CN101372766A - Technological process for producing viscose fiber filament by secondary impregnation production - Google Patents
Technological process for producing viscose fiber filament by secondary impregnation production Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title abstract description 20
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- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 10
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- 229960001763 zinc sulfate Drugs 0.000 claims description 5
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract 3
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- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 3
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Abstract
The invention discloses a technique method for producing viscose fiber filaments by adopting secondary dipping. In the method, the secondary dipping technology is adopted based on the technique of primary dipping for producing viscose fiber filaments; besides, the concentration difference of free bases in secondary alkali liquid and soda cellulose are utilized to separate out partial free bases; simultaneously the semi-fiber content of the soda cellulose is reduced; under the situation of not affecting the amount of the combined soda, the secondary reactions during an etiolation process are reduced; the adding amount of carbon bisulfide is reduced; the viscose quality is ensured; and the dipping effect is improved by adding a novel addition agent in the secondary dipping process; proper aging, etiolation, ripening and spinning techniques are selected to produce the viscose filaments with high quality; besides, the production cost is reduced; the production efficiency is improved and the environment pollution is reduced.
Description
Technical field
The present invention relates to a kind of process of producing viscose fiber filament, is the process that viscose fiber filament is produced in a kind of employing " secondary dipping process " specifically.
Background technology
The alkali cellulose preparation is first procedure that viscose is produced, the alkali cellulose quality quality that it is produced, be directly connected to the quality of viscose glue preparation, and then the quality, especially the viscose filament yarn production that influence smart glue fiber final products there is higher requirement to the alkali cellulose quality of production.When China's development fifties viscose, pentahapto mechanism viscose glue is adopted in the short fiber growth, the preparation of alkali cellulose and viscose glue is closed in one, batch viscose machine is not adopted in long filament production, increase temperature experienced technology and continue to use the box proofing of traditional batch (-type), promptly make and make it yellow again after the alkali cellulose and make viscose glue.The sixties, alkali fiber preparation technology was progressive to some extent along with development in science and technology, the one-time continuous process for dipping occurred, than the box very much progress that is impregnated with, realized the production serialization, improved the production capacity of single device, reduce labour intensity, also improved the alkali cellulose quality of stability simultaneously.Whole viscose fibre industry production field appears having swept across in this new technology, and box impregnation technology has been substituted, and the batch viscose machine of short winding production usefulness also has been substituted.To the end of the seventies in the world the achievement of viscose production scientific research the double-steeping new technology of system alkali cellulose has appearred, and at first in short fiber production, be applied.This new technology has shown its superiority on using, not only improved the alkali cellulose quality, and short fiber production unit consumption simultaneously also reduces significantly.
Viscose filament yarn association has proposed and will use this new technology on viscose filament yarn is produced, and called each factory to strengthen this application study when annual meeting was had a meeting in Jiujiang in 1992.Application in viscose filament yarn production has obtained some achievements and understanding to the double-steeping new technology.
Dipping is a cellulose at alkali lye is that the effect of NaOH solution issues the process that biochemical reaction and physical action generate alkali cellulose.Theoretically, the alkali of cellulose and any concentration can both generate alkali cellulose in the pulp.Tradition steeping liquor concentration is 230～250g/L, and what dipping process took place is two kinds of effects: the one, and chemical change, cellulose and alkali generate the process of alkali cellulose.This part alkali is called in conjunction with alkali, is the basis of yellow effect in conjunction with the assurance of alkali number.The 2nd, the physics change, a part of alkali lye infiltrates pulp and has neither part nor lot in chemical reaction, but is adsorbed on around the big molecule of alkali cellulose, is referred to as free alkali.Assurance is in conjunction with alkali number the time, the amount of free alkali also increases thereupon, and a large amount of free alkalis enters the yellow operation, and the side reaction occurrence probability increases greatly, thereby influence the yellow effect, reduced production efficiency, caused in the viscose glue first fine higher with alkali content (weight) ratio simultaneously, the chemical industry material consumes high, cost increases, and contain the alkali height in the discharging waste liquid, sulfide increases, and causes environmental pollution.If adopt the immersion liquid of low concentration at the very start, though can reduce the content of free alkali, the hydrolysis that generates alkali cellulose is violent, and is feasible on the low side in conjunction with alkali number, can't satisfy the yellow requirement.
Summary of the invention
Technical problem to be solved by this invention is: a kind of process that adopts double-steeping to produce viscose fiber filament is provided, this method uses " double-steeping " method to produce viscose fiber filament, reduce production cost, improved production efficiency, reduced environmental pollution.
