CN1194119C - Bamboo Viscose fibre and its preparing method - Google Patents
Bamboo Viscose fibre and its preparing method Download PDFInfo
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- CN1194119C CN1194119C CNB031284965A CN03128496A CN1194119C CN 1194119 C CN1194119 C CN 1194119C CN B031284965 A CNB031284965 A CN B031284965A CN 03128496 A CN03128496 A CN 03128496A CN 1194119 C CN1194119 C CN 1194119C
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- 239000000835 fiber Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 32
- 229920000297 Rayon Polymers 0.000 title claims abstract description 24
- 235000017166 Bambusa arundinacea Nutrition 0.000 title claims abstract description 12
- 235000017491 Bambusa tulda Nutrition 0.000 title claims abstract description 12
- 241001330002 Bambuseae Species 0.000 title claims abstract description 12
- 235000015334 Phyllostachys viridis Nutrition 0.000 title claims abstract description 12
- 239000011425 bamboo Substances 0.000 title claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 36
- 238000009835 boiling Methods 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 238000012545 processing Methods 0.000 claims abstract description 4
- 238000004061 bleaching Methods 0.000 claims description 57
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 50
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 28
- 239000000460 chlorine Substances 0.000 claims description 28
- 229910052801 chlorine Inorganic materials 0.000 claims description 28
- 239000003513 alkali Substances 0.000 claims description 27
- 230000014759 maintenance of location Effects 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000010306 acid treatment Methods 0.000 claims description 15
- 238000007670 refining Methods 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 8
- 229910052717 sulfur Inorganic materials 0.000 claims description 8
- 239000011593 sulfur Substances 0.000 claims description 8
- 239000002585 base Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000010411 cooking Methods 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- 238000009897 hydrogen peroxide bleaching Methods 0.000 claims description 6
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 9
- 238000007598 dipping method Methods 0.000 abstract description 8
- 238000009874 alkali refining Methods 0.000 abstract description 7
- 238000009987 spinning Methods 0.000 abstract description 7
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 5
- 238000001035 drying Methods 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 4
- 238000000227 grinding Methods 0.000 abstract description 3
- 238000012805 post-processing Methods 0.000 abstract description 3
- 241000894006 Bacteria Species 0.000 abstract description 2
- 239000004576 sand Substances 0.000 abstract 2
- 206010033546 Pallor Diseases 0.000 abstract 1
- 238000003483 aging Methods 0.000 abstract 1
- 230000032683 aging Effects 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000012856 packing Methods 0.000 abstract 1
- 238000007781 pre-processing Methods 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
- 238000004383 yellowing Methods 0.000 abstract 1
- 238000005660 chlorination reaction Methods 0.000 description 19
- 235000011121 sodium hydroxide Nutrition 0.000 description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 14
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 12
- 238000006116 polymerization reaction Methods 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- 230000003115 biocidal effect Effects 0.000 description 6
- 229920002678 cellulose Polymers 0.000 description 6
- 235000010980 cellulose Nutrition 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 6
- 239000004744 fabric Substances 0.000 description 6
- 239000001913 cellulose Substances 0.000 description 5
- 229920002472 Starch Polymers 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000005554 pickling Methods 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 239000008107 starch Substances 0.000 description 4
- 235000019698 starch Nutrition 0.000 description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 4
- 229960001763 zinc sulfate Drugs 0.000 description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- -1 more precisely Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-O oxonium Chemical compound [OH3+] XLYOFNOQVPJJNP-UHFFFAOYSA-O 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
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- 108090000790 Enzymes Proteins 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
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- 229940088598 enzyme Drugs 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 108010059892 Cellulase Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 229920001410 Microfiber Polymers 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 208000030961 allergic reaction Diseases 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 229940106157 cellulase Drugs 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
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- Artificial Filaments (AREA)
- Paper (AREA)
Abstract
The present invention relates to a viscose fiber and a preparation method thereof by bamboo. The method comprises the steps of bamboo preparation, blanking, screening, material washing, preprocessing, boiling, sand removing, concentrating, chlorinating, alkali refining, blanching, acid processing, sand removing, concentrating, papermaking, dipping, squeezing, pulverizing, ageing, yellowing, grinding, dissolving, filtrating, debubbling, filtrating, spinning, drafting, cutting off, post processing, drying and packing. The viscose fiber prepared from bamboo used as raw materials according to the steps has the characteristics of bacteria resistance, favorable slipperiness and coolness, fineness, brightness, etc. Therefore, fiber products have natural antibacterial properties, and the present invention develops and creates a new field for the viscose fiber and functional products thereof.
Description
Technical field
The present invention relates to promptly prepare fiber by pulp and paper making method by the plant fiber material producd fibers, more precisely, bamboo viscose fiber and preparation method thereof.
