CN103556249B - A kind of palm viscose and preparation method thereof - Google Patents
A kind of palm viscose and preparation method thereof Download PDFInfo
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- 229920000297 Rayon Polymers 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000003513 alkali Substances 0.000 claims abstract description 71
- 238000000034 method Methods 0.000 claims abstract description 46
- 238000007598 dipping method Methods 0.000 claims abstract description 31
- 230000008569 process Effects 0.000 claims abstract description 24
- 238000009835 boiling Methods 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 238000009987 spinning Methods 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- 238000004061 bleaching Methods 0.000 claims abstract description 12
- 239000000835 fiber Substances 0.000 claims description 63
- 239000002002 slurry Substances 0.000 claims description 37
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- 238000010411 cooking Methods 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 16
- 235000013399 edible fruits Nutrition 0.000 claims description 12
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000428 dust Substances 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 239000003292 glue Substances 0.000 claims description 6
- 230000008676 import Effects 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 claims description 5
- 150000004056 anthraquinones Chemical class 0.000 claims description 5
- 230000000740 bleeding effect Effects 0.000 claims description 5
- 230000001112 coagulating effect Effects 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 5
- 230000029087 digestion Effects 0.000 claims description 5
- 238000002386 leaching Methods 0.000 claims description 5
- 230000014759 maintenance of location Effects 0.000 claims description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 5
- 235000011152 sodium sulphate Nutrition 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- 239000011593 sulfur Substances 0.000 claims description 5
- 239000002562 thickening agent Substances 0.000 claims description 5
- 238000010407 vacuum cleaning Methods 0.000 claims description 5
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 5
- 229960001763 zinc sulfate Drugs 0.000 claims description 5
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000002166 wet spinning Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000010306 acid treatment Methods 0.000 abstract description 5
- 230000004069 differentiation Effects 0.000 abstract description 4
- 238000013459 approach Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000007380 fibre production Methods 0.000 abstract description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract description 2
- 238000012805 post-processing Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 229920002488 Hemicellulose Polymers 0.000 description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 11
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 8
- 229920001131 Pulp (paper) Polymers 0.000 description 6
- 239000007844 bleaching agent Substances 0.000 description 6
- 238000007670 refining Methods 0.000 description 6
- 229920000742 Cotton Polymers 0.000 description 5
- 241000219000 Populus Species 0.000 description 5
- 229920002678 cellulose Polymers 0.000 description 5
- 239000001913 cellulose Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 229920005610 lignin Polymers 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 description 4
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 4
- 235000019341 magnesium sulphate Nutrition 0.000 description 4
- 238000004537 pulping Methods 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 3
- 235000017491 Bambusa tulda Nutrition 0.000 description 3
- 241001330002 Bambuseae Species 0.000 description 3
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 3
- 240000000961 Setaria parviflora Species 0.000 description 3
- 239000011425 bamboo Substances 0.000 description 3
- 238000003908 quality control method Methods 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- 238000007493 shaping process Methods 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 239000004155 Chlorine dioxide Substances 0.000 description 2
- 229920000875 Dissolving pulp Polymers 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 235000019398 chlorine dioxide Nutrition 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 150000002972 pentoses Chemical class 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000006424 Flood reaction Methods 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010036 direct spinning Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000011121 hardwood Substances 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005956 quaternization reaction Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 230000000192 social effect Effects 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- Artificial Filaments (AREA)
Abstract
The present invention relates to a kind of viscose produced for raw material with palm discarded object and preparation method thereof, its step comprises: preliminary treatment, boiling, shove, washing, front choosing, concentrated, oxygen delignification, bleaching, acid treatment, washing, pressure screens, concentrated, squeezing, a thermokalite dipping, squeezing, secondary alkali steeping, squeezing, experienced, yellow, grinding, dissolve, filter, deaeration, spinning, post processing, dry, this patent of invention solves palm and prepares difficult point in pulp and Making viscose procedure of fibre production, production process technology flow process is simple, be not only viscose and provide a kind of new raw material, add raw material differentiation rate, and provide a kind of new approach for processing palm discarded object in a large number, decrease environmental pollution, what improve palm discarded object utilizes added value.
Description
Technical field
The present invention relates to a kind of viscose and preparation method thereof, specifically relate to a kind of viscose produced for raw material with palm discarded object and preparation method thereof, belong to textile technology field.
