CN1390990A - Degradable flat fibre bundle and its preparing process - Google Patents
Degradable flat fibre bundle and its preparing process Download PDFInfo
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- CN1390990A CN1390990A CN 02113166 CN02113166A CN1390990A CN 1390990 A CN1390990 A CN 1390990A CN 02113166 CN02113166 CN 02113166 CN 02113166 A CN02113166 A CN 02113166A CN 1390990 A CN1390990 A CN 1390990A
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Abstract
A flat fibre bundle is prepared from cotton pulp, wood pulp, or their mixture through alkalizing, sulfonating to obtain cellulose sulfonate as spinning dope, spinning by nozzle, bundling, plasticizing, drawing, washing in water, and desulfurizing. The coagulating bath for spinning contains sulfuric acid and zinc sulfate. Its advantages are large surface area and high looseness.
Description
One, technical field
The present invention relates to a kind of preparation of biodegradable fiber, especially cellulose degradable flat fibre bundle and preparation method thereof.
Two, background technology
Chemical fibre (comprising other fiber) product market competition is more and more fierce, but chemical fibre industry subject matter is at present, unreasonable products structure, and differential degree is not high, causes the competition among enterprises level low, will face competition in the international market after the adding World Trade Organization.Stress the huge challenge of technology content, product specification, especially the production and operation green fiber focus of enterprise production and management especially of easily degrading.Composition as 93,112,922 1 kinds of cellulose ester of Chinese patent application.This cellulose esters contains the cellulose ester of the low replacement of 10wt% at least, its average substitution degree＜2.15, and resolution ratio (by ASTM125209-91 effusion CO#-[2] amount record as indicator) is at least 60wt% all around.Be suitable for making the various article that comprise cigarette filter and so on fabric.And for example among the WO9625538, multi-component system comprises: a starch-resin, comprise vinylacetate and copolymer without any the unsaturated monomer of functional group, but that this system prepares fabric is still not ideal enough.All good inadequately as surface area, bulking intensity etc., conventional fibre bundle elasticity, wet simultaneously elastic force is poor, and dyeability is good inadequately, and filament strength is poor.
Three, summary of the invention
The present invention seeks to: a kind of degradable fibre bundle is provided, especially degradable flat fibre bundle and preparation method thereof, this product cross section presents special-shaped flat form, surface area is big, the bulking intensity height, the especially wet elastic performance of good springiness is good, easily degraded, good environmental protection, the textile raw material that dyeability is good.Be applicable to that high-grade handicraft and extraordinary dress ornament select raw material for use, especially the senior raw material on the green level ground of manufacture of intraocular.
Technical solution of the present invention is: degradable flat fibre bundle system adopts cotton pulp or wood pulp or its mixture to make cellulose xanthate by alkalization, yellow, form stoste spinning glue, then through following technology: stoste spinning glue, spinnerets spinning, a boundling, the plasticizing of plasticizing groove, two boundling drawing-offs, rinsing bowl, hauling machine, a washing, a desulfurization, two desulfurization, two washings, finished product dress bag.
Regeneration cellulose under above-mentioned specific spinning process condition.Because this product spins refining by native cellulose and forms, the element formation mainly comprises carbon, hydrogen, oxygen, can be degraded to carbon dioxide and water fully at occurring in nature, environment is not polluted, with respect to fiber products such as the acrylic fibers that are difficult to decompose, terylene, degradable flat fibre bundle has been realized the demand of environmental protection, has adapted to social material civilization's level and has improved the development trend of coordinating mutually with balance of nature, will become the mainstream development direction of following chemical fibre industry.
Further improvement of the present invention is: the flat hole shape spinning of spinnerets, this product cross section presents special-shaped flat form, surface area is big, the bulking intensity height, remedied the logy shortcoming of conventional fibre bundle, improved simultaneously the performance of wet elastic force difference greatly, just novel degradable flat fibre bundle becomes the environmental-protecting performance height, dyeability is good, bright in colour, filament strength big, the good raw material of good springiness.Be applicable to that high-grade handicraft and extraordinary dress ornament select raw material for use, especially the senior raw material on the green level ground of manufacture of intraocular.