Technical background
At present, viscose is to be raw material with native celluloses such as timber, cotton linters, a kind of broad-spectrum regenerated celulose fibre that makes through a series of processing procedures such as boiling, acid treatment, bleaching.Because this fiber and fabric thereof have good moisture adsorption and releasing, and be soft, comfortable and easy to wear,, be subjected to consumers in general's favor deeply near natural woolliness.Particularly back to nature, green consumption is current, is that the fabric demand of raw material grows with each passing day especially with the natural fabric, and still 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 from health, health care equal angles, also more characteristic requirement is proposed textile raw material, the most outstanding promptly requires at antibiotic, bacteria resistance function, antibiotic both at home and abroad now, odourproof fiber and fabric are at fiber or fabric and produce the later stage, add medicament and are surrounded on fiber surface and achieve the goal.But in dress and application process along with the influence of wearing and tearing and physics such as washing, chemical action, its function will descend so that lose gradually, does not reach real antibiotic purpose, and medicament also can cause certain allergic reaction simultaneously, thereby may influence wearer's skin, make it to wear uncomfortable.
Summary of the invention
The object of the present invention is to provide a kind of bamboo wood plant material that utilizes to produce viscose, this fiber not only has the characteristic of common viscose fiber, and kept antibacterial material to greatest extent, need not carry out chemicals treatment, promptly have antibiotic, fungi-proofing effect, and without any side effects to human body, be not afraid of washing, wear-resisting again, fabric is durable, and antibiotic persistence is long, also has characteristics such as smooth, nice and cool, fine and smooth, light.
Another object of the present invention is to provide a kind of preparation method of viscose, this method comprises: utilize conventional pulp and paper making method, alkaline process for example, inferior sodium method, oxonium base method etc. makes thick slurry, and then makes viscose through a series of processing procedures such as acid treatment, bleachings.
The viscose that utilizes method of the present invention to make has unique characteristic as not being afraid of washing, wear-resisting and lasting antibiotic property, and the cutter of obtaining really of described characteristic is managed still not fully aware of at present.The applicant thinks, this and raw materials used confidential relation arranged, may make final viscose have particular performances just because of the distinctive antibacterial material of bamboo wood itself.In addition, also have some relations with preparation technology.
In preparation method of the present invention, at first can adopt alkaline process, sulphite process or the thick slurry of improved oxonium base method preparation, especially adopt the thick slurry of sulphite process or improved oxonium base method preparation.Its process conditions can obtain by conventional technological means to those skilled in the art, and for example when adopting higher temperature, pressure can correspondingly reduce.When adopting higher alkali charge, digestion time can correspondingly reduce or the like.
When adopting improved oxygen-alkali cooking, its cooking schedule is preferably: alkali charge: in NaOH to oven dry stock amount 8-16%; Liquor ratio: 1: 4-6; H
2O
2: to oven dry stock amount 1-3%; Logical oxygen pressure: 0.70-0.90Mpa; Heated up total time: 150-240 minute; Holding temperature: 125-132 ℃; Temperature retention time: 6-11 hour.Cooking quality: KMnO
4Value 4-10; The degree of polymerization 〉=620; First fibre 〉=97%.In addition, those of ordinary skills know, because H
2O
2Very easily decomposition, passivation etc., therefore, in order more to help boiling, in digestion process, can also add some auxiliary agents commonly used, for example surfactant, metal-chelator or the like are known to those skilled in the art, need not to make creative work.Can also carry out preliminary treatment to raw material before boiling in addition, for example pretreated condition can be liquor ratio: 1: 2.5-3.5; 160 ℃-180 ℃ of boiling temperatures; Time 100-180 minute.
When adopting sulphite process (sodium base) boiling, total acid is greater than 4%, combined acid is 1.0-3.0, the boiling maximum temperature is 165 ℃, the insulation of employing secondary: holding temperature: 120-140 ℃ for the first time, temperature retention time: 60-120 minute, holding temperature: 140-165 ℃ for the second time, temperature retention time: 120-240 minute, fluid temperature 60-90 ℃.Cooking quality: the degree of polymerization 〉=620, first fibre 〉=97%.
Certainly,, raw material is got the raw materials ready, blank, screened, washes material etc. no matter adopt which kind of digesting technoloy, removing impurity such as silt, bamboo bits, the conventional steps that all is absolutely necessary, and also this also is known to those skilled in the art.For example bamboo wood can be cut into the bamboo chip of long 20-40 millimeter.For example can use the hot water wash material, water temperature 60-80 ℃, the time can be at 10-20 minute.
After the boiling, can carry out desanding, concentrate, slurry to remove foreign material such as silt, irony, and be concentrated into technological requirement by thickener, for example concrete technical conditions are: remove the dense 0.5-0.7% of mortar, desanding pressure 0.30-0.33Mpa, the dense 3-4% of thickener outlet slurry.It is to be noted that these conditions can do suitable adjustment as the case may be, this is known to those skilled in the art.
