the present invention is: the invention provides a kind of is the viscose and preparation method thereof of raw material production with the industrial hemp.Adopting new natural plants industrial hemp is raw material, alleviated the nervous situation of raw material supplies such as cotton linter, timber, fast growing, the abundant industrial hemp resource of fiber content have been made full use of, and be that the viscose of raw material production has antibacterial and deodorizing, moisture absorbing and sweat releasing, uvioresistant features with the industrial hemp, after testing, the antibacterial effect highly significant of this viscose.Use the fiber of the inventive method preparation to have good flexibility, water imbibition, dyeability, can make separately fabric also can with other fiber blends.Method of the present invention, simple possible, method of the present invention is except some conventional steps that adopted common viscose fiber preparation method, when handling at this special raw material of industrial hemp, adopted and dodged quick-fried method, cellulosic percentage composition contained in the industrial hemp is improved, make industrial hemp through the quick-fried processing of sudden strain of a muscle the time, play expanded effect, and impurity such as some lignin have tentatively been removed, for sufficient preparation has been carried out in the infiltration of cooking liquor in the boiling afterwards, before dipping, utilize kneading or grinding leaser to carry out the branch silk resulting industrial hemp pulp, make that the mixing of impregnation stage is more even, therefore the time of dipping also can well be removed contained lignin in the pulp under relatively shorter situation, impurity such as colloid.
The specific embodiment
Embodiment 1
It is the feedstock production viscose that present embodiment relates to the full stalk of industrial hemp.
(1) dodge quick-fried: will get the raw materials ready, the industrial hemp raw material behind the blank is placed on and dodges in the quick-fried machine, adopts the steam humidification pressurization, when pressure reaches 0.8Mpa, keep after 10 minutes the moment release of pressure.
(2) prehydrolysis: will dodge industrial hemp raw material after quick-fried liquor ratio 1: 4, prehydrolysis is 80 minutes under the condition that temperature is 160 ℃.
(3) kraft cooking: liquor ratio 1: 3, total alkali content is (with Na
2The O meter) 25%, sulphidity 15% is incubated 130 ℃ for the first time, temperature retention time 90 minutes, and holding temperature is 155 ℃ for the second time, temperature retention time 180 minutes.
(4) chlorination, bleaching, acid treatment:
Once bleach in bleaching machine earlier, the oven dry stock chlorine dosage is 2% relatively, and bleached pulp is dense 4%, 45 ℃ of temperature, and the time is 50 minutes, and bleaching is carried out acid treatment after finishing, and the hydrochloric acid consumption is 3% to oven dry stock in the acid treatment, and the time is 30 minutes, temperature is a normal temperature; Carry out the secondary bleaching afterwards, the oven dry stock chlorine dosage is 0.3% relatively, and the time is 20 minutes, and temperature is a normal temperature, and bleaching is carried out acid treatment after finishing, and the hydrochloric acid consumption is 2% to oven dry stock in the acid treatment, and the time is 15 minutes.
(5) alkali refining:
Described alkali refining is specially: concentration sodium hydroxide is 130g/l, and the time is 120 minutes, and it is dense 10% that alkali refining is starched, and the temperature of alkali refining is 25 ℃.
(6) rub mill with the hands:
Utilize kneading or grinding leaser to rub hemp dissolving pulp with the hands mill and divide silk, the constant volume Weight control that makes raw material is at 150g/l, and wherein the rotating speed of kneading or grinding leaser is 250r/min.
(7) dipping:
Carry out in treating tank, the hemp dissolving pulp that will carry out after the branch silk through kneading or grinding leaser is dipping 25 minutes in 50 ℃ the sodium hydroxide solution for the 220g/l temperature in concentration.
(8) experienced, yellow:
Experiencedly carry out in experienced drum, actual conditions is: 60 ℃ of temperature, 30 minutes time, viscosity 0.005MPaS.Yellow is carried out in xanthating machine, and actual conditions is: the carbon disulfide consumption is 35% of an alkali cellulose weight, 20 ℃ of yellow beginning temperature, and the whole temperature of yellow is 33 ℃, the yellow time is 80 minutes.
