CN101988216B - Method for circularly preparing solvents in Lyocell fiber preparation process - Google Patents
Method for circularly preparing solvents in Lyocell fiber preparation process Download PDFInfo
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- CN101988216B CN101988216B CN200910055892.4A CN200910055892A CN101988216B CN 101988216 B CN101988216 B CN 101988216B CN 200910055892 A CN200910055892 A CN 200910055892A CN 101988216 B CN101988216 B CN 101988216B
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- bath
- solvent
- boundling
- body lotion
- lyocell fiber
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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Abstract
The invention relates to the field of chemical fiber manufacturing, in particular to a new method for circularly recycling Lyocell fiber solvents. The method for circularly preparing solvents in a Lyocell fiber preparation process comprises the following steps: spraying bath fluid to the two sides of thread-lines by an atomizing nozzle in a vertical fog-type solidifying chamber; after the bath fluid drops in a bundling bath along the surfaces of the thread lines and the thread lines are bundled by the bundling bath, feeding the thread lines into a post-processing stage to complete the spinning process; feeding redundant bath fluid into an auxiliary bundling bath by the bundling bath; after the bath fluid in the auxiliary bundling bath is filtered, respectively feeding the bath fluid back to the atomizing nozzle, the bundling bath and a recovered fluid storage tank; and after the bath fluid in the recovered fluid storage tank is filtered and purified, taking the obtained bath fluid as the raw material for preparing spinning solution. In the invention, the bath fluid can directly be fed and used for solution preparation, which saves the investment on concentrating equipment and the consumption on steam and power, greatly reduces the investment and production cost of cellulose fiber production by using a solvent method, and creates a condition for vigorously promoting the green process of cellulose fiber production by using the solvent method.
Description
Technical field
The invention belongs to chemical fibre and manufacture field, relate in particular to a kind of method that Lyocell fiber solvent circulation is reclaimed.
Background technology
1905 taking the cellulose that extracts in string since raw material production chemical fibres industryization is come out first, be all using inorganic salt solution as solvent, have nitrate method, cuprammonium process, CS
2method.Wherein use CS
2method regenerated celulose fibre is referred to as viscose, since 1904 last century suitability for industrialized production, and existing 105 years history.Approximately 3,100,000 tons of global viscose total outputs in 2008, Chinese viscose output is 131.88 ten thousand tons.
But owing to using CS in manufacture process
2and cause environment waste gas, waste water serious environment pollution, human nerve, brain, internal organ, skin etc. are had to harm, therefore, the production of this fiber has just been subject to strict environmental protection policy restriction at the last century mid-term, impels countries in the world to be devoted to study, to develop novel solvent and carrys out regenerated fiber to reduce environmental pollution.
NMMO (N-methyl beautiful jade oxide) is a kind of organic solvent, biochemical toxicity is optimum, can not cause biomutation, the cellulose fibre process of producing as solvent taking NMMO (N-methyl beautiful jade oxide) is as physical process, and without any chemical reaction, solvent recycles pollution-free, be called as environmental protection fiber, therefore, one appears on the market, and is just subject to people and payes attention to.
Within 1980 the earliest, first obtain technique and product patent by German Akzo-Nobel company, 1989 by international artificial silk and the synthetic fiber Bureau of Standards (BISFA) definite designation: make raw material with regenerated cellulose, with NMMO(N-methyl code quinoline-N-oxide) make solvent, the fiber that spinning is made, called after Lyocell.The implication prefix Lyo-of Lyocell is that Greek represents the meaning of dissolving, and suffix-cell represents the cellulosic meaning, and the implication of whole Lyocell represents that this fiber can carry out biodegradable green fiber.
Lyocell fiber has numerous characteristics: intensity is as polyamide fibre, meticulous as silk, has again the washability of terylene, the gas permeability of cotton fiber.It also has fibrillation effect, can produce the not surface effect of getable similar peach face of conventional fibre.Lyocell fiber is strong and wet strong and famous with high level cadre.Under hygrometric state, the fracture strength of Lyocell damage only 6%, extends and does not almost change; Its heat-resisting quantity is good, and in 190 DEG C, 30s, the strength damage of staple fibre is that 7%o is better than Wet-spinning regenerated celulose fibre; Dry, wet strength is all fine, reach and close fine level, and seldom have contraction.Be called " green fiber that 21 century is the most promising " by insider or be referred to as " environmental friendliness fiber ".