As the field of papermaking those of ordinary skill know, after desanding, concentrating,, should bleach it in order to ensure pulp brightness.In the present invention, can use conventional method for bleaching, for example adopt tri-stage bleaching commonly used in the paper industry, it is chlorination → alkali refining → bleaching, chlorination can be carried out in the chlorination tower, and its concrete technical conditions are: the chlorination chlorine dosage to oven dry stock is 1-4%, and dense 2.8-3.2% is starched in chlorination, time of chlorinating 40-60 minute, chlorination temperature was a normal temperature.Certainly, as the case may be, also can change above-mentioned condition, making described change is known to those skilled in the art, and these changes are also included within the scope of the present invention.
Alkali refining carries out in the alkalization tower after the chlorination, and concrete technical conditions are: starch dense 5-10%, NaOH is 2-6% to the consumption of oven dry stock, and extraction temperature is 70-90 ℃, H
2O
2Consumption to oven dry stock is 0.5-1.5%, and the energy amount of oxygen is 0.4-0.6% to the consumption of oven dry stock, and the time is 60-100 minute.It is believed that the alkali refining that adopts increase oxygen of the present invention and hydrogen peroxide to handle is to obtain the requisite process conditions of viscose of the present invention.
Bleaching is carried out in bleaching machine, and concrete technical conditions are: the dense 5-8% of bleached pulp, promptly keep antibacterial material as far as possible according to purified pulp quality requirement and antibacterial material characteristic, and bleaching divides two sections variate bleachings:
First section pH=9-11, the chlorine dosage of oven dry stock is 1-3% relatively, temperature 35-38 ℃, time 90-180 minute,
Second section pH=2-4, the chlorine dosage 0.2-0.5% of relative oven dry stock, time 10-30 minute,
Bleaching Quality: whiteness 〉=76%, the degree of polymerization 〉=450, first fibre 〉=93%.
In addition, also can adopt other method for bleaching, for example can adopt following bleaching technology condition in bleaching machine: the bleaching of I section: chlorine dosage is 2-5% to the consumption of oven dry stock, temperature 45-55 ℃, and bleaching alkalinity≤250g/m
3, bleaching time 120-240 minute.II section bleaching: the oven dry stock acid treatment with acid amount 1-2%, time 20-50 minute, is washed to below the acid content 0.5g/L.The bleaching of III section: to the bleaching chlorine dosage 1-3% of oven dry stock, temperature 30-40 ℃, bleaching alkalinity≤150g/m
3, bleaching time 60-180 minute, be washed till residual acid≤0.5g/L.Bleaching Quality requires: whiteness 〉=76%, the degree of polymerization 〉=450, alpha cellulose 〉=93%.
For making viscose, the acid treatment step that is absolutely necessary also is that those of ordinary skills are known.Acid treatment can be carried out in bleaching machine, and concrete technical conditions are: the hydrochloric acid consumption is 2-5% to oven dry stock, and the time is 20-60 minute, and temperature is a normal temperature.Certain acid-treated condition can be made appropriate change as the case may be, the kind of the acid of being adopted for example, time and temperature or the like.And these changes are also included within the scope of the present invention.
If desired, also can carry out desanding, concentrate slurry after the acid treatment, can carry out desanding in desander, desanding be after thickener makes concentration of slurry be concentrated into 3.0-3.5%.Manufacture paper with pulp in pulp machine then, the concrete technical conditions of manufacturing paper with pulp can be quantitative 400-700g/m
2, moisture content 8.5-11.5%.
Step afterwards is an impregnation steps, and it can carry out in treating tank, and concrete technical conditions are: dipping temperature 30-40 ℃, and concentration of lye 230-250g/l, dip time 15-30 minute.Certainly, what those of ordinary skills should know is that above-mentioned condition can be carried out suitable adjustment, for example suitably improves temperature and the corresponding minimizing time, as can flooding in 50-60 ℃ scope, and these changes are also included within the scope of the present invention.
Squeezing step is then carried out in squeezer, and concrete technical conditions are: the fine content 31-33% of first, and caustic soda content 14-16%.Certainly, what those of ordinary skills should know is that above-mentioned condition can be carried out suitable adjustment, for example suitably improve temperature and the corresponding minimizing time, and these changes is also included within the scope of the present invention.
Experiencedly carry out in experienced drum, concrete technical conditions are: experienced temperature 16-26 ℃, yellow is carried out in xanthating machine, and concrete technical conditions are: the carbon disulfide consumption is the 30-35% of alkali cellulose weight, and finishing temperature 35-40 ℃, yellow time, 40-80 minute.Certainly, what those of ordinary skills should know is that above-mentioned condition can be carried out suitable adjustment, for example suitably improve temperature and the corresponding minimizing time, and these changes is also included within the scope of the present invention.