Background technology
Cellulosic fibre is viscose mainly, and due to good hygroscopicity, comfortable and easy to wear, spinnability is excellent, is widely used, and Chang Yumian, hair or various synthetic fiber blending, intertexture, for all kinds of clothes and decorative textile product, be well received by consumers.At present, what in viscose raw material, application was ripe mainly contains cotton pulp and wood pulp, also has a small amount of numb material and timber, and by the impact that cultivated land resource restriction and output of cotton increase, cotton linter resource increases will be subject to larger restriction.Conventional processing methods is produced Cotton Pulp and is consumed high, and black liquor waste pollutes large, if Cotton Pulp does not solve black liquor problem, will progressively be replaced by wood pulp; In wood pulp application aspect, external fast growing wood development is more ripe, and China's area of woods is limited, and the fast growing wood production cycle is longer, and purposes is comparatively wide, and only papermaking just consumes a large amount of timber every year, causes resource fewer and feweri, wood pulps major part dependence on import; The numb material of part, bamboo wood through coming unstuck, except lignin after can direct spinning, and higher by numb material, bamboo material price, greatly increase production cost, the ratio therefore accounted in viscose raw material is little.Raw material is differential is the important directions that the viscose differentiation of product develops, and develops the viscose raw material made new advances and not only can alleviate raw material problem in short supply, also have impetus to whole industry.
Along with oil, natural gas etc. more can not face exhaustion by new resources, country more and more payes attention to the utilization of biomass energy.Palm original producton location is western part and the middle part in Africa, and Malaysia and south east asia are planted all in a large number.In Malaysia, palm is most important economic plants, and annual generation 3,000 ten thousand tons of discarded objects, comprise trunk, compound leaf and empty fruit cluster.The hollow palm fruit string fiber of annual generation, namely the empty fruit cluster after palm fruit string excision oil fruit, through de-oiling, extract, tear after produce fiber, about 4,000,000 tons, up to now there is no and find suitable processing method, the overwhelming majority makes landfill and burning disposal, both wastes resource, pollute environment again, this resource of efficient and rational exploitation has higher economic worth and social effect.Analyze from the raw material aspect of viscose pulp, compare with fast growing hard wood poplar, hollow palm fruit string fiber belongs to moderate-length fiber, fibre length is slightly shorter than poplar, the larger wall of lumen is thin, nitric acid in chemical composition-ethanol content of cellulose is lower than poplar 8%, but poly-pentose is lower than poplar 10%, Klason lignin content is also a little less than poplar, with pulping and paper-making unlike, Making viscose fiber pulp as far as possible only retains alpha cellulose in producing, and removes the impurity such as hemicellulose (mostly being poly-pentose) and lignin.Palm filament inner hollow, moisture pick-up properties is excellent, good permeability, Anti-moth-eating, and fiber softening degree is higher, and becoming that discarded object throws away is the great wasting of resources.
The utilization of palm discarded object has caused the attention of pulping and papermaking industry, but still blank in textile fabric field.Novel biomass resource-palm viscose the abundant raw material source of developing green environmental protection, cheap, belong to the high added value recycling of discarded object, there is great potential and broad based growth prospect.Pulping and paper-making requires to retain cellulose and hemicellulose as far as possible, and viscose pulp requires to remove hemicellulose as far as possible, because hemicellulose molecule chain is shorter, in viscose is produced, all harmful effect is produced to working procedures such as dipping, experienced, yellows.Therefore comparatively papermaking is high for viscose pulp requirement alpha cellulose purity.No matter pulping is chemical pulp or mechanical pulp, the fiber fineness that boiling goes out all does not reach the requirement of viscose pulp, as publication number be CN1332293A to patent discloses a kind of take palm shell as the method for raw pulp papermaking, NaOH consumption 18-22%, publication number be CN1737254A patent discloses a kind of continuously boiling hollow palm fruit string fiber pulp and paper making method, active alkali consumption 15-20%, test finds, palm prepares dissolving pulp under low alkali charge, the lignin of the thick slurry residual after boiling and hemicellulose all do not reach the requirement of viscose pulp.