Product basic mechanical design feature index such as following table
The degradable flat fibre bundle performance indications
The flat fibre bundle of index request sequence number project 1 line density deviation ratio (%) ± 10.00 2 does that fracture strength (CN/dtex) 〉=1.25 3 dried elongation at break (%) 〉=8.00 4 wet breaking strengths (CN/dtex) 〉=0.55 5 residual sulfur contents (mg/100g)≤50.0 6 faults (mg/100g)≤4.0 7 whiteness deviations (%) Mo ± 28 moisture content (%)≤60.0,9 greasy dirt yellowish fibers (mg/100g), 0 10 lousiness are good without 11 brightness
Annotate: 1) Mo is determined by user producer.The official regain of fibre bundle is 13.0%
Four, description of drawings
Fig. 1 is the production technology flow chart
Five, the specific embodiment
Degradable flat fibre bundle system adopts cotton pulp or wood pulp or its mixture to make cellulose xanthate by alkalization, yellow, form stoste spinning glue, then through following technology: stoste spinning glue, spinnerets spinning, a boundling, the plasticizing of plasticizing groove, two boundling drawing-offs, rinsing bowl, hauling machine, a washing, a desulfurization, two desulfurization, two washings, finished product dress bag.
Main technologic parameters is as follows:
1, pulp: can adopt single cotton pulp or wood pulp is raw material, can also following proportioning: cotton pulp: wood pulp=7-3: 3-7, process conditions indifference in this scope.The technology that cellulose xanthate is made in alkalization, yellow is as follows: this is common process: it is 228-230g/l that single-steeping, dipping alkali concn are adopted in alkalization, temperature is 58-62 ℃, yellow technology is as follows, the yellow temperature is an initial temperature: 20 ± 1 ℃, temperature is 21 ± 1 ℃ eventually, and the carbon disulfide addition is 33-34% (a first fibre relatively).
2, spinning glue: first fibre: 8.95 ± 0.15%
Contain alkali: 5.35 ± 0.15% NaOH
Viscosity: 30-37 second (falling ball method)
Degree of ripeness: 10.5 ± 1ml (10%NH4CL value)
Carbon disulfide addition: 31-35%, for example 33% (the fine wood pulp ratio of first is increased, and carbon disulfide is suitably added)
3, spinning:
Spinning head specification: 480 holes * 0.08 * 2.4 * 74
The shape of spinneret orifice is that the bight is the rectangular opening of circular arc, can also be elliptical aperture.
Measuring pump: 30ml/r spins speed: 60m/min
4, coagulating bath:
Sulfuric acid: 108-137g/L, especially 115-137g/L, 125-127g/L is better
Zinc sulfate: 9-13g/L is 10-13g/L especially, and 11 ± 0.5g/L is better
Sodium sulphate: 310-340g/ is 325 ± 5g/L especially
Temperature: 50 ± 2 ℃, 50 ± 1 ℃ better
5, plasticizing-bath:
Temperature: 98 ± 2 ℃ of sulfuric acid: 20-25g/L
6, washing:
Water quality: demineralized water temperature: normal temperature
7, desulfurization is bathed: composition (sodium sulfite)
Temperature: 85 ± 2 ℃ of concentration: 14 ± 1g/L
With the production fiber number is that the degradable flat fibre bundle of 93.6dtex is an example, because of the particularity of product, has mainly done following technology adjustment in actual production:
1, spinning coagulation bath is formed
The concentration of sulfuric acid is directly connected to the quality of spinning spinnability and the physical and mechanical properties of finished fiber in the coagulation bath composition, because 93.6dtex fibre single thread fiber number is thick partially, it is long to finish the reaction required time, conventional fibre produce the rich experiences basis on through long-felt, test, coagulating bath concentration is controlled at 125-127g/L.
The content of zinc sulfate also affects the physical and mechanical properties of finished fiber in the coagulating bath, and for improving the intensity of finished fiber, the sulfuric acid zinc concentration is decided to be 11 ± 0.5g/L in the coagulating bath.
Sodium sulfate concentration is controlled at 325 ± 5g/L in the coagulating bath, plays a part to improve finished fiber intensity equally.
2, drawing-off distributes
HR401 type spinning machine is adopted in spinning, and drawing-off divides and finishes for three times this machine to tow, i.e. spinning head → draw-off godet drawing-off, a draw-off godet → collection drawing-off, collection one → collect two drawing-offs.Little because of producing the degradable flat fibre bundle total draft, the reasonability that drawing-off distributes will play decisive influence to the intensity and the degree of stretching of finished fiber, this also is one of main difficulty of producing this product, grope through overtesting, we are defined as the drawing-off distribution at last: draw-off godet+collection one drawing-off is adjusted into 20-30%, and collection one → collection two drawing-offs are adjusted into 5-10%.