Then, according to the processing method of viscose routine slurry is ground and spinning.Grinding is carried out in thick, refiner, and concrete technical conditions are: corase grind granularity＜6 millimeter, correct grinding granularity＜10 micron.Concrete spinning condition in spinning machine is as follows:
Acid bath liquid is formed: sulfuric acid 80-100g/l, and sodium sulphate 200-300g/l, zinc sulfate 30-45g/l, acid bath drop＜5g/l, soaks long 400-500 millimeter by temperature 35-45 ℃.
Certainly, what those of ordinary skills should know is, above-mentioned condition can be carried out suitable adjustment, for example suitably improves temperature and the corresponding minimizing time, kind of the acid of being adopted etc. for example, and these changes are also included within the scope of the present invention.
Be drawing-off, post processing (refining) and drying after this, the technical conditions of these treatment steps all are that those skilled in the art know.For example in machine cluster, carry out drawing-off condition can for: total draft 1.9-2.2 doubly, 1.0 times of spinneret drafts.Refining condition in the refiner is: 40-50 ℃ of a wash water temperature, 60-70 ℃ of alkali cleaning temperature, alkali concn 6-8g/l, 45-55 ℃ of two wash water temperature, three wash temperature 40-50 ℃, last oil concentration 6-8g/l, last oil temperature normal temperature, hydrogen peroxide bleaching concentration 0.05-0.15%, bleaching temperature normal temperature, refining time 10-15 minute.Also pickling can be arranged in addition in two wash, its concentration is 0.6-1.8g/L, and temperature is a normal temperature.Drying condition in drying machine for example can for: proparea bake out temperature 80-90 ℃, middle district bake out temperature 90-100 ℃, back zone bake out temperature 90-95 ℃, drying time 10-20 minute.
Described post processing (refining) also can be handled with enzyme and substitute, for example, under slightly acidic condition, carry out cellulose treatment, in the hope of passing through biocatalysis, reduce microfibre, make fiber surface smooth, and strengthen fungi-proofing function, described enzyme is handled concrete technical conditions can be cellulase consumption: 19.8-22.8EGU/kg, pH5-6, temperature 30-40 ℃, be sprayed on fiber surface with 0.6g/l concentration, handled 20-30 minute.
The performance of viscose of the present invention is as follows: do fracture strength: 〉=1.90cN/dtex; Wet breaking strength: 〉=1.0cN/dtex; Dried elongation at break: 〉=16.0%; Line density deviation ratio: ± 7.00%; Length variation rate: ± 7.0%; Overcut fibre :≤1.0%; Over-length fibre :≤20.0mg/100g; Residual sulfur content :≤20.0mg/100g; Fault :≤12mg/100g.
Embodiment
Below in conjunction with specific embodiments the present invention is made a more detailed description, should be noted that, at these all embodiment that list only is illustrative, and does not mean that the scope of the invention is limited, and the present invention is limited by the scope of appended claims and equivalent thereof.
Embodiment 1
(1) preliminary treatment: liquor ratio 1: 2.5,160 ℃ of temperature, 180 minutes time.
(2) boiling: alkali charge in NaOH to oven dry stock amount 8%, liquor ratio 1: 4, hydrogen peroxide is to oven dry stock amount 1%, logical oxygen pressure 0.70Mpa heats up 150 minutes total times 125 ℃ of holding temperatures, temperature retention time 11 hours.
(3) chlorination: the chlorination chlorine dosage is to oven dry stock amount 1%, and it is dense 3.2% that chlorination is starched, time of chlorinating 60 minutes, chlorination temperature normal temperature.
(4) alkali refining: starch densely 5%, the NaOH consumption is to oven dry stock amount 2%, and 90 ℃ of extraction temperatures, hydrogen peroxide be to oven dry stock amount 0.5%, and logical amount of oxygen is to oven dry stock amount 0.4%, 100 minutes time.
(5) bleaching:
First section pH=9, chlorine dosage be to oven dry stock amount 1%, 38 ℃ of temperature, 180 minutes time.
Second section pH=2, chlorine dosage be to oven dry stock amount 0.2%, 30 minutes time.
(6) acid treatment: the hydrochloric acid consumption is to oven dry stock amount 2%, 60 minutes time, temperature normal temperature.
(7) dipping: 30 ℃ of dipping temperatures, concentration of lye 230g/l, dip time 30 minutes.
(8) squeezing: the fine content of first: 31%, caustic soda content 16.0%.
(9) experienced: temperature is 16 ℃.
(10) yellow: the carbon disulfide consumption is 30% of an alkali cellulose weight, 35 ℃ of finishing temperatures, 80 minutes time.
(11) spinning: acid bath liquid is formed: sulfuric acid 80g/l, and sodium sulphate 200g/l, zinc sulfate 30g/l, 35 ℃ of temperature are soaked long 500 millimeters.