The present invention is on the basis of the technology of traditional single-steeping production viscose fiber filament, adopt the double-steeping technology, add auxiliary agent in the double-steeping process, improve dipping effect, improve the alkali cellulose quality, select suitable experienced, yellow, maturation, spinning technique simultaneously for use, produce the high-quality viscose filament yarn, solved people and wanted the technical problem that solves for a long time always.
Technical scheme of the present invention is: the process of producing viscose fiber filament with double-steeping, raw material adopts cellulose pulp, as adopting the special-purpose pulp cotton pulp of the long filament dregs of rice, wood pulps or pulp, its degree of polymerization is 550～600, and dynamic viscosity is 12.5 ± 1.0mPa.s, alpha cellulose content 〉=95%, ash≤0.08%, iron content≤18mg/kg, whiteness 〉=80%, moisture content 10 ± 1.5%.
Comprise following key step,
Single-steeping, single pressing, precomminution, double-steeping, twice pressing, precomminution, fine powder are broken, experienced, yellow, dissolving, mixing, filtration, maturation, deaeration and spinning, and concise, oven dry with become aftertreatment technology step such as tube.
Described single-steeping step, the concentration of steeping liquor are 230～250g/L, and dipping temperature is 50～55 ℃;
Described double-steeping step, the concentration of steeping liquor are 160～180g/L, and dipping temperature is 50～55 ℃; In described steeping liquor, add auxiliary agent, its consumption be in the pulp raw material the fine content of first 0.01～0.1%; Described auxiliary agent will be to adopt V32 or Afilan ZS; And the concentration of steeping liquor preferably adopts 170～180g/L in the double-steeping step;
Described experienced step, the material that the rapid back of fine powder quick short steps is obtained experienced 7～9 hours, cools off at 20～24 ℃ under 38～48 ℃ temperature then earlier; Employing is experienced in experienced drum or ageing chamber;
Described yellow step, CS
2Addition be in the alkali cellulose after experienced the fine content of first 28～32%;
Described maturation step, the maturation time is 35～40 hours;
Described spinning step, the coagulation bath composition that solidifies in coagulating basin are sulfuric acid 110～140g/L, zinc sulfate 10～15g/L, sodium sulphate 260～300g/L; Coagulation bath temperature is 49～53 ℃; Transparency 〉=1000mm, drawing-off distributes: shower nozzle drawing-off-8～12%, drawing-off 15～25% between dish.
Owing to adopt double-steeping technology, in the double-steeping step, add V32 or Afilan ZS, improved the dipping effect of pulp raw material, in experienced step, adopt experiencedly in experienced drum or ageing chamber, the discreteness of cellulosic degree of polymerization is reduced, uniformity improves, by experienced, the alkali cellulose degree of polymerization distribution narrows down, thereby improves the viscose glue inherent quality.
Double-steeping technology is on the basis of adopting conventional single-steeping, alkali cellulose after the alkali lye of working concentration 160～180g/L squeezes dipping floods again, utilize the concentration difference of free alkali in secondary alkali lye and the alkali cellulose, separate out the part free alkali, reduced half fine content of alkali cellulose simultaneously.Under situation about not influencing in conjunction with alkali number, reduced the generation of side reaction in the yellow process, reduce the addition of carbon disulfide, guarantee viscose quality.
Owing to adopt double-steeping, half fine content is low in the alkali cellulose, CS
2Addition be 28～32% (with respect to the fine content of first in the alkali cellulose), and when adopting traditional single-steeping explained hereafter viscose filament yarn, CS
2Addition at least 35% (with respect to the fine content of first in the alkali cellulose), therefore, this technology has not only reduced production cost, has also reduced environmental pollution, realizes low toxicity spinning, favourable operator's is healthy.And the maturation time shortened about 12 hours, improved productivity ratio greatly.
The specific embodiment
Embodiment 1: adopt double-steeping to produce the process of viscose fiber filament, the raw material of use is the special-purpose pulp of long filament; Its degree of polymerization is 550～600, and dynamic viscosity is 12.5 ± 1.0mPa.s, alpha cellulose content 〉=95%, ash≤0.08%, iron content≤18mg/kg, whiteness 〉=80%, moisture content 10 ± 1.5%.