Although China has also had some and novel solvent method to produce the relevant patent of regenerated celulose fibre technique in recent years.But current more than 99.9% factory still continues to use traditional viscose process and produces regenerated celulose fibre, wherein the cost recovery of solvent is high is main cause.
Last century end, in Lyocell technology, spinning adopts the dry method that squirts mostly in the world.Although heat transfer type changes, and spinning speed is increased, mass transfer method is still basic identical with traditional viscose process, and the body lotion concentration of coagulating bath and the control of temperature also adopt large bath raio endless form to maintain that it is stable.The concentration of coagulation bath NMMO of generally delivering to recycle section is lower, also must after evaporation and concentration, just can reach 50% and prepare workshop section for stoste after purification.
Due to NMMO very easily with water combination, under 100Pa pressure, boiling point is 115 DEG C.Therefore, utilize traditional multiple-effect evaporation to concentrate or film evaporation technology, steam consumption is all very high; The investment of film evaporation equipment and power consumption are also very high.
As shown in Figure 1, spinning solution in prior art (the NMMO solution of containing cellulose) by metering, filter, extruding spray silk becomes a stoste thread to enter coagulating tank to carry out coagulating bath, stoste thread is in coagulating bath, surface concentrated phase solvent and water are constantly diffused in coagulation bath, and stoste thread surface solidify to form as-spun fibre gradually.In order to ensure the uniformity of fiberizing quality, the design of technological process must ensure following 2 points:
1) body lotion that strand concentration around changed that upgrades in time, the concentrated phase solvent on stoste thread surface could continuously be diffused into surface adhesion and bathe in film, and fiber surface structure could be evenly closely.Therefore, body lotion must be mobile instead of static with constant flow rate.
2) concentration of coagulating bath and amount also increase along with stoste thread enters groove inter-sync continuously, in order to ensure the uniformity of fiberizing, the variation of bath temperature and concentration must be controlled in the scope of strand quality requirements that guarantee enters body lotion continuously, is generally error to be no more than ± 0.2% left and right solvent strength.Need to discharge by the coagulation bath of enrichment in time simultaneously, and suitably increase the concentration that dilution water correction changes, constant to ensure the relative concentration of coagulation bath.The coagulation bath of discharge section will deliver to solvent recovery workshop section purified treatment concentrated after, go stoste to prepare workshop section and prepare spinning solution.For energy-conservation, general producer is all arranged on partly-exposed basement by circulating slot; Owing to adopting large bath raio, the constant of its temperature can only lean on natural heat dissipation, increases storage tank liquid level natural evaporation area as far as possible.
The design of body lotion internal circulating load can be calculated and draw according to following formula:
W
Q＝——————
e
In formula: Q: the internal circulating load t/h of coagulating bath body lotion
w:spinning solution is brought solvent (moisture) the amount t/h of coagulating bath into
e:the drop wt% that coagulating bath change in concentration allows
Can draw from above formula analysis: the concentration drop value of coagulation bath
eless, the internal circulating load Q of coagulating bath is larger, and circulating slot, the circulating pump ability of mating are also larger, and equipment investment and operating cost (power consumption, steam consumption) all will increase.From fiberizing mechanism, coagulating bath concentration drop
eless, fiberizing quality is more relatively stable, and general control is at 1-2%.
Suppose that cellulose fibre hourly output is 1000 kilograms (producing 8000 tons per year), in spinning solution, the concentration of solvent is 88%, brings the solvent (moisture) of coagulating bath into
wbe 8.33 tons/time, coagulating bath initial concentration is 12%, coagulating bath concentration drop
efor ± 2%.