(12) end product quality:
Do fracture strength: 2.26CN/dtex,
Wet breaking strength: 1.34CN/dtex,
Dried elongation at break: 24.1%,
The line density deviation ratio :+0.60%,
The length variation rate :-5.8%,
Overcut fibre: 0.2%,
Over-length fibre: 3.3mg/100g,
Residual sulfur content: 8.1mg/100g,
Fault: 3.5mg/100g,
Greasy dirt yellowish fiber: 0mg/100g,
Do the strong coefficient of variation: 12.56%,
Whiteness: 76.6%,
Oil content: 0.16%
Regain: 11.93%,
Grade: high-class product.
Embodiment 2
(1) preliminary treatment: liquor ratio 1: 3,170 ℃ of temperature, 150 minutes time.
(2) boiling: alkali charge in NaOH to oven dry stock amount 13%, liquor ratio 1: 5, hydrogen peroxide is to oven dry stock amount 2%, logical oxygen pressure 0.80Mpa heats up 200 minutes total times 128 ℃ of holding temperatures, temperature retention time 8.5 hours.
(3) chlorination: the chlorination chlorine dosage is to oven dry stock amount 2.5%, and it is dense 3.0% that chlorination is starched, time of chlorinating 50 minutes, chlorination temperature normal temperature.
(4) alkali refining: starch densely 8%, the NaOH consumption is to oven dry stock amount 4%, and 80 ℃ of extraction temperatures, hydrogen peroxide be to oven dry stock amount 1%, and logical amount of oxygen is to oven dry stock amount 0.5%, 80 minutes time.
(5) bleaching:
First section pH=10, chlorine dosage be to oven dry stock amount 2%, 37 ℃ of temperature, 130 minutes time.
Second section pH=3, chlorine dosage be to oven dry stock amount 0.35%, 20 minutes time.
(6) acid treatment: the hydrochloric acid consumption is to oven dry stock amount 3.5%, 40 minutes time, temperature normal temperature.
(7) dipping: 35 ℃ of dipping temperatures, concentration of lye 240g/l, dip time 24 minutes.
(8) squeezing: the fine content of first: 32.1%, caustic soda content 15.3%.
(9) experienced: temperature is 20 ℃.
(10) yellow: the carbon disulfide consumption is 33% of an alkali cellulose weight, 37 ℃ of finishing temperatures, 60 minutes time.
(11) spinning: acid bath liquid is formed: sulfuric acid 90g/l, and sodium sulphate 260g/l, zinc sulfate 39g/l, 40 ℃ of temperature are soaked long 450 millimeters.
(13) end product quality:
Do fracture strength: 2.23CN/dtex,
Wet breaking strength: 1.52CN/dtex,
Dried elongation at break: 23.3%,
The line density deviation ratio :+0.99%,
The length variation rate :-2.6%,
Overcut fibre: 0.4%,
Over-length fibre: 2.2mg/100g,
Residual sulfur content: 9.8mg/100g,
Fault: 2.1mg/100g,
Greasy dirt yellowish fiber: 0mg/100g,
Do the strong coefficient of variation: 15.40%,
Whiteness: 77.2%,
Oil content: 0.12%
Regain: 12.93%,
Grade: high-class product.
Embodiment 3
(1) preliminary treatment: liquor ratio 1: 3.5,180 ℃ of temperature, 100 minutes time.
(2) boiling: alkali charge in NaOH to oven dry stock amount 16%, liquor ratio 1: 6, hydrogen peroxide is to oven dry stock amount 3%, logical oxygen pressure 0.90Mpa heats up 240 minutes total times 132 ℃ of holding temperatures, temperature retention time 6 hours.
(3) chlorination: the chlorination chlorine dosage is to oven dry stock amount 4%, and it is dense 2.8% that chlorination is starched, time of chlorinating 40 minutes, chlorination temperature normal temperature.
(4) alkali refining: starch densely 10%, the NaOH consumption is to oven dry stock amount 6%, and 70 ℃ of extraction temperatures, hydrogen peroxide be to oven dry stock amount 1.5%, and logical amount of oxygen is to oven dry stock amount 0.6%, 60 minutes time.
(5) bleaching:
First section pH=11, chlorine dosage be to oven dry stock amount 3%, 35 ℃ of temperature, 180 minutes time.
Second section pH=4, chlorine dosage be to oven dry stock amount 0.5%, 10 minutes time.
(6) acid treatment: the hydrochloric acid consumption is to oven dry stock amount 5%, 20 minutes time, temperature normal temperature.
(7) dipping: 40 ℃ of dipping temperatures, concentration of lye 250g/l, dip time 10 minutes.
(8) squeezing: the fine content of first: 33.0%, caustic soda content 14.0%.
(9) experienced: temperature is 26 ℃.