(9) spinning:
Carry out at the spinning machine, spin speed: 55m/min, the consisting of of acid bath liquid: sulfuric acid 110g/l, sodium sulphate 290g/l, zinc sulfate 12g/l, acid bath drop 4g/l. temperature is 50 ℃.
(10) refining,
Carry out in refiner, actual conditions is: a washing temperature: normal temperature; Two washing temperature: 50 ℃;
Three washing temperature: 50 ℃; Desulfurization bath temperature: 75 ℃; Desulfurization bath concentration: 8.0g/l
Hydrogen peroxide concentration: 0.16%; Last oil concentration: 5g/l, temperature is a normal temperature;
Moisture behind the high pressure bundle car: 50～55%
(11) dry, packing
Prepared end product quality is:
Do fracture strength: 2.63CN/dtex; Wet breaking strength: 1.61CN/dtex; Dried elongation at break: 21%; Line density deviation ratio :+0.95%; Length variation rate :+0.3%; Overcut fibre: 0.4%; Over-length fibre: 5.2mg/100g; Residual sulfur content: 9.1mg/100g; Fault 2.1mg/100g; Do the strong coefficient of variation 10.8%;
Embodiment 2
The industrial hemp stalk that present embodiment relates to remove the bast part is the feedstock production viscose.
(1) dodge quick-fried: the industrial hemp raw material of chopping is placed on dodges in the quick-fried machine, adopt the steam humidification pressurization, when pressure reaches 1.2Mpa, keep after 8 minutes the moment release of pressure.
(2) prehydrolysis: liquor ratio 1: 6,175 ℃ of holding temperatures, temperature retention time 60 minutes.
(3) kraft cooking: liquor ratio 1: 5, total alkali content is (with Na
2The O meter) 20%, sulphidity 5% is incubated 140 ℃ for the first time, temperature retention time 80 minutes, and holding temperature is 160 ℃ for the second time, temperature retention time 130 minutes.
(4) chlorination, bleaching, acid treatment:
Once bleach in bleaching machine earlier, the oven dry stock chlorine dosage is 1% relatively, and bleached pulp is dense 5%, 50 ℃ of temperature, and the time is 90 minutes, and bleaching is carried out acid treatment after finishing, and the hydrochloric acid consumption is 2% to oven dry stock in the acid treatment, and the time is 20 minutes, temperature is a normal temperature; Carry out the secondary bleaching afterwards, the oven dry stock chlorine dosage is 0.2% relatively, and the time is 20 minutes, and temperature is a normal temperature, and bleaching is carried out acid treatment after finishing, and the hydrochloric acid consumption is 1% to oven dry stock in the acid treatment, and the time is 30 minutes.
(5) alkali refining:
This step comprises that the slurry to gained after the acid treatment carries out desanding, concentrates, and can carry out desanding in desander, removes sand after thickener makes concentration of slurry be concentrated into 3.0-3.5%.Described alkali refining is specially: concentration sodium hydroxide is 200g/l, and the time is 60 minutes, and it is dense 12% that alkali refining is starched, and the temperature of alkali refining is 20 ℃.
(6) rub mill with the hands:
Utilize kneading or grinding leaser to rub hemp dissolving pulp with the hands mill and divide silk, the constant volume Weight control that makes raw material is at 120g/l, and wherein the rotating speed of kneading or grinding leaser is 350r/min.
(7) dipping:
Be immersed in the treating tank and carry out, the industrial hemp pulp that will carry out after the branch silk through kneading or grinding leaser is dipping 25 minutes in 50 ℃ the sodium hydroxide solution for the 220g/l temperature in concentration.
(8) experienced, yellow:
Experiencedly carry out in experienced drum, actual conditions is: temperature 30-60 ℃, and time 30-90 minute, viscosity 0.006MPaS.Yellow is carried out in xanthating machine, and actual conditions is: the carbon disulfide consumption is 45% of an alkali cellulose weight, and the whole temperature of yellow is 33 ℃, and the yellow time is 50 minutes.