3, plasticizing-bath concentration is adjusted;
Because the 93.6dtex degradable flat fibre bundle is thick partially, adds that spinning speed reaches 60m/Min, moulding remains not enough in the spinning bath so only depend on, and this also is one of difficulty of producing this product maximum.From collecting a tow, the still last viscose glue that solidifies is arranged in the tow, need in plasticizing-bath, further finish cellulose regenerated reaction, so plasticizing-bath concentration is brought up to 20-25g/L.
4, treatment process
Because the degradable flat fibre bundle tow is thick, difficulty is cleaned in post processing, reaches standard for guaranteeing the finished product residual sulfur content, temperature and concentration that desulfurization is bathed have suitably been improved, temperature is controlled at 85 ± 2 ℃, and desulfurization is bathed and is adopted sodium sulfite, and its concentration is controlled at about 14g/L.
The quality index of finished product
Can produce 10-120D fiber number fibre bundle product according to user's needs, conventional 85D degradable flat fibre bundle is as follows through the quality inspection index:
Fiber number: 93.6dtex
Do fracture strength; 1.35CN/dtex
Dried elongation at break: 12%
Wet breaking strength: 0.62CN/dtex
Residual sulfur content: 46.8mg/100g
Whiteness: 74.5%
Outward appearance, gloss: good
Conclusion:
In research and development degradable flat fibre bundle product of the present invention and technical process:
1, solves degradable flat fibre bundle and produced a series of technical barriers in the moulding process, spinning, spinnerets have been designed voluntarily, adopt the processing of electrolysis laser fine techniques, on spinning plate, process the flat hole that is fine to micron, make the fibre section present special flat form, technical difficulty is big;
2, this fiber surface area is big, and bulking intensity height, cellulose are under the high-temperature acidic state, and the plasticization drawing by about 10% has improved intensity greatly;
3, this product is a native cellulose fibre, can be degraded to carbon dioxide and water fully at occurring in nature, be a kind ofly have that environmental-protecting performance is strong, dyeability is good, filament strength is big, elasticity and the high good raw material of bulking intensity;
4, this product is high-tech, high added value, broad-spectrum multifunctional special-shaped fiber, is widely used in artificial green level ground, high-grade handicraft etc., also as the raw material of selecting for use of high-grade dress ornament, belongs to Green Product, and the market demand is big, growth is fast.
Claims (8)
1, degradable flat fibre bundle and preparation method thereof, it is characterized in that being to adopt cotton pulp or wood pulp or its mixture to make cellulose xanthate by alkalization, yellow, form stoste spinning glue, then through following technology: wash behind stoste spinning glue, spinnerets spinning, a boundling, the plasticizing of plasticizing groove, two boundling drawing-offs, rinsing bowl, the hauling machine, desulfurization and finished product dress wrap, the spinning coagulation bath prescription is as follows: sulfuric acid: 108-137g/L, zinc sulfate: 9-13g/L.。
2, by described degradable flat fibre bundle of claim 1 and preparation method thereof, the ratio that it is characterized in that cotton pulp and wood pulp mixture was from 3: 7 to 7: 3.
3, by described degradable flat fibre bundle of claim 1 and preparation method thereof, the shape that it is characterized in that spinning head is oval, can also be that the bight is the rectangular opening of circular arc.
4, by described degradable flat fibre bundle of claim 1 and preparation method thereof, it is characterized in that the spinning coagulation bath prescription is as follows: sulfuric acid: 115-137g/L, 125-127g/L is better, zinc sulfate: 10-13g/L is 11 ± 0.5g/L especially, sodium sulphate: 310-340g/ is 325 ± 5g/L especially, in temperature: solidify under 50 ± 2 ℃ the condition.
5, by described degradable flat fibre bundle of claim 1 and preparation method thereof, it is characterized in that the drawing-off distribution method: drawing-off divides and finishes for three times to tow, it is spinning head → draw-off godet drawing-off, draw-off godet → collection one drawing-off, collection one drawing-off → collection two drawing-offs: draw-off godet → collection one drawing-off is adjusted into 20-30%, collects a drawing-off → collection two drawing-offs and is adjusted into 5-10%.