Calculate according to above-mentioned formula:
Selected body lotion circulating pump ability be at least 416.5 tons/time; In circulation per hour 5 times, the circulation fluid storage tank capacity configuring is at least 83.3 tons.The proportion of supposing body lotion is that this circulating pump ability is 400m so close to water
3/ h, circulation fluid storage tank dischargeable capacity is 80m
3.
Meanwhile, the coagulation bath that need be 14% by the concentration that has 8.33 tons per hour goes recycle section to purify the solvent (wherein 50% water) that rear simmer down to stoste is prepared 50% required concentration of workshop section.
As calculated: moisture=8.33 (1-14% ÷ 50%)=6 (ton/time) that need to evaporate
1 ton of cellulose fibre of every production, solvent concentration section energy consumption is amounted to 1.15 tons of standard coals.Only direct concentrated cost of solvent of coal is about 1000 yuans of/ton of fibers.Consider power consumption, artificial, depreciation of equipment etc., the concentrated production cost of solvent recovery of fiber per ton is up to 1200 yuan/ton of left and right.
So the Lyocell fiber that adopts " green solvent "-methyl morpholine oxide to prepare cellulose fibre is popularized all very difficult so far in the whole world, approximately 100,000 tons/year of Lyocell fiber whole world total outputs in 2008, account for regenerated celulose fibre total amount below 5%.
Summary of the invention
Technical problem to be solved by this invention is to provide solvent circulation preparation method in a kind of Lyocell fiber preparation process, the method adopts the vertical chamber of solidifying to spray cooling, make the body lotion of collecting not need concentrated can being directly used in to prepare spinning solution, greatly reduce the circulation cost recovery of NMMO solvent.
The present invention is achieved in that solvent circulation preparation method in a kind of Lyocell fiber preparation process, spinning solution metering, after filtration, enter filament spinning component spinnerets, enter vertical mist formula by filament spinning component spinnerets extruding ejection strand and solidify chamber, vertical mist formula is solidified indoor atomizer body lotion is sprayed onto to strand two sides, body lotion falls into boundling bath together along strand surface, strand is sent into post-processing stages and is finished spinning line after boundling is bathed boundling, boundling bath is sent unnecessary body lotion into boundling and is bathed in auxiliary groove, boundling is sent respectively atomizer back to after bathing the body lotion filtration in auxiliary groove, boundling bath and recovery liquid storage tank, the body lotion reclaiming in liquid storage tank purifies the rear raw material as preparing spinning solution more after filtration.
The body lotion solvent strength that the vertical mist formula that described boundling bath is collected is solidified whereabouts, chamber is 45～50%.
Described boundling is bathed auxiliary groove and sent into the body lotion that reclaims liquid storage tank through precipitation---to be filtered after the cleaning procedure of---anion exchange---cation exchange, directly delivers to spinning solution and prepare workshop section's use.
Described post-processing stages is sent into washing machine washing silk after being included in the drawing-off of drawing-off bath.
In described drawing-off bath, unnecessary body lotion is first sent into drawing-off and is bathed in auxiliary groove, then sends atomizer back to as body lotion.
Described boundling is bathed auxiliary groove and drawing-off and is bathed auxiliary groove and send the body lotion of atomizer back to and first will enter head tank and allocate online concentration and temperature.
The coagulation bath of the described solvent of preparing spinning solution and atomizer ejection is all the aqueous solution of organic solvent NMMO, and the NMMO solvent strength of preparing the raw material of spinning solution is 50%～80%, and in coagulation bath, NMMO solvent strength is 10%～18%.
A described water of washing of washing that silk produces is 2～10% NMMO solvent.
The body lotion of 45%～50%NMMO solvent strength that the coagulation bath employing of described 10%～18%NMMO solvent strength is bathed from boundling and the concentration of bathing from drawing-off are at a water of washing of 2～10%NMMO solvent strength, and both proportionally measure to be mixed with and form.