(9) spinning:
Carry out at the spinning machine, spin speed: 55m/min, the consisting of of acid bath liquid: sulfuric acid 130g/l, sodium sulphate 2310g/l, zinc sulfate 10-15g/l, acid bath drop 3g/l. temperature is 45 ℃.
(10) refining,
Carry out in refiner, actual conditions is: a washing temperature: normal temperature; Two washing temperature: 50～55 ℃;
Three washing temperature: 50～55 ℃; Desulfurization bath temperature: 70～75 ℃; Desulfurization bath concentration: 7.0～8.0g/l
Hydrogen peroxide concentration: 0.15～0.18%; Last oil concentration: 5～6g/l, temperature is a normal temperature;
Moisture behind the high pressure bundle car: 50～55%
(11) dry, packing
Prepared end product quality is: do fracture strength: 2.52CN/dtex; Wet breaking strength: 1.53CN/dtex; Dried elongation at break: 18.0%; Line density deviation ratio :+1.12%; Length variation rate :+0.5%; Overcut fibre: 0.2%; Over-length fibre: 3.5mg/100g; Residual sulfur content: 8.0mg/100g; Fault 4.5mg/100g; Do the strong coefficient of variation 13.26%.
Embodiment 3
The industrial hemp stalk that present embodiment relates to remove the bast part is the feedstock production viscose.
(1) dodge quick-fried: the material of chopping is dodged in the quick-fried machine in continous mode, adopts the steam humidification pressurization, when pressure reaches 0.6Mpa, keep after 15 minutes the moment release of pressure.
(2) prehydrolysis: liquor ratio 1: 5,150 ℃ of holding temperatures, temperature retention time 120 minutes.
(3) kraft cooking: liquor ratio 1: 4, total alkali content is (with Na
2The O meter) 40%, sulphidity 25% is incubated 150 ℃ for the first time, temperature retention time 60 minutes, and holding temperature is 170 ℃ for the second time, temperature retention time 90 minutes.
(4) chlorination, bleaching, acid treatment:
Once bleach in bleaching machine earlier, the oven dry stock chlorine dosage is 3% relatively, and bleached pulp is dense 5%, 39 ℃ of temperature, and the time is 60 minutes, and bleaching is carried out acid treatment after finishing, and the hydrochloric acid consumption is 5% to oven dry stock in the acid treatment, and the time is 20 minutes, temperature is a normal temperature; Carry out the secondary bleaching afterwards, the oven dry stock chlorine dosage is 0.5% relatively, and the time is 30 minutes, and temperature is a normal temperature, and bleaching is carried out acid treatment after finishing, and the hydrochloric acid consumption is 1% to oven dry stock in the acid treatment, and the time is 30 minutes.
(5) alkali refining:
This step comprises that the slurry to gained after the acid treatment carries out desanding, concentrates, and can carry out desanding in desander, removes sand after thickener makes concentration of slurry be concentrated into 3.0-3.5%.Described alkali refining is specially: concentration sodium hydroxide is 160g/l, and the time is 100 minutes, and it is dense 10% that alkali refining is starched, and the temperature of alkali refining is 30 ℃.
(6) rub mill with the hands:
Utilize kneading or grinding leaser to rub hemp dissolving pulp with the hands mill and divide silk, the constant volume Weight control that makes raw material is at 130g/l, and wherein the rotating speed of kneading or grinding leaser is 350r/min.
(7) dipping:
Carry out in treating tank, the hemp dissolving pulp that will carry out after the branch silk through kneading or grinding leaser is dipping 15 minutes in 30 ℃ the aqueous slkali for the 260g/l temperature in concentration.
(8) experienced, yellow:
Experiencedly carry out in experienced drum, actual conditions is: 60 ℃ of temperature, 30 minutes time, viscosity 0.005-0.007MPaS.Yellow is carried out in xanthating machine, and actual conditions is: the carbon disulfide consumption is 26% of an alkali cellulose weight, and the whole temperature of yellow is 28 ℃, and the yellow time is 100 minutes.
(9) spinning:
Carry out at the spinning machine, spin speed: 55m/min, the consisting of of acid bath liquid: sulfuric acid 120g/l, sodium sulphate 300g/l, zinc sulfate 15g/l, acid bath drop 4g/l. temperature is 50 ℃.
