CN1539032A - Precipitating bath - Google Patents
Precipitating bath Download PDFInfo
- Publication number
- CN1539032A CN1539032A CNA028155386A CN02815538A CN1539032A CN 1539032 A CN1539032 A CN 1539032A CN A028155386 A CNA028155386 A CN A028155386A CN 02815538 A CN02815538 A CN 02815538A CN 1539032 A CN1539032 A CN 1539032A
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- Prior art keywords
- stillpot
- coagulation liquid
- discharge nozzle
- cover plate
- hole
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
Abstract
A precipitating bath for holding a coagulation liquid for the precipitation of shaped bodies formed from a spinning solution has a bottom and at least one precipitating bath discharge nozzle mounted in the bottom, the at least one discharge nozzle having an intake port and opposite it a discharge port for the passage therethrough of the shaped bodies formed from the spinning solution, the bath also having at least one inlet for the coagulation liquid and at least one outlet for the coagulation liquid. The precipitating bath is characterised in that it has a cover sheet with at least one hole for holding the at least one precipitating bath discharge nozzle, the cover sheet being positioned above the at least one inlet for the coagulation liquid and beneath at least one outlet for the coagulation liquid, and in that the at least one precipitating bath discharge nozzle in the at least one hole in the cover sheet is arranged such that one or more orifices are formed in the cover sheet in a ring around the at least one precipitating bath discharge nozzle. A process for the preparation of cellulosic shaped bodies is provided in which an extruded solution of cellulose in a tertiary amine N-oxide and, optionally, water is introduced into a coagulation liquid, for example in such a precipitating bath, for coagulation, wherein during the precipitation the coagulation liquid flows in countercurrent to the direction of movement of the shaped solution, at least in the region of the inlet of the shaped solution into the coagulation liquid.
Description
Invention field
The present invention relates to put the stillpot of coagulation liquid, in order to the body of precipitation from spinning solution formation.Described stillpot has a base plate and at least one to be contained in stillpot discharge nozzle on the base plate, and described at least one discharge nozzle has an import and is positioned at an outlet on its opposite, so that the body that is formed by spinning solution passes through; Described stillpot also has at least one coagulation liquid import and the outlet of at least one coagulation liquid.In addition, the present invention relates to prepare the method for cellulose body, in the method, cellulose is at tertiary amine N-oxide and may also have in the solution of water and be shaped with the condition of high temperature, the solution that is shaped is pushed in the gas medium that enters in the gas phase zone (gap) of being scheduled to, and the shaping solution that will extrude then feeds coagulation liquid so that precipitation.
Background of invention
Above-mentioned stillpot and said method are known, for example, and can be referring to JP-A-61-19805.This patent has been introduced the equipment that is used for the high speed wet spinning, and it spins initial spinning solution to the spinning funnel from nozzle.In this funnel, spinning solution contacts with coagulation liquid, and this coagulation liquid is carried along the spinning funnel wall, and body is precipitated.In funnel, spinning solution quickens significantly.But this may cause turbulent flow when spinning solution is run into coagulation liquid.This turbulent flow usually causes spinning process to be interrupted, and therefore, adopts described stillpot of JP-A-61-19805 and described method to provide stable spinning process for only a few cellulose spinning solution.Can't deny, in the embodiment of JP-A-61-19805, mentioned winding speed up to 1500 meters/minute, but, this is to obtain by the complicated and expensive like this method of several Accelerating funnels has been installed, and the result is will to start easily on the one hand, spinning process is stable again on the one hand, and this is quite difficult.
From EP-A-0817873, also can see a method of preparation cellulose fibre, be about to contain and dissolved spinning of cellulose solution and clamp-on in the gas medium in the predetermined gas phase zone (gap), then it is immersed in the collection surface in the predetermined condensation region, and by collection surface, the cellulose fibre that pull obtains also winds up.In the method, the extruding spinning solution of gas phase zone back is accelerated to a predetermined speed, the cohesion that adds laminar flow is bathed, and the direction of this laminar flow direction and extruding spinning solution is roughly the same at least.In the method, coagulation liquid adds the flow path of spinning solution from the side, and the flow direction of spinning solution and coagulation liquid is basic keeping parallelism in whole condensation region, and the gained cellulose fibre goes out to deflection leaving the condensation region rear side, winds up then.
The method that EP-A-0817873 introduced has reduced the shortcoming that is caused by the turbulent flow in the spinning funnel among the JP-A-61-19805 really, and more stable method really.And the cost of the complexity of the described technology of EP-A-0817873 and this technology equipment needed thereby of enforcement is also much lower.But, when the spinning speed height, when output was also high simultaneously, the described method of EP-A-0817873 also can cause the unstability of this technology, thereby causes the gained yarn inhomogeneous, even caused spinning process to interrupt.Inter alia, cause these instable factors to also have, when precipitating with existing equipment and/or the feasible body that is formed by spinning solution of technology, these bodies usually stick together.
The preferred embodiment for the present invention
The present invention at first seeks to provide a