In the spinning solution viscose glue preparation process of producing viscose, impregnation technology is immersed in sodium hydroxide solution by the pulp of drying to carry out quaternization, generates alkali cellulose.Now very great Viscose Fiber Plant is all that the fine integration of slurry is produced, can design completely need not be dry pulp, directly carrying out alkali steeping with squeezing out the wet pulp dregs of rice after certain moisture, dipping not only can be made more even, and save a large amount of steam.Be squeezing process after dipping process, effect squeezes out by unnecessary alkali lye in slurry congee with squeezer.If the fiber of pulp is shorter, hemicellulose level is high, and squeezer stock tank pressure will be caused high, blocking filter screen.The patent No. is the short route low-energy-consumption production method that the Chinese patent of ZL201110049019.1 discloses a kind of bamboo viscose fiber, adopt technique to be that pulp is without manufacturing paper with pulp, directly flood, wherein in impregnation technology first time dipping temperature 35 ~ 45 DEG C, NaOH concentration 600 ~ 650g/l, it is longer that this technique is only applicable to fiber, the pulp that content of alphacellulose is higher, if hemicellulose content is high, fibre length is shorter, at 35 ~ 45 DEG C of temperature, hemicellulose stripping quantity in short time in treating tank in alkali fibre is not high, the fiber of Small molecular chain blocks squeezer filter screen, cause squeezing quality uneven, squeezer efficiency is low, affect spinning output.
Summary of the invention
The present invention is directed to the problems referred to above, provide a kind of palm viscose and production method thereof, solution palm prepares the difficult point in pulp and Making viscose procedure of fibre production, production process technology flow process is simple, be not only viscose and provide a kind of new raw material, add raw material differentiation rate, and provide a kind of new approach for processing palm discarded object in a large number, decrease environmental pollution, what improve palm discarded object utilizes added value.
For achieving the above object, the technical solution used in the present invention is: a kind of palm viscose, is characterized in that: raw material are hollow palm fruit string fiber or palm trunk, compound leaf, through the viscose that wet spinning is prepared from.
Below the further improvement to technique scheme:
Described a kind of palm viscose, its technical indicator is as follows: dry fracture strength > 2.20cN/dtex, wet breaking strength > 1.25cN/dtex, dry elongation at break > 18.0%.
Described a kind of palm viscose, it is characterized in that: its technical indicator is as follows: line density deviation ratio ± 1.5%, length variation rate ± 2.4%, overcut fibre≤0.4%, over-length fibre≤2.7mg/100g, residual sulfur content≤7.4mg/100g, fault≤2.5mg/100g, the dry strong coefficient of variation≤10.2%.
A preparation method for palm viscose, comprises cooking process, in described cooking process, and boiling slurry index: alpha cellulose >=90.0%, viscosity 11.2 ~ 14.8mpa.s, permanganate number 4.5 ~ 7.8.
In described cooking process: cooking liquor addition counts 30% ~ 35% of relative over dry palm material quality with NaOH; Cooking liquor sulphidity is 18% ~ 20%.; Digesting assistant anthraquinone addition is 0.05% ~ 0.2% of relative over dry palm material quality; Liquor ratio is 1:3.0 ~ 6.0; Cooking liquor temperature 80 ~ 90 DEG C; Write a prescription liquid circulating pump SAPMAC method 10 ~ 20min; Add steam to heat up, point secondary temperature elevation, wherein 30 ± 5 minutes heating-up time, pressure 0.30 ± 0.03Mpa in boiling vessel, once 10 ± 2 minutes little steam bleeding time, in boiling vessel, overbottom pressure is normal pressure; 40 ± 5 minutes secondary temperature elevation time, temperature rises to 140 ~ 170 DEG C, temperature retention time 120 ~ 180min.。
A preparation method for palm viscose, also comprises shove operation, in described shove operation, and black digestion liquid residual alkali 22.3-29.6 g/l, shove disposed slurry mass dryness fraction 15 ~ 25%.
A preparation method for palm viscose, also comprises dipping process, in described dipping process, floods at twice, a high-temperature concentrated alkali dipping temperature: 90 ~ 100 DEG C, single-steeping naoh concentration: 400 ~ 420g/l; Double-steeping leaching temperature: 50 ~ 55 DEG C, dipping naoh concentration: 180 ~ 190g/l.
A preparation method for palm viscose, also comprises washing procedure, carries out hot water vacuum cleaning in described washing procedure, water temperature 50 ~ 60 DEG C, vacuum: 0.01 ~ 0.03Mpa; Washing disposed slurry index: ash content mass content≤1.2%, iron divides≤140mg/kg.
A preparation method for palm viscose, also comprises oxygen delignification operation, in described oxygen delignification operation, alkali charge to oven dry stock 2 ~ 3%, temperature 85 ~ 95 DEG C, oxygen pressure 0.3 ~ 0.5Mpa, time 50 ~ 80min.