(10) refining,
Carry out in refiner, actual conditions is: a washing temperature: normal temperature; Two washing temperature: 50～55 ℃;
Three washing temperature: 50～55 ℃; Desulfurization bath temperature: 70～75 ℃; Desulfurization bath concentration: 7.0～8.0g/l
Hydrogen peroxide concentration: 0.15～0.18%; Last oil concentration: 5～6g/l, temperature is a normal temperature;
Moisture behind the high pressure bundle car: 50～55%
(11) dry, packing
Prepared end product quality is: do fracture strength: 2.40CN/dtex; Wet breaking strength: 1.51CN/dtex; Dried elongation at break: 20.0%; Line density deviation ratio :-2.25%; Length variation rate: 6.2%; Overcut fibre: 0.6%; Over-length fibre: 3.8mg/100g; Residual sulfur content: 11.2mg/100g; Fault 5.8mg/100g; Do the strong coefficient of variation 14.25%;
Embodiment 4
The industrial hemp stalk that present embodiment relates to remove the bast part is the feedstock production viscose.
(1) alkaline cooking:
Liquor ratio 1: 4, total alkali content is (with Na
2The O meter) 27%, be incubated 150 ℃ for the first time, temperature retention time 70 minutes, holding temperature is 165 ℃ for the second time, temperature retention time 135 minutes.
(2) rub mill with the hands and divide silk: rotating speed 350r/min, natural bulk density 130g/l.
(3) alkali steeping: 30 ℃ of temperature, pressure 0.3Mpa, 90 minutes time.
(4) end product quality:
Do fracture strength: 2.3CN/dtex; Wet breaking strength: 1.42CN/dtex; Dried elongation at break: 22%; Line density deviation ratio :-3.6%; Length variation rate :-3.2%; Overcut fibre: 0.3%; Over-length fibre: 8.0mg/100g; Residual sulfur content: 10.5mg/100g; Fault: 6.3mg/100g; Do the strong coefficient of variation: 11.6%.
Embodiment 5
The bast that present embodiment relates to the industrial hemp stalk that comes unstuck is divided into the feedstock production viscose.
(1) prehydrolytic sulfate process boiling:
Prehydrolysis: liquor ratio 1: 6,150 ℃ of holding temperatures, temperature retention time 120 minutes.
Kraft cooking: liquor ratio 1: 5, total alkali content (in Na2O) 40%, sulphidity 18% is incubated 130 ℃ for the first time, temperature retention time 60 minutes, holding temperature is 175 ℃ for the second time, temperature retention time 90 minutes.
(2) rub mill with the hands and divide silk: rotating speed 260r/min, natural bulk density 120g/l.
(3) alkali soaks: 40 ℃ of temperature, pressure 0.2Mpa, 120 minutes time.
All the other steps are identical with embodiment 1
End product quality: do fracture strength: 2.45CN/dtex; Wet breaking strength: 1.51CN/dtex; Dried elongation at break: 23.1%; Line density deviation ratio :+2%; Length variation rate :+6.8%; Overcut fibre: 0.9%; Over-length fibre: 11mg/100g; Residual sulfur content: 8.7mg/100g; Fault: 2.1mg/100g does the strong coefficient of variation: 14.1%;
Embodiment 6
The industrial hemp hemp stalk that present embodiment relates to remove the bast part is the feedstock production viscose.
(1) kraft cooking:
Liquor ratio 1: 3.5, total alkali content is (with Na
2The O meter) 20%, sulphidity 15%, temperature retention time 120 minutes, 175 ℃ of holding temperatures.
(2) alkali refining: starch dense 15%, alkali charge 7%, 135 ℃ of temperature, 90 minutes time
(3) rub mill with the hands and divide silk: rotating speed 350r/min, natural bulk density 130g/l.
(4) alkali soaks: 30 ℃ of temperature, pressure 0.3Mpa, 90 minutes time.