The processing step that adopts is as follows:
A, single-steeping, single pressing and pulverizing
Pulp dropped in the single-steeping bucket flood, the concentration of alkali lye is 240g/L in the treating tank, and dipping temperature is 51.5 ℃, through single-steeping, and half fine content 19.0g/L, the content of first fibre is 27.5% in the alkali cellulose, the alkali fibre contains alkali 17.8%.Then macerate is taken out and carry out single pressing and precomminution, make thick material;
B, double-steeping, twice pressing and fine powder are broken
To carry out double-steeping in the thick material input double-steeping bucket, concentration of lye is 172g/L in the treating tank, dipping temperature is 51.0 ℃, and add auxiliary agent in maceration extract, described auxiliary agent is the V32 that is produced by Dutch Akzo Nobel N.V., its consumption be in the pulp raw material the fine content of first 0.05%, through double-steeping, half fine content 8.0g/L, the content of first fibre is 30.2% in the alkali fibre, the alkali fibre contains alkali 14.5%; Then macerate is taken out once more, it is broken to carry out twice pressing, precomminution and fine powder, makes thin material;
C, experienced, yellow and dissolving
Thin material is put into experienced drum, under 41 ℃ temperature, experienced 8 hours, 21 ℃ of coolings of carrying out 12 hours, obtain alkali cellulose then.Then the alkali cellulose after experienced is dropped in the xanthating machine, add the CS of 30.0% (to the fine content of first in the alkali cellulose)
2, carry out yellow, generate cellulose xanthate; Subsequently the cellulose xanthate that obtains is dissolved in dissolving machine, make viscose glue;
Owing to adopt double-steeping technology, improved the dipping effect of pulp raw material, in the double-steeping step, add V32, improve the alkali cellulose uniformity, thereby improved the viscose glue inherent quality.
Because be to adopt double-steeping technology, the content of half fibre is low in the alkali cellulose, CS
2Addition only need about 30% (with respect to the fine content of first in the alkali cellulose), and when adopting traditional single-steeping explained hereafter viscose filament yarn, CS
2Addition at least 35% (with respect to the fine content of first in the alkali cellulose), therefore, this technology has not only reduced production cost, has also reduced the pollution to environment.
D, mixing, filtration, maturation and deaeration
Mixing, filtration, maturation and deaeration processing step, the production technology of itself and known viscose filament yarn is basic identical, and difference is, owing to adopt the double-steeping method, reduces CS in the yellow process
2Addition, can shorten the maturation time greatly, be 38 hours when the maturation time, the index of spinning glue is reached, first fibre 8.2% contains alkali 5.8%, viscosity 35 seconds, degree of ripeness 9.2mL shortened greatly than 50 hours the maturation time of adopting the long filament pulp, had improved productivity ratio.
E, spinning
Spinning viscose glue after the maturation is pressed into spinning machine shower nozzle aperture and after flowing out, enter in the coagulating bath by sulfuric acid and sulfate combination, at this moment, sulfuric acid impels cellulose xanthate to decompose, again become cellulose again, in coagulating basin, form regenerated cellulose filaments one by one.The composition of coagulating bath composition: sulfuric acid 120g/L, zinc sulfate 11.2g/L, sodium sulphate 285g/L, transparency 〉=1000mm, 50.2 ℃ of coagulation bath temperatures.Drawing-off distributes: shower nozzle drawing-off-8%, drawing-off 15% between dish.
F, concise, oven dry, become tube
Above-mentioned long filament crude product through post processings such as concise, oven dry, one-tenth tubes, is made the viscose filament yarn finished product that can use and sell.
The viscose filament yarn fiber index that is made by above-mentioned technology is:
Do fracture strength: 2.24cN/dtex
Wet breaking strength: 1.02cN/dtex
Dried elongation at break: 19.2%
The dried extension at break coefficient of variation (CV value): 6.20%
Line density (fiber number) deviation :-4.0%
The line density coefficient of variation (CV value): 3.0%
The twist coefficient of variation (CV value): 9.8%
Monofilament radical deviation: 0%
Residual sulfur content: 7.20mg/100g
Dye uniformity: 3.5 grades
Embodiment 2: substantially the same manner as Example 1, its difference is,
In the single-steeping step, the concentration of alkali lye is 230g/L in the treating tank, and dipping temperature is 54.5 ℃;
In the double-steeping step, the concentration of steeping liquor is 180g/L, and dipping temperature is 53.5 ℃, adds auxiliary agent A filan ZS in maceration extract, consumption be in the pulp raw material the fine content of first 0.08%;
In the experienced step, in the time of 45 ℃ experienced 7 hours, subsequently 22 ℃ of coolings 11.5 hours;
In the yellow step, CS
2Addition be equivalent to 28.5% of the fine content of first in the alkali cellulose;
In the maturation step, the maturation time is 36 hours; Spinning glue index, the first fibre: 8.1%, contain alkali: 5.6%, viscosity: 32s, degree of ripeness: 9.8ml.