A preparation method for palm viscose, is characterized in that: further comprising the steps of:
Before select operation, select in operation before described, slurry desanding concentration 0.5 ~ 1.5%, desanding pressure is 0.25 ~ 0.35Mpa;
Enrichment process, in described enrichment process, thickener outlet slurry dense 3 ~ 5%;
Bleaching process, in described bleaching process, viscosity: 9.1 ~ 10.8mpa.s after drift;
Decker concentrates and squeezing process, is concentrated to direct squeezing after slurry dense 3 ~ 5% is condensed into palm pulp through decker.Pulp after described squeezing moisture 50 ~ 55%.Described pulp technical performance index: alpha cellulose mass content>=88.0%, viscosity 9.0 ~ 11.8mpa.s, ash content mass content≤0.14%, iron divides≤30mg/kg, whiteness>=76%, little dust≤180mm
2/ kg, large dust≤1.0/kg;
Squeezing subsequent pulverization step, the fine first fibre of the rear alkali of described pulverizing 22 ~ 28%, alkali fibre contains alkali 15 ~ 18%, the fine first fibre 28 ~ 31% of secondary alkali, and secondary alkali fibre is containing alkali 13 ~ 15%;
Experienced operation, fine half fine content≤3% of described experienced import alkali, cuprammonium viscosity 5.1 ~ 6.0mpa.s, fine half fine content≤8% of outlet alkali;
Yellow operation, in described yellow operation, CS
2be 31 ~ 34% to the fine addition of first, yellow time 30 ~ 60min;
Dissolving, mixing, filtration, bubble removal step, through the spinning glue that above-mentioned operation is obtained, quality is first fibre 7.0 ~ 9.2%, containing alkali 4.0 ~ 4.98%, viscosity 30 ~ 48s, degree of ripeness 10.2 ~ 18ml;
Spinning process, in described spinning process, coagulating bath adopts sulfuric acid 100 ~ 150g/l, sodium sulphate 300 ~ 350g/l, zinc sulfate 10 ~ 20g/l, temperature 35 ~ 55 DEG C.
Beneficial effect of the present invention:
1, the invention provides a kind of raw material of new Making viscose fiber, the palm viscose performance indications prepared by this method are excellent, expand the raw material field of viscose, alleviate viscose pulp material shortage problem, increase the raw material differentiation rate of viscose.
2, the present invention processes the approach that discarded hollow palm fruit string fiber provides a kind of high added value in a large number, and solution palm discards the problem of environmental pollution that empty fruit cluster fiber causes.
3, digesting technoloy provided by the invention can for palm raw material, cellulose of effectively purifying, and stripping major part impurity, slurry reaches dissolving pulp index request.
4, the present invention adopts pulp not dry, and after squeezing, the method for direct high-temperature concentrated alkali dipping, not only save and dry cost, and dipping is more even, effectively removes hemicellulose, keep squeezer pressure stability.
5, preparation method of the present invention is simple, easy to operate, economize energy, and can be realized by conventional pulp, viscose fiber production line.
Detailed description of the invention
Except as otherwise noted, described in the present invention, percentage is mass percent.
embodiment 1
The preparation method of palm viscose of the present invention, its step comprises: preliminary treatment, boiling, shove, washing, front choosing, concentrated, oxygen delignification, bleaching, acid treatment, washing, pressure screening, concentrated, squeezing, thermokalite dipping, squeezing, secondary alkali steeping, squeezing, experienced, yellow, grinding, dissolving, filtration, deaeration, spinning, post processing, oven dry.
It is as follows that pulp prepares concrete steps:
(1) preliminary treatment: segment monkey grass being cut to 3-5cm, enters the impurity such as dry type desander removing sand.
(2) boiling: cooking liquor addition counts 30% of relative over dry palm material quality with NaOH, cooking liquor sulphidity is 20%, digesting assistant anthraquinone addition is 0.05% of relative over dry palm material quality, and liquor ratio is 1:3.0, cooking liquor temperature 80 DEG C, write a prescription and start to add steam after liquid circulating pump SAPMAC method 10min and heat up, divide secondary temperature elevation, wherein 30 minutes heating-up time, pressure 0.30Mpa in boiling vessel, the once 10 minutes little steam bleeding time, in boiling vessel, overbottom pressure is normal pressure; 40 minutes secondary temperature elevation time, temperature rises to 170 DEG C, temperature retention time 120min;
Boiling slurry index: alpha cellulose 90.5%, viscosity 13.1mpa.s, permanganate number 6.3.
(3) shove: the palm slurry Var-nip press spurted concentrates, the residual alkali 22.3g/l of black digestion liquid, shove disposed slurry mass dryness fraction 15%.
(4) wash: carry out hot water vacuum cleaning, water temperature 50 DEG C, vacuum: 0.015Mpa;
Washing disposed slurry index: ash content mass content 1.05%, iron divides 120mg/kg.