All the other steps are identical with embodiment 2
End product quality: do fracture strength: 2.5CN/dtex; Wet breaking strength: 1.58CN/dtex; Dried elongation at break: 23.6%; Line density deviation ratio :+1.25%; Length variation rate :-3.0%; Overcut fibre: 0.3%; Over-length fibre: 2.8mg/100g; Fault 9.0mg/100g; Do the strong coefficient of variation 12.00%.
Embodiment 7
The bast that present embodiment relates to the industrial hemp stalk that comes unstuck with process is divided into the feedstock production viscose.
(1) alkaline cooking technology:
Liquor ratio 1: 4.7, total alkali content is (with Na
2The O meter) 25%, sulphidity 0%, temperature retention time 160 minutes, 170 ℃ of holding temperatures.
(2) alkali refining: starch dense 18%, alkali charge 5%, 120 ℃ of temperature, 73 minutes time
(3) rub mill with the hands and divide silk: rotating speed 260r/min, natural bulk density 120g/l.
(4) alkali soaks: 40 ℃ of temperature, pressure 0.2Mpa, 120 minutes time.
All the other steps are identical with embodiment 3
End product quality: do fracture strength: 2.25CN/dtex; Wet breaking strength: 1.35CN/dtex; Dried elongation at break: 24.5%; Line density deviation ratio :-0.5%; Length variation rate: 2.0%; Overcut fibre: 0.3%; Over-length fibre: 4.5mg/100g; Fault: 7.5mg/100g; Do the strong coefficient of variation: 10.00%.
Embodiment 8
Present embodiment relates to the full stalk feedstock production of industrial hemp viscose.
(1) kraft cooking:
Liquor ratio 1: 5.5, total alkali content is (with Na
2The O meter) 40%, sulphidity 25%, temperature retention time 180 minutes, 160 ℃ of holding temperatures.
(2) alkali refining: starch dense 20%, alkali charge 10%, 150 ℃ of temperature, 60 minutes time.
(3) rub mill with the hands and divide silk: rotating speed 500r/min, natural bulk density 150g/l.。
(4) alkali soaks: 30 ℃ of temperature, pressure 0.3Mpa, 90 minutes time.
All the other steps are identical with embodiment 3.
End product quality: do fracture strength: 2.32CN/dtex; Wet breaking strength: 1.42CN/dtex; Dried elongation at break: 20.5%; Line density deviation ratio: 0.5%; Length variation rate: 1.8%; Overcut fibre: 0.9%; Over-length fibre: 3.5mg/100g; Fault 6.5mg/100g; Do the strong coefficient of variation 15.00%.
Claims (13)
1. viscose, it is characterized in that: described viscose is feedstock production with the industrial hemp, the dried fracture strength of described viscose: 〉=2.2CN/dtex; Wet breaking strength: 〉=1.3CN/dtex; Dried elongation at break: 〉=18.0%; Line density deviation ratio: ± 7.00%; Length variation rate: ± 9.0%; Overcut fibre :≤1.0%; Over-length fibre :≤20.0mg/100g; Residual sulfur content :≤15.0mg/100g; Fault≤25mg/100g; Do the strong coefficient of variation≤18.00%.
2. viscose according to claim 1 is characterized in that described raw material is the bast part through the industrial hemp stalk that comes unstuck or do not come unstuck, and perhaps the full stalk of industrial hemp perhaps removes bast industrial hemp hemp stalk partly.
3. the preparation method of viscose according to claim 1 and 2, comprise get the raw materials ready, blank, boiling, selected, chlorination, bleaching, acid treatment, alkali refining, manufacture paper with pulp, flood, squeezing, pulverizing, experienced, yellow, dissolving, spinning, refining, drying, packing, it is characterized in that after carrying out blank before boiling, also through dodging quick-fried process.
4. method according to claim 3 is characterized in that described sudden strain of a muscle is quick-fried to be specially: the material of chopping is placed on dodges in the quick-fried machine, adopt the steam humidification pressurization, when pressure reaches 0.6-1.2Mpa, keep after 8-15 minute the moment release of pressure.
5. method according to claim 3 is characterized in that before the dipping, utilizing kneading or grinding leaser to rub pulp with the hands mill and dividing silk after manufacturing paper with pulp, and the constant volume Weight control that makes raw material is at 120～150g/l, and wherein the rotating speed of kneading or grinding leaser is 250-500r/min.