(10) yellow: the carbon disulfide consumption is 35% of an alkali cellulose weight, 40 ℃ of finishing temperatures, 40 minutes time.
(11) spinning: acid bath liquid is formed: sulfuric acid 100g/l, and sodium sulphate 300g/l, zinc sulfate 45g/l, 45 ℃ of temperature are soaked long 400 millimeters.
(13) end product quality:
Do fracture strength: 2.24CN/dtex,
Wet breaking strength: 1.37CN/dtex,
Dried elongation at break: 24.7%,
The line density deviation ratio :+1.09%,
The length variation rate :-2.8%,
Overcut fibre: 0.5%,
Over-length fibre: 3.5mg/100g,
Residual sulfur content: 9.9mg/100g,
Fault: 2.2mg/100g,
Greasy dirt yellowish fiber: 0mg/100g,
Do the strong coefficient of variation: 14.18%,
Whiteness: 76.1%,
Oil content: 0.12%
Regain: 12.98%,
Grade: high-class product.
Embodiment 4
Basic process steps is identical with embodiment 1-3, and the condition of different is boiling and bleaching is different, wherein
1. boiling: total acid 5.0%, combined acid 1.0%, holding temperature is 140 ℃ for the first time, and temperature retention time is 60 minutes for the first time, and holding temperature is 165 ℃ for the second time, and temperature retention time is 120 minutes for the second time, 60 ℃ of fluid temperature, the degree of polymerization 700, first fibre 97.0%.
2. bleaching:
The I section: chlorine dosage is to oven dry stock amount 5%, and 55 ℃ of temperature, are bleached alkalinity 250g/m at 120 minutes time
3
The II section: acid treatment, 20 minutes time, is washed to and contains sour 0.5g/L oven dry stock amount 2% with acid amount;
The III section: chlorine dosage is to oven dry stock amount 3%, 40 ℃ of temperature, and bleaching contains alkali 150g/m
3, 180 minutes time, be washed to and contain sour 0.5g/L, whiteness: 78%, first fibre 94.5%, the degree of polymerization 670.
3. refining: 45 ℃ of wash water temperature, 70 ℃ of alkali cleaning temperature, alkali concn 6g/L, 50 ℃ of two wash water temperature, acid concentration 1.0g/L, pickling temperature normal temperature, 50 ℃ of three wash water temperature, last oil concentration 7g/L, last oil temperature normal temperature.Hydrogen peroxide bleaching concentration 0.05%, normal temperature, refining time 15 minutes.
End product quality:
Do fracture strength: 2.25CN/dtex,
Wet breaking strength: 1.33CN/dtex,
Dried elongation at break: 24.1%,
The line density deviation ratio :+0.61%,
The length variation rate :-5.6%,
Overcut fibre: 0.2%,
Over-length fibre: 3.2mg/100g,
Residual sulfur content: 8.0mg/100g,
Fault: 3.4mg/100g,
Greasy dirt yellowish fiber: 0.1mg/100g,
Do the strong coefficient of variation: 12.51%,
Whiteness: 76.2%,
Oil content: 0.15%,
Regain: 11.93%,
Grade: Grade A.
Embodiment 5
This embodiment is the same with embodiment 4, and just some process conditions is different, wherein:
1. boiling: total acid 7.0%, combined acid 2.0%, holding temperature is 135 ℃ for the first time, and temperature retention time is 80 minutes for the first time, and holding temperature is 155 ℃ for the second time, and temperature retention time is 180 minutes for the second time, 80 ℃ of fluid temperature, the degree of polymerization 750, first fibre 97.2%.
2. bleaching:
The I section: chlorine dosage is to oven dry stock amount 4%, and 48 ℃ of temperature, are bleached alkalinity 220g/m at 240 minutes time
3
The II section: acid treatment, 40 minutes time, is washed to and contains sour 0.3g/L oven dry stock amount 1.5% with acid amount;
The III section: chlorine dosage is to oven dry stock amount 1%, 30 ℃ of temperature, and bleaching contains alkali 130g/m
3, 60 minutes time, be washed to and contain sour 0.4g/L, whiteness: 77%, first fibre 93.1%, the degree of polymerization 760.
3. refining: 40 ℃ of wash water temperature, 60 ℃ of alkali cleaning temperature, alkali concn 8g/L, 55 ℃ of two wash water temperature, acid concentration 1.8g/L, pickling temperature normal temperature, 40 ℃ of three wash water temperature, last oil concentration 8g/L, last oil temperature normal temperature.Hydrogen peroxide bleaching concentration 0.10%, normal temperature, refining time 12 minutes.