(5) front choosing: slurry desanding concentration 0.5%, desanding pressure is 0.25Mpa.
(6) concentrated: thickener outlet slurry dense 3%.
(7) oxygen delignification: alkali charge to oven dry stock 2%, magnesium sulfate addition to oven dry stock 0.3%, temperature 85 DEG C, oxygen pressure 0.5Mpa, time 50min.
(8) bleach: adopt hydrogen peroxide as bleaching agent, bleaching temperature 45 DEG C, sodium metasilicate addition is 2% of relative over dry stock quality, and magnesium sulfate addition is 0.5% of relative over dry stock quality, hydrogen peroxide addition is 8% of relative over dry stock quality, bleaching time 60min;
Viscosity: 9.1mpa.s after drift;
Again through acid treatment, washing, pressure screening, be concentrated to direct squeezing after slurry dense 3% through decker and be condensed into palm pulp, the pulp after squeezing moisture 55%;
Adopt said method produce pulp quality: alpha cellulose mass content 88.5%, viscosity 9.0mpa.s, ash content mass content 0.12%, iron divides 26mg/kg, whiteness 78%, little dust 152mm
2/ kg, large dust 1.0/kg.
Above-mentioned pulp is carried out viscose production, comprises the following steps: dipping, squeezing, pulverize, experienced, yellow, dissolving, mixing, filtration, deaeration, spinning, cut-out, refining, baking operation, concrete steps are as follows:
Dipping: high-temperature concentrated alkali dipping temperature 90 DEG C, single-steeping naoh concentration 420g/l, double-steeping leaching temperature 50 DEG C, dipping uses naoh concentration 190g/l;
Hollow palm fruit string fiber single fiber is shorter, because raw material is higher containing lignin, hemicellulose is higher, viscosity could be dropped to stronger digesting technoloy the scope that viscose pulp requires, and the fiber of Small molecular chain is more, because of pulp continuously in treating tank with alkaline reaction, the conventional dipping temperature of about 50 DEG C, there is the time of staying short, hemicellulose is residual many, difficulty is squeezed after causing alkali fibre dipping, the problem that stock tank pressure is high, hemicellulose level is high, cause experienced viscosity unstable, the disadvantages such as yellow side reaction is many, for solving the problem, the present invention adopts high-temperature concentrated alkali to flood, effective removal hemicellulose and the short fiber of strand, improve cellulose purity.
Pulverize after squeezing: pulverize the fine first fibre of a rear alkali 22%, alkali fibre containing alkali 18%, the fine first fibre 28% of secondary alkali, secondary alkali fibre is containing alkali 15%.
Experienced: the fine half fine content 2.2% of import alkali, cuprammonium viscosity 5.1mpa.s, the fine half fine content 6.2% of outlet alkali.
Yellow: CS2 is 31% to the fine addition of first, yellow time 60min.
Obtain spinning glue through dissolving, mixing, filtration, deaeration after yellow, quality control is first fibre 7.0%, containing alkali 4.98%, and viscosity 48s, degree of ripeness 10.2ml.
Spinning: coagulating bath adopts sulfuric acid 100g/l, sodium sulphate 300g/l, zinc sulfate 10g/l, temperature 55 DEG C;
Tow after shaping makes viscose through cut-out, refining, oven dry.
Employing the present embodiment obtains end properties index and is: dry fracture strength 2.23cN/dtex, wet breaking strength 1.31cN/dtex, dry elongation at break 19.5%, line density deviation ratio+0.8%, length variation rate+3%, overcut fibre 0.2%, over-length fibre 2.2mg/100g, residual sulfur content 6.0mg/100g, fault 2.1mg/100g, the dry strong coefficient of variation 13.0%.
embodiment 2
(1) preliminary treatment: segment monkey grass being cut to 3-5cm, enters the impurity such as dry type desander removing sand.
(2) boiling: cooking liquor addition counts 35% of relative over dry palm material quality with NaOH, and cooking liquor sulphidity is 18%, digesting assistant anthraquinone addition is 0.5% of relative over dry palm material quality, and liquor ratio is 1:5.0, cooking liquor temperature 90 DEG C.Write a prescription and start to add steam after liquid circulating pump SAPMAC method 20min and heat up, point secondary temperature elevation, wherein 35 minutes heating-up time, pressure 0.33Mpa in boiling vessel, once 12 minutes little steam bleeding time, in boiling vessel, overbottom pressure is normal pressure; 35 minutes secondary temperature elevation time, temperature rises to 140 DEG C, temperature retention time 150min;
Boiling slurry index: alpha cellulose 91.1%, viscosity 14.8mpa.s, permanganate number 7.8.