The present invention adopts vertical mist formula to solidify chamber and makes fiberizing, once manufacturing process determination in whole production process, in coagulation bath, the concentration of NMMO and temperature remain constant, flow regulator and body lotion cool-heat-exchanger+temperature control system in proportion online, fully ensure the quality of fiberizing, simultaneously by adjusting the solidifying process of strand, the concentration of boundling body lotion can be brought up to 50%, the body lotion of 50% concentration after purification just can directly be delivered to stoste preparation and use, cancel the solvent enrichment process in original production flow process, save the equipment investment such as circulating pump and jumbo circulating slot of the large bath raio of coagulating bath, the power consumption of construction investment and operation, investment to concentrator and steam, power consumption are saved, altogether approximately can save and account for the equipment investment of gross investment approximately 10～15% and 30% steam consumption, investment and the production cost of producing cellulose fibre through solvent are greatly reduced, 1 ton of procedure of fibre production cost of every production can decline nearly 1000 yuans, for the producing cellulose fibre through solvent of wideling popularize friendly process has been created condition.
Brief description of the drawings
Fig. 1 is classical body lotion circulation theory block diagram;
Fig. 2 is vertical mist formula coagulation bath circulation preparation principle block diagram.
In figure: 1 filament spinning component spinnerets, 2 vertical mist formulas are solidified chamber, 3 atomizers, 4 boundling baths, 5 boundlings and bathed auxiliary groove, 6 head tanks, 7 and reclaim liquid storage tanks, 8 drawing-off baths, 9 drawing-offs and bathe auxiliary groove.
Detailed description of the invention
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's statement, these equivalent form of values fall within the application's appended claims limited range equally.
As shown in Figure 2, solvent circulation preparation method in a kind of Lyocell fiber preparation process, weaving stoste enters filament spinning component spinnerets 1 after filtering, being sprayed into strand by filament spinning component spinnerets 1 enters vertical mist formula and solidifies chamber 2, vertical mist formula is solidified atomizer 3 on chamber 2 and is sprayed body lotion and carry out cooling to strand, then the body lotion of ejection enters boundling bath 4 together with strand, strand boundling carries out drawing-off after having bathed, cut off, wash silk bleach, oil, dry and pack, end spinning line; The unnecessary body lotion that boundling bath 4 is collected is sent into boundling and is bathed in auxiliary groove 5, boundling is divided into three parts after bathing the body lotion filtration in auxiliary groove 5, a part is sent atomizer 3 back to after allocating concentration and temperature by head tank 6 is online, a part is sent boundling bath 4 back to and is used as body lotion, another part is sent to and reclaims liquid storage tank 7, then after filtration, purification as the raw material of preparing spinning solution; The water of washing that washing machine washing silk produces is sent into 8 recycles of drawing-off bath; In described drawing-off bath 8, unnecessary body lotion is sent into drawing-off and is bathed in auxiliary groove 9, then sends atomizer 3 back to as body lotion by head tank 6 allotments.
In circulation preparation process of the present invention, in the spinning solution using, solvent NMM0 concentration is 80%～90%, in process of production, by regulating spray volume and the concentration of atomizer body lotion, in stoste, the cellulose of NMM0 and dissolving is separated, enter into the body lotion film that is bonded at stoste thread surface, the body lotion NMM0 maximum concentration that falls into boundling bath can reach 45%～50%; The boundling bath circulation of a part is delivered to atomizer and is contacted with stoste thread.In boundling bath, the NMM0 solution of concentration 50% left and right can be directly as the solvent of preparing spinning solution; The aqueous solution of washing that contains 2～10% NMM0 that a stage generation is washed in post processing is all used as the source of preparing fresh atomizer body lotion used, and a fresh water of washing all comes from the water that stoste is prepared reduced pressure concentration generation in workshop section's pulp course of dissolution.
In whole circulation preparatory phase, the coagulation bath of all NMM0 of containing, wash a water and all adopt closed cycle, zero-emission, therefore, solvent NMM0 theoretical recovery can reach 100%, does not need to configure evaporation concentration device.
Described boundling is bathed auxiliary groove and is sent into the body lotion that reclaims liquid storage tank through precipitation---after the cleaning procedure of filtration---anion exchange---cation exchange, directly deliver to spinning solution and prepare workshop section's use, do not need through evaporation and concentration operation, this solvent just can meet the requirement of former liquid preparing process.