End product quality:
Do fracture strength: 2.22CN/dtex,
Wet breaking strength: 1.50CN/dtex,
Dried elongation at break: 23.6%,
The line density deviation ratio :+0.77%,
The length variation rate :-2.7%,
Overcut fibre: 0.3%,
Over-length fibre: 3.0mg/100g,
Residual sulfur content: 8.7mg/100g,
Fault: 2.1mg/100g,
Greasy dirt yellowish fiber: 0mg/100g,
Do the strong coefficient of variation: 13.45%,
Whiteness: 77.4%,
Oil content: 0.11%,
Regain: 12.10%,
Grade: Grade A.
Embodiment 6
This embodiment is the same with embodiment 4, and just some process conditions is different, wherein:
1. boiling: total acid 8.0%, combined acid 3.0%, holding temperature is 120 ℃ for the first time, and temperature retention time is 120 minutes for the first time, and holding temperature is 140 ℃ for the second time, and temperature retention time is 240 minutes for the second time, 90 ℃ of fluid temperature.
2. bleaching:
The I section: chlorine dosage is to oven dry stock amount 2%, and 45 ℃ of temperature, are bleached alkalinity 200g/m at 180 minutes time
3
The II section: acid treatment, 50 minutes time, is washed to and contains sour 0.25g/L oven dry stock amount 1% with acid amount;
The III section: chlorine dosage is to oven dry stock amount 2%, 35 ℃ of temperature, and bleaching contains alkali 140g/m
3, 120 minutes time, be washed to and contain sour 0.5g/L, whiteness: 76%, first fibre 96%, the degree of polymerization 626.
3. refining: 50 ℃ of wash water temperature, 60 ℃ of alkali cleaning temperature, alkali concn 6g/L, 45 ℃ of two wash water temperature, acid concentration 0.6g/L, pickling temperature normal temperature, 40 ℃ of three wash water temperature, last oil concentration 6g/L, last oil temperature normal temperature.Hydrogen peroxide bleaching concentration 0.15%, normal temperature, refining time 10 minutes.
End product quality:
Do fracture strength: 2.24CN/dtex,
Wet breaking strength: 1.41CN/dtex,
Dried elongation at break: 24.7%,
The line density deviation ratio :+0.95%,
The length variation rate :-3.0%,
Overcut fibre: 0.4%,
Over-length fibre: 2.8mg/100g,
Residual sulfur content: 9.6mg/100g,
Fault: 2.3mg/100g,
Greasy dirt yellowish fiber: 0mg/100g,
Do the strong coefficient of variation: 15.20%,
Whiteness: 76.2%,
Oil content: 0.12%,
Regain: 12.90%,
Grade: Grade A.
Claims (10)
1. a bamboo viscose fiber is characterized in that: do fracture strength: 〉=1.90cN/dtex; Wet breaking strength: 〉=1.0cN/dtex; Dried elongation at break: 〉=16.0%; Line density deviation ratio: ± 7.00%; Length variation rate: ± 7.0%; Overcut fibre :≤1.0%; Over-length fibre :≤20.0mg/100g; Residual sulfur content :≤20.0mg/100g; Fault :≤12mg/100g; Adopt following conditions of cooking in its preparation process: alkali charge: in NaOH to oven dry stock amount 8-16%; Liquor ratio: 1: 4-6; H
2O
2: to oven dry stock amount 1-3%; Logical oxygen pressure: 0.70-0.90Mpa; Heated up total time: 150-240 minute; Holding temperature: 125-132 ℃; Temperature retention time: 6-11 hour.
2. viscose according to claim 1, it is characterized in that: adopt sulphite process (sodium base) boiling, its condition is: total acid is greater than 4%, combined acid is 1.0-3.0%, and the boiling maximum temperature is 165 ℃, adopts the secondary insulation: holding temperature: 120-140 ℃ for the first time, temperature retention time: 60-120 minute, holding temperature: 140-165 ℃ for the second time, temperature retention time: 120-240 minute, fluid temperature 60-90 ℃.
3. viscose according to claim 1 and 2, it is characterized in that: adopt two sections variate bleachings, condition is: first section pH=9-11, the chlorine dosage of oven dry stock is 1-3% relatively, temperature 35-38 ℃, time 90-180 minute, second section pH=2-4, the chlorine dosage 0.2-0.5% of relative oven dry stock, time 10-30 minute.
4. according to each viscose of aforementioned claim, it is characterized in that: adopt following conditions of bleaching: the bleaching of I section: chlorine dosage is 2-5% to the consumption of oven dry stock, temperature 45-55 ℃, and bleaching alkalinity≤250g/m
3, bleaching time 120-240 minute; II section bleaching: the oven dry stock acid treatment with acid amount 1-2%, time 20-50 minute, is washed to below the acid content 0.5g/L; The bleaching of III section: to the bleaching chlorine dosage 1-3% of oven dry stock, temperature 30-40 ℃, bleaching alkalinity≤150g/m
3, bleaching time 60-180 minute, be washed till residual acid≤0.5g/L.