In the spinning step, coagulating bath: sulfuric acid 125g/l, zinc sulfate 11.8g/L, sodium sulphate 295g/L, transparency 〉=1010mm, 50 ℃ of coagulation bath temperatures; Spinning technique: shower nozzle drawing-off 11%, drawing-off 23% between dish.
The viscose filament yarn fiber index that is made by above-mentioned technology is:
Do fracture strength: 2.35cN/dtex
Wet breaking strength: 1.10cN/dtex
Dried elongation at break: 18.6%
The dried extension at break coefficient of variation (CV value): 7.10%
Line density (fiber number) deviation :+3.0%
The line density coefficient of variation (CV value): 4.0%
The twist coefficient of variation (CV value): 7.8%
Monofilament radical deviation: 0%
Residual sulfur content: 8.20mg/100g
Dye uniformity: 3.5 grades
Embodiment 3: substantially the same manner as Example 1, its difference is,
In the double-steeping step, the concentration of steeping liquor is 160g/L, adds auxiliary agent V32 in maceration extract, consumption be in the pulp raw material the fine content of first 0.1%;
In the experienced step, in the time of 38 ℃ experienced 9 hours, subsequently 24 ℃ of coolings 10 hours;
In the yellow step, CS
2Addition be equivalent to 31.0% of the fine content of first in the alkali cellulose;
In the maturation step, the maturation time is 39 hours; Spinning glue index, the first fibre: 8.3%, contain alkali: 5.8%, viscosity: 38s, degree of ripeness: 10.1ml.
In the spinning step, coagulating bath: sulfuric acid 130g/l, sodium sulphate 300g/l, zinc sulfate 12g/L, 50.5 ℃ of temperature, transparency 1000mm; Spinning technique: shower nozzle drawing-off 4.2%, drawing-off 20% between dish.
The viscose filament yarn fiber index that is made by above-mentioned technology is:
Do fracture strength: 2.16cN/dtex
Wet breaking strength: 1.02cN/dtex
Dried elongation at break: 19.6%
The dried extension at break coefficient of variation (CV value): 8.1%
Line density (fiber number) deviation :+4.0%
The line density coefficient of variation (CV value): 4.2%
The twist coefficient of variation (CV value): 6.8%
Monofilament radical deviation: 0%
Residual sulfur content: 6.20mg/100g
Dye uniformity: 3.5 grades
The present invention is not limited to the foregoing description, experiment showed, the wood pulps or the bamboo pulp that above-mentioned processing step are implemented on the equivalent technology index, also can reach same technique effect.
Claims (3)
1. adopt double-steeping to produce the process of viscose fiber filament, the employing cellulose pulp is a raw material, may further comprise the steps: single-steeping, single pressing, precomminution, double-steeping, twice pressing, precomminution, fine powder are broken, experienced, yellow, dissolving, mixing, filtration, maturation, deaeration, spinning and post processing, it is characterized in that:
Described single-steeping step, steeping liquor concentration are 230～250g/L, and dipping temperature is 50～55 ℃;
Described double-steeping step, steeping liquor concentration are 160～180g/L, and dipping temperature is 50～55 ℃; And in described steeping liquor, add auxiliary agent, auxiliary dosage be in the pulp raw material the fine content of first 0.01～0.1%;
Described experienced step, the material that the rapid back of fine powder quick short steps is obtained experienced 7～9 hours, cools off at 20～24 ℃ under 38～48 ℃ temperature then earlier;
Described yellow step, CS
2Addition be in the alkali cellulose after experienced the fine content of first 28～32%;
Described maturation step, the maturation time is 35～40 hours;
Composition is sulfuric acid 110～140g/L, zinc sulfate 10～15g/L, sodium sulphate 260～300g/L in the described spinning step, coagulating bath; Coagulation bath temperature is 49～53 ℃; Transparency 〉=1000mm, drawing-off distributes: shower nozzle drawing-off-8～12%, drawing-off 15～25% between dish.
2. employing double-steeping as claimed in claim 1 is produced the process of viscose fiber filament, and it is characterized in that: described double-steeping step, steeping liquor concentration are 170～180g/L.
3. employing double-steeping as claimed in claim 1 is produced the process of viscose fiber filament, and it is characterized in that: described auxiliary agent is V32 or Afilan ZS.
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| CN112758957A (en) * | 2020-12-28 | 2021-05-07 | 宜宾丝丽雅股份有限公司 | Process for purifying sodium hydroxide concentration by electrodialysis |
| CN112853550A (en) * | 2020-12-28 | 2021-05-28 | 宜宾丝丽雅股份有限公司 | Treatment method for recycling alkali liquor |
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