(3) shove: the palm slurry Var-nip press spurted concentrates, the residual alkali 25.4g/l of black digestion liquid, shove disposed slurry mass dryness fraction 18%.
(4) wash: carry out hot water vacuum cleaning, water temperature 55 DEG C, vacuum: 0.025Mpa.
Washing disposed slurry index: ash content mass content 1.13%, iron divides 138mg/kg.
(5) front choosing: slurry desanding concentration 0.8%, desanding pressure is 0.29Mpa.
(6) concentrated: thickener outlet slurry dense 4%.
(7) oxygen delignification: alkali charge to oven dry stock 2.5%, magnesium sulfate addition to oven dry stock 0.4%, temperature 90 DEG C, oxygen pressure 0.3Mpa, time 80min.
(8) bleach: adopt clorox as bleaching agent, bleaching temperature 50 DEG C, sulfamic acid addition is residual chlorine 0.6g/l, bleaching time 60min in 1%, ten minutes of relative over dry stock quality;
Viscosity: 10.8mpa.s after drift.
(9) again through acid treatment, washing, pressure screening, be concentrated to direct squeezing after slurry dense 4% through decker and be condensed into palm pulp, the pulp after squeezing moisture 53%.
Adopt said method produce pulp quality: alpha cellulose mass content 89.1%, viscosity 11.8mpa.s, ash content mass content 0.10%, iron divides 20mg/kg, whiteness 76%, little dust 148mm
2/ kg, large dust 0.8/kg.
Above-mentioned pulp is carried out viscose production, and step comprises: dipping, squeezing, pulverize, experienced, yellow, dissolving, mixing, filtration, deaeration, spinning, cut-out, refining, baking operation, concrete steps are as follows:
Dipping: high-temperature concentrated alkali dipping temperature 95 DEG C, single-steeping naoh concentration 410g/l, double-steeping leaching temperature 55 DEG C, dipping uses naoh concentration 180g/l.
Pulverize after squeezing: pulverize the fine first fibre of a rear alkali 26%, alkali fibre containing alkali 16%, the fine first fibre 29% of secondary alkali, secondary alkali fibre is containing alkali 14%.
Experienced: the fine half fine content 2.8% of import alkali, cuprammonium viscosity 5.8mpa.s, the fine half fine content 7.3% of outlet alkali.
Yellow: CS2 is 32% to the fine addition of first, yellow time 50min.
Obtain spinning glue through dissolving, mixing, filtration, deaeration after yellow, quality control is first fibre 8.3%, containing alkali 4.55%, and viscosity 30s, degree of ripeness 18ml.
Spinning: coagulating bath adopts sulfuric acid 120g/l, sodium sulphate 330g/l, zinc sulfate 16g/l, temperature 45 C.
Tow after shaping makes viscose through cut-out, refining, oven dry.
Employing the present embodiment obtains end properties index and is: dry fracture strength 2.42cN/dtex, wet breaking strength 1.42cN/dtex, dry elongation at break 18.3%, line density deviation ratio+1.5%, length variation rate+1.6%, overcut fibre 0.4%, over-length fibre 2.7mg/100g, residual sulfur content 7.4mg/100g, fault 2.5mg/100g, the dry strong coefficient of variation 10.2%.
embodiment 3
(1) preliminary treatment: segment monkey grass being cut to 3-5cm, enters the impurity such as dry type desander removing sand.
(2) boiling: cooking liquor addition counts 33% of relative over dry palm material quality with NaOH, and cooking liquor sulphidity is 19%, digesting assistant anthraquinone addition is 0.2% of relative over dry palm material quality, and liquor ratio is 1:6.0, cooking liquor temperature 85 DEG C.Write a prescription and start to add steam after liquid circulating pump SAPMAC method 15min and heat up, point secondary temperature elevation, wherein 25 minutes heating-up time, pressure 0.27Mpa in boiling vessel, once 8 minutes little steam bleeding time, in boiling vessel, overbottom pressure is normal pressure; 45 minutes secondary temperature elevation time, temperature rises to 160 DEG C, temperature retention time 180min.
Boiling slurry index: alpha cellulose 90.2%, viscosity 11.2mpa.s, permanganate number 4.5.
(3) shove: the palm slurry Var-nip press spurted concentrates, the residual alkali 29.6g/l of black digestion liquid, shove disposed slurry mass dryness fraction 25%.
(4) wash: carry out hot water vacuum cleaning, water temperature 60 DEG C, vacuum: 0.03Mpa.