5. according to each viscose of aforementioned claim, it is characterized in that: refining condition is: 40-50 ℃ of a wash water temperature, 60-70 ℃ of alkali cleaning temperature, alkali concn 6-8g/l, 45-55 ℃ of two wash water temperature, three wash temperature 40-50 ℃, last oil concentration 6-8g/l, last oil temperature normal temperature, hydrogen peroxide bleaching concentration 0.05-0.15%, bleaching temperature normal temperature, refining time 10-15 minute.
6. method for preparing one of claim 1-5 viscose comprises: processing such as boiling, bleaching, acid treatment, refining, it is characterized in that: conditions of cooking is: alkali charge: in NaOH to oven dry stock amount 8-16%; Liquor ratio: 1: 4-6; H
2O
2: to oven dry stock amount 1-3%; Logical oxygen pressure: 0.70-0.90Mpa; Heated up total time: 150-240 minute; Holding temperature: 125-132 ℃; Temperature retention time: 6-11 hour.
7. method for preparing one of claim 1-5 viscose, it is characterized in that: adopt sulphite process (sodium base) boiling, total acid is greater than 4%, combined acid is 1.0-3.0, and the boiling maximum temperature is 165 ℃, adopts the secondary insulation: holding temperature: 120-140 ℃ for the first time, temperature retention time: 60-120 minute, holding temperature: 140-165 ℃ for the second time, temperature retention time: 120-240 minute, fluid temperature 60-90 ℃.
8. method according to claim 6 is characterized in that: adopt two sections variate bleachings, condition is:
First section pH=9-11, the chlorine dosage of oven dry stock is 1-3% relatively, temperature 35-38 ℃, time 90-180 minute,
Second section pH=2-4, the chlorine dosage 0.2-0.5% of relative oven dry stock, time 10-30 minute.
9. method according to claim 7 is characterized in that, adopts following conditions of bleaching: the bleaching of I section: chlorine dosage is 2-5% to the consumption of oven dry stock, temperature 45-55 ℃, and bleaching alkalinity≤250g/m
3, bleaching time 120-240 minute; II section bleaching: the oven dry stock acid treatment with acid amount 1-2%, time 20-50 minute, is washed to below the acid content 0.5g/L; The bleaching of III section: to the bleaching chlorine dosage 1-3% of oven dry stock, temperature 30-40 ℃, bleaching alkalinity≤150g/m
3, bleaching time 60-180 minute, be washed till residual acid≤0.5g/L.
10. according to each method of claim 6-9, it is characterized in that: refining condition is: 40-50 ℃ of a wash water temperature, 60-70 ℃ of alkali cleaning temperature, alkali concn 6-8g/l, 45-55 ℃ of two wash water temperature, three wash temperature 40-50 ℃, last oil concentration 6-8g/l, last oil temperature normal temperature, hydrogen peroxide bleaching concentration 0.05-0.15%, bleaching temperature normal temperature, refining time 10-15 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031284965A CN1194119C (en) | 2002-05-14 | 2003-05-08 | Bamboo Viscose fibre and its preparing method |
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN02117667.1 | 2002-05-14 | ||
| CN 02117667 CN1381620A (en) | 2002-05-14 | 2002-05-14 | Viscose rayon made of bamboo and its preparing process |
| CN02130026.7 | 2002-08-13 | ||
| CN 02130026 CN1399011A (en) | 2002-08-13 | 2002-08-13 | Bamboo viscose fiber and its production process |
| CNB031284965A CN1194119C (en) | 2002-05-14 | 2003-05-08 | Bamboo Viscose fibre and its preparing method |
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| CN1458306A CN1458306A (en) | 2003-11-26 |
| CN1194119C true CN1194119C (en) | 2005-03-23 |
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| CN1294322C (en) * | 2004-04-23 | 2007-01-10 | 赵子群 | Process for preparing bamboo grout cakes used for production of secondary cellulose acetate sheets |
| CN1296533C (en) * | 2004-10-18 | 2007-01-24 | 保定天鹅股份有限公司 | Bamboo pulp regenerated cellulose viscose filament rayon and preparing method |
| CN100558952C (en) * | 2007-03-24 | 2009-11-11 | 山东海龙股份有限公司 | Bamboo charcoal viscose fiber and its manufacturing method |
| FR2941465B1 (en) | 2009-01-27 | 2011-04-29 | Oreal | COSMETIC PRODUCT APPLICATION DEVICE COMPRISING BAMBOO FIBERS AND METHOD OF MANUFACTURING THE SAME |
| CN103572631B (en) * | 2013-11-11 | 2015-04-22 | 新疆富丽达纤维有限公司 | Preparation method of pulp for regenerating papermaking pulp into viscose staple fiber |
| CN106283223B (en) * | 2015-05-18 | 2019-10-01 | 吉林化纤股份有限公司 | Spinning head used in the preparation method and preparation process of flat viscose filament yarn |
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