6. according to claim 3 or 4 or 5 described methods, it is characterized in that adopting the method for prehydrolysis-kraft cooking to be specially: earlier in liquor ratio 1: 4～6, under the condition that holding temperature is 150～175 ℃ with the raw material prehydrolysis temperature retention time got ready 60～120 minutes; Be 1: 3～5 in liquor ratio then, alkali charge is with Na
2The O meter under the condition of sulphidity 5～25%, is warming up to 130～150 ℃, temperature retention time 60～90 minutes to over dry raw material 20～40%; Be warming up to 155～170 ℃ afterwards again, temperature retention time 90～180 minutes.
7. according to claim 3 or 4 or 5 described methods, it is characterized in that adopting the concrete grammar of alkaline cooking to be: in liquor ratio is 1: 3.5～5.5, and alkali charge is with Na
2Under O meter 18～25% the condition to the over dry raw material, be warming up to 160～175 ℃ after temperature retention time 120～180 minutes.
8. according to claim 3 or 4 or 5 described methods, it is characterized in that the quality of the pulp of gained after described manufacturing paper with pulp is: alpha cellulose 〉=90%, viscosity 〉=8.0mPas, whiteness 〉=60%, moisture 9.0 ± 0.5%, iron branch≤140ppm.
9. according to claim 3 or 4 or 5 described methods, it is characterized in that described dipping is specially: the hemp dissolving pulp that will carry out after the branch silk through kneading or grinding leaser is 220-260g/l in concentration, and temperature is dipping 10-25 minute in 40-60 ℃ the NaOH solution.
10. according to claim 3 or 4 or 5 described methods, before it is characterized in that after selected, manufacturing paper with pulp, also comprise the process of alkali refining; Described alkali refining is specially: the concentration of NaOH is 130-200g/l, and the time is 60-120 minute, and alkali refining is starched dense 6-12%, and the temperature of alkali refining is 20-35 ℃.
11. will go 3 or 4 or 5 described methods according to right, it is characterized in that described bleaching and acid treatment are:
Once bleach in bleaching machine earlier, the oven dry stock chlorine dosage is 1-3% relatively, the dense 4-6% of bleached pulp, temperature 39-50 ℃, the time is 40-90 minute, and bleaching is carried out acid treatment after finishing, the hydrochloric acid consumption is 2-5% to oven dry stock in the acid treatment, and the time is 20-60 minute, and temperature is a normal temperature; Carry out the secondary bleaching afterwards, the oven dry stock chlorine dosage is 0.2%-0.5% relatively, and the time is 20-40 minute, and temperature is a normal temperature, and bleaching is carried out acid treatment after finishing, and the hydrochloric acid consumption is 1-3% to oven dry stock in the acid treatment, and the time is 10-30 minute.
12., it is characterized in that described yellow condition is: CS according to claim 3 or 4 or 5 described methods
2The 25-40% of the relative methylcellulose content of addition, the time is 90-130 minute, the yellow initial temperature is 19-20 ℃, warm 25-32 ℃ eventually of yellow, vacuum :≤-0.08Mpa.
13., it is characterized in that described spinning is specially: carry out the consisting of of acid bath liquid at the spinning machine: sulfuric acid 110-130g/l according to claim 3 or 4 or 5 described methods, sodium sulphate 280-310g/l, zinc sulfate 10-15g/l, acid bath drop＜5g/l, temperature is 45-55 ℃.
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| CNB2007101306067A CN100523320C (en) | 2007-07-10 | 2007-07-10 | Viscose fiber and its preparing method |
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| CN103114339A (en) * | 2013-03-18 | 2013-05-22 | 河南舒莱卫生用品有限公司 | Preparation method of hemp stalk viscose fiber and application thereof |
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| CN107475803B (en) * | 2017-08-25 | 2021-04-16 | 浙江伊彤服饰有限公司 | Preparation method of moisture-absorbing and sweat-releasing soft fiber and fiber obtained by preparation method |
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