The coagulation bath of the described solvent of preparing spinning solution and atomizer ejection is all the aqueous solution of organic solvent NMMO, and the NMMO solvent strength of preparing the raw material of spinning solution is 50%～80%, and in coagulation bath, NMMO solvent strength is 10%～18%.
A described water of washing of washing that silk produces is 2～10% NMMO solvent.
The body lotion of the 50%NMMO solvent strength that the coagulation bath employing of 10%～18%NMMO solvent strength is bathed from boundling and the concentration of bathing from drawing-off are greatly about a water of washing of 2～10%NMMO solvent strength, and both proportionally measure to be mixed with and form.
The solidification liquid that contains certain density organic solvent NMMO sticks to strand surface and forms liquid film after metering, atomization ejection, concentration while entering boundling bath approximately can be controlled in 50%, and its Main Means is to realize by initial concentration and the temperature of regulation and control atomizer spray volume, atomized liquid.
In the process of recycle NMMO solvent, regulate and control on the one hand the speed of heat and mass between body lotion and strand by this method by controlling the spray volume of fresh atomization coagulation bath and initial concentration; After adopting circulating pump again to send to atomization a part of boundling body lotion on the other hand, be again ejected into strand surface.In whole process, present gradient distribution along concentration and the Temperature Distribution of spinning journey atomized liquid, radially match with the gradient of the intermembranous heat and mass of body lotion with strand, therefore, strand internal structure is more even, and mechanical performance is more excellent.This point all cannot be accomplished at classical Wet-spinning or in the dry spray Wet-spinning of new release in recent years.
Claims (9)
1. solvent circulation preparation method in a Lyocell fiber preparation process, it is characterized in that: spinning solution metering, after filtration, enter filament spinning component spinnerets, enter vertical mist formula by filament spinning component spinnerets extruding ejection strand and solidify chamber, vertical mist formula is solidified indoor atomizer body lotion is sprayed onto to strand two sides, body lotion falls into boundling bath together along strand surface, strand is sent into post-processing stages and is finished spinning line after boundling is bathed boundling, boundling bath is sent unnecessary body lotion into boundling and is bathed in auxiliary groove, boundling is sent respectively atomizer back to after bathing the body lotion filtration in auxiliary groove, boundling bath and recovery liquid storage tank, the body lotion reclaiming in liquid storage tank purifies the rear raw material as preparing spinning solution more after filtration.
2. solvent circulation preparation method in Lyocell fiber preparation process as claimed in claim 1, is characterized in that: the body lotion solvent strength that the vertical mist formula that described boundling bath is collected is solidified whereabouts, chamber is 45～50%.
3. solvent circulation preparation method in Lyocell fiber preparation process as claimed in claim 1, it is characterized in that: described boundling is bathed auxiliary groove and sent into the body lotion that reclaims liquid storage tank through precipitation---to be filtered after the cleaning procedure of---anion exchange---cation exchange, directly deliver to spinning solution and prepare workshop section's use.
4. solvent circulation preparation method in the Lyocell fiber preparation process as described in any claim in claim 1～3, is characterized in that: described post-processing stages is sent into washing machine washing silk after being included in the drawing-off of drawing-off bath.
5. solvent circulation preparation method in Lyocell fiber preparation process as claimed in claim 4, is characterized in that: in described drawing-off bath, unnecessary body lotion is first sent into drawing-off and bathed in auxiliary groove, then sends atomizer back to as body lotion.
6. solvent circulation preparation method in Lyocell fiber preparation process as claimed in claim 5, is characterized in that: described boundling is bathed auxiliary groove and drawing-off and bathed auxiliary groove and send the body lotion of atomizer back to and first will enter head tank and allocate online concentration and temperature.