6, by described degradable flat fibre bundle of claim 1 and preparation method thereof, it is characterized in that from collecting a tow, still the last viscose glue that solidifies is arranged in the tow, need in plasticizing-bath, further finish cellulose regenerated reaction, so the plasticizing-bath concentration of sodium sulfite is brought up to 20-25g/L.
7, by described degradable flat fibre bundle of claim 1 and preparation method thereof, it is characterized in that the temperature and the concentration of the desulfurization bath sodium sulfite of aftertreatment technology, temperature is controlled at 85 ± 2 ℃, concentration is controlled at 14g/L.
8, degradable flat fibre bundle is characterized in that being to adopt cotton pulp or wood pulp or its mixture to make cellulose xanthate by alkalization, yellow, forms stoste spinning glue, and the fibre section shape is oval after the spinning, can also be that the bight is the rectangular opening of circular arc.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 02113166 CN1219114C (en) | 2002-06-14 | 2002-06-14 | Degradable flat fibre bundle and its preparing process |
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| CN 02113166 CN1219114C (en) | 2002-06-14 | 2002-06-14 | Degradable flat fibre bundle and its preparing process |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101135067B (en) * | 2006-08-28 | 2010-09-15 | 宜宾丝丽雅股份有限公司 | Ultra-coarse denier flat shredded and method for making same |
| CN101922059A (en) * | 2010-08-17 | 2010-12-22 | 东华大学 | Production process of colored flat acrylic fiber and production line thereof |
| CN103215680A (en) * | 2013-04-08 | 2013-07-24 | 宜宾海丝特纤维有限责任公司 | Production technology of viscose extinction monofilament |
| CN103215679A (en) * | 2013-04-08 | 2013-07-24 | 宜宾海丝特纤维有限责任公司 | Production technology of viscose flat monofilament |
| CN103526320A (en) * | 2013-10-28 | 2014-01-22 | 唐山三友集团兴达化纤有限公司 | Method for producing flat viscose fibers and spinneret used during production |
| CN103774262A (en) * | 2014-01-24 | 2014-05-07 | 阜宁澳洋科技有限责任公司 | Superfine ultrashort viscose staple fiber for environment-friendly filtering material and preparation method thereof |
| CN103958749A (en) * | 2011-11-29 | 2014-07-30 | 凯尔海姆纤维制品有限责任公司 | Regenerated cellulose fiber |
| CN106521672A (en) * | 2016-08-29 | 2017-03-22 | 山东银鹰化纤有限公司 | Preparation method of ultra-short flat fiber |
-
2002
- 2002-06-14 CN CN 02113166 patent/CN1219114C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101135067B (en) * | 2006-08-28 | 2010-09-15 | 宜宾丝丽雅股份有限公司 | Ultra-coarse denier flat shredded and method for making same |
| CN101922059A (en) * | 2010-08-17 | 2010-12-22 | 东华大学 | Production process of colored flat acrylic fiber and production line thereof |
| CN101922059B (en) * | 2010-08-17 | 2012-07-04 | 东华大学 | Production process of colored flat acrylic fiber and production line thereof |
| CN103958749A (en) * | 2011-11-29 | 2014-07-30 | 凯尔海姆纤维制品有限责任公司 | Regenerated cellulose fiber |
| CN103958749B (en) * | 2011-11-29 | 2016-10-05 | 凯尔海姆纤维制品有限责任公司 | Regenerated celulose fibre |
| CN103215680A (en) * | 2013-04-08 | 2013-07-24 | 宜宾海丝特纤维有限责任公司 | Production technology of viscose extinction monofilament |
| CN103215679A (en) * | 2013-04-08 | 2013-07-24 | 宜宾海丝特纤维有限责任公司 | Production technology of viscose flat monofilament |
| CN103526320A (en) * | 2013-10-28 | 2014-01-22 | 唐山三友集团兴达化纤有限公司 | Method for producing flat viscose fibers and spinneret used during production |
| CN103526320B (en) * | 2013-10-28 | 2016-01-20 | 唐山三友集团兴达化纤有限公司 | The spinning head used in the production method of flat viscose fiber and production process |
| CN103774262A (en) * | 2014-01-24 | 2014-05-07 | 阜宁澳洋科技有限责任公司 | Superfine ultrashort viscose staple fiber for environment-friendly filtering material and preparation method thereof |
| CN106521672A (en) * | 2016-08-29 | 2017-03-22 | 山东银鹰化纤有限公司 | Preparation method of ultra-short flat fiber |
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| CN1219114C (en) | 2005-09-14 |
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