Washing disposed slurry index: ash content mass content 0.98%, iron divides 110mg/kg.
(5) front choosing: slurry desanding concentration 1.5%, desanding pressure is 0.35Mpa.
(6) concentrated: thickener outlet slurry dense 5%.
(7) oxygen delignification: alkali charge to oven dry stock 3%, magnesium sulfate addition to oven dry stock 0.6%, temperature 95 DEG C, oxygen pressure 0.4Mpa, time 70min.
(8) bleach: adopt chlorine dioxide as bleaching agent, add hydrochloric acid size mixing material PH to 3.5, bleaching temperature 70 DEG C, chlorine dioxide addition to oven dry stock 4.0%, bleaching time 60min;
Viscosity: 10.8mpa.s after drift.
(9) again through acid treatment, washing, pressure screening, be concentrated to direct squeezing after slurry dense 5% through decker and be condensed into palm pulp, the pulp after squeezing moisture 50%.
Adopt said method produce pulp quality: alpha cellulose mass content 88.3%, viscosity 10.3mpa.s, ash content mass content 0.11%, iron divides 18mg/kg, whiteness 78%, little dust 174mm
2/ kg, large dust 0.9/kg.
Above-mentioned pulp is carried out viscose production, and step comprises: dipping, squeezing, pulverize, experienced, yellow, dissolving, mixing, filtration, deaeration, spinning, cut-out, refining, baking operation, specific as follows.
Dipping: high-temperature concentrated alkali dipping temperature 100 DEG C, single-steeping naoh concentration 400g/l.Double-steeping leaching temperature 53 DEG C, dipping uses naoh concentration 185g/l.
Pulverize after squeezing: pulverize the fine first fibre of a rear alkali 28%, alkali fibre containing alkali 15%, the fine first fibre 31% of secondary alkali, secondary alkali fibre is containing alkali 13%.
Experienced: the fine half fine content 2.6% of import alkali, cuprammonium viscosity 6.0mpa.s, the fine half fine content 6.3% of outlet alkali.
Yellow: CS2 is 34% to the fine addition of first, yellow time 30min.
Obtain spinning glue through dissolving, mixing, filtration, deaeration after yellow, quality control is first fibre 9.2%, containing alkali 4.03%, and viscosity 42s, degree of ripeness 16ml.
Spinning: coagulating bath adopts sulfuric acid 150g/l, sodium sulphate 350g/l, zinc sulfate 20g/l, temperature 35 DEG C.
Tow after shaping makes viscose through cut-out, refining, oven dry.
Employing the present embodiment obtains end properties index and is: dry fracture strength 2.38cN/dtex, wet breaking strength 1.29cN/dtex, dry elongation at break 20.1%, line density deviation ratio ﹣ 0.8%, length variation rate+2.4%, overcut fibre 0.2%, over-length fibre 1.3mg/100g, residual sulfur content 6.2mg/100g, fault 2.3mg/100g, the dry strong coefficient of variation 8.5%.
Claims (8)
1. a preparation method for palm viscose, is characterized in that: raw material are hollow palm fruit string fiber or palm trunk, compound leaf, through the viscose that wet spinning is prepared from;
The preparation method of described palm viscose, comprises cooking process, in described cooking process, and boiling slurry index: first fibre >=90.0%, viscosity 11.2 ~ 14.8mPa.s, permanganate number 4.5 ~ 7.8;
Cooking liquor addition counts 30% ~ 35% of relative over dry palm material quality with NaOH; Cooking liquor sulphidity is 18% ~ 20%; Digesting assistant anthraquinone addition is 0.05% ~ 0.2% of relative over dry palm material quality; Liquor ratio is 1:3.0 ~ 6.0; Cooking liquor temperature 80 ~ 90 DEG C; Write a prescription liquid circulating pump SAPMAC method 10 ~ 20min; Add steam to heat up, point secondary temperature elevation, wherein a heating-up time 30 ± 5min, pressure 0.30 ± 0.03MPa in boiling vessel, once little steam bleeding time 10 ± 2min, in boiling vessel, overbottom pressure is normal pressure; Secondary temperature elevation time 40 ± 5min, temperature rises to 140 ~ 170 DEG C, temperature retention time 120 ~ 180min.
2. the preparation method of a kind of palm viscose according to claim 1, is characterized in that: also comprise shove operation, in described shove operation, and black digestion liquid residual alkali 22.3-29.6 g/L, shove disposed slurry mass dryness fraction 15 ~ 25%.