7. solvent circulation preparation method in Lyocell fiber preparation process as claimed in claim 6, it is characterized in that: the coagulation bath of the described solvent of preparing spinning solution and atomizer ejection is all the aqueous solution of organic solvent NMMO, the NMMO solvent strength of preparing the raw material of spinning solution is 50%～80%, and in coagulation bath, NMMO solvent strength is 10%～18%.
8. solvent circulation preparation method in Lyocell fiber preparation process as claimed in claim 7, is characterized in that: a described water of washing of washing that silk produces is 2～10% NMMO solvent.
9. solvent circulation preparation method in Lyocell fiber preparation process as claimed in claim 8, it is characterized in that: the body lotion of 45～50%NMMO solvent strength that the coagulation bath employing of described 10%～18%NMMO solvent strength is bathed from boundling and the concentration of bathing from drawing-off are at a water of washing of 2～10%NMMO solvent strength, and both proportionally measure to be mixed with and form.
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| CN200910055892.4A CN101988216B (en) | 2009-08-04 | 2009-08-04 | Method for circularly preparing solvents in Lyocell fiber preparation process |
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|---|---|---|---|
| CN200910055892.4A CN101988216B (en) | 2009-08-04 | 2009-08-04 | Method for circularly preparing solvents in Lyocell fiber preparation process |
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| CN101988216A CN101988216A (en) | 2011-03-23 |
| CN101988216B true CN101988216B (en) | 2014-08-06 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105597580B (en) * | 2014-10-27 | 2018-04-06 | 中国石油化工股份有限公司 | The device for formulating and compound method of solidification liquid and application |
| CN104831422A (en) * | 2015-04-27 | 2015-08-12 | 江苏龙马绿色纤维有限公司 | Method for recycling waste liquid of spinning stock solution |
| CN105568401A (en) * | 2015-12-12 | 2016-05-11 | 大连理工大学 | Ultrasonic atomization assisted electrospinning technique |
| CN106222771B (en) | 2016-07-22 | 2019-02-22 | 中国纺织科学研究院有限公司 | A kind of preparation method of cellulose fibre |
| CN106283276B (en) * | 2016-08-30 | 2019-08-20 | 中国纺织科学研究院有限公司 | Solvent method produces the recovery method of N-methyl morpholine oxide during cellulose |
| CN106521657B (en) * | 2016-10-09 | 2019-03-22 | 保定天鹅新型纤维制造有限公司 | Tow washing process after a kind of Lyocell fiber spinning |
| TW202031950A (en) * | 2018-12-05 | 2020-09-01 | 奧地利商蘭仁股份有限公司 | Method for solvent and cellulose recycling in the manufacture of cellulosic spunbonded nonwovens |
| CN115323516A (en) * | 2020-12-25 | 2022-11-11 | 内蒙古双欣环保材料股份有限公司 | Six-effect evaporation, condensation and recovery device and method for fiber tow washing water |
| CN112779612B (en) * | 2021-01-07 | 2023-11-14 | 山东鸿泰鼎新材料科技有限公司 | Efficient production and manufacturing method and equipment for lyocell fibers |
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| US4477951A (en) * | 1978-12-15 | 1984-10-23 | Fiber Associates, Inc. | Viscose rayon spinning machine |
| US5053138A (en) * | 1989-10-16 | 1991-10-01 | Lenzing Aktiengesellschaft | Process for purifying an aqueous solution of N-methyl-morpholine N-oxide |
| CN1603479A (en) * | 2004-09-07 | 2005-04-06 | 东华大学 | Solvent recovery process for solvent method cellulose fiber preparation |
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2009
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4477951A (en) * | 1978-12-15 | 1984-10-23 | Fiber Associates, Inc. | Viscose rayon spinning machine |
| US5053138A (en) * | 1989-10-16 | 1991-10-01 | Lenzing Aktiengesellschaft | Process for purifying an aqueous solution of N-methyl-morpholine N-oxide |
| CN1603479A (en) * | 2004-09-07 | 2005-04-06 | 东华大学 | Solvent recovery process for solvent method cellulose fiber preparation |
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| 孟志芬等.绿色Lyocell纤维的工艺研究.《化学世界》.1998,(第12期), |
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