3. the preparation method of a kind of palm viscose according to claim 1, it is characterized in that: also comprise dipping process, in described dipping process, dipping at twice, a high-temperature concentrated alkali dipping temperature: 90 ~ 100 DEG C, single-steeping naoh concentration: 400 ~ 420g/L; Double-steeping leaching temperature: 50 ~ 55 DEG C, dipping naoh concentration: 180 ~ 190g/L.
4. the preparation method of a kind of palm viscose according to claim 1, is characterized in that: also comprise washing procedure, carries out hot water vacuum cleaning in described washing procedure, water temperature 50 ~ 60 DEG C, vacuum: 0.01 ~ 0.03MPa; Washing disposed slurry index: ash content mass content≤1.2%, iron divides≤140mg/kg.
5. the preparation method of a kind of palm viscose according to claim 1, is characterized in that: also comprise oxygen delignification operation, in described oxygen delignification operation, alkali charge is to oven dry stock 2 ~ 3%, temperature 85 ~ 95 DEG C, oxygen pressure 0.3 ~ 0.5MPa, time 50 ~ 80min.
6. the preparation method of a kind of palm viscose according to claim 1, is characterized in that: further comprising the steps of:
Before select operation, select in operation before described, slurry desanding concentration 0.5 ~ 1.5%, desanding pressure is 0.25 ~ 0.35MPa;
Enrichment process, in described enrichment process, thickener outlet slurry dense 3 ~ 5%;
Bleaching process, in described bleaching process, viscosity: 9.1 ~ 10.8mPa.s after drift;
Decker concentrates and squeezing process, is concentrated to direct squeezing after slurry dense 3 ~ 5% is condensed into palm pulp through decker; Pulp after described squeezing moisture 50 ~ 55%; Described pulp technical performance index: fine mass content>=88.0% of first, viscosity 9.0 ~ 11.8mPa.s, ash content mass content≤0.14%, iron divides≤30mg/kg, whiteness>=76%, little dust≤180mm
2/ kg, large dust≤1.0/kg;
Squeezing subsequent pulverization step, the fine first fibre of the rear alkali of described pulverizing 22 ~ 28%, alkali fibre contains alkali 15 ~ 18%, the fine first fibre 28 ~ 31% of secondary alkali, and secondary alkali fibre is containing alkali 13 ~ 15%;
Experienced operation, fine half fine content≤3% of described experienced import alkali, cuprammonium viscosity 5.1 ~ 6.0mPa.s, fine half fine content≤8% of outlet alkali;
Yellow operation, in described yellow operation, CS
2be 31 ~ 34% to the fine addition of first, yellow time 30 ~ 60min;
Dissolving, mixing, filtration, bubble removal step, through the spinning glue that above-mentioned operation is obtained, quality is first fibre 7.0 ~ 9.2%, containing alkali 4.0 ~ 4.98%, viscosity 30 ~ 48s, degree of ripeness 10.2 ~ 18mL;
Spinning process, in described spinning process, coagulating bath adopts sulfuric acid 100 ~ 150g/L, sodium sulphate 300 ~ 350g/L, zinc sulfate 10 ~ 20g/L, temperature 35 ~ 55 DEG C.
7. the palm viscose that obtains of the preparation method of a kind of palm viscose according to claim 1, it is characterized in that: its technical indicator is as follows: dry fracture strength > 2.20cN/dtex, wet breaking strength > 1.25cN/dtex, dry elongation at break > 18.0%.
8. the palm viscose that obtains of the preparation method of a kind of palm viscose according to claim 1, it is characterized in that: its technical indicator is as follows: line density deviation ratio ± 1.5%, length variation rate ± 2.4%, overcut fibre≤0.4%, over-length fibre≤2.7mg/100g, residual sulfur content≤7.4mg/100g, fault≤2.5mg/100g, the dry strong coefficient of variation≤10.2%.
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| CN106498527A (en) * | 2016-09-23 | 2017-03-15 | 恒天海龙（潍坊）新材料有限责任公司 | A kind of process for producing high-wet-modulus fibre cellulose fiber |
| CN107254718A (en) * | 2017-05-05 | 2017-10-17 | 东至县鸿棉工贸有限责任公司 | A kind of short flannel pulping process |
| CN110478134B (en) * | 2019-08-29 | 2022-09-23 | 嘉兴学院 | Palm fiber absorbing material and preparation method thereof |
| CN115821408A (en) * | 2022-12-06 | 2023-03-21 | 金光纤维(江苏)有限公司 | Viscose staple fiber production method capable of reducing carbon disulfide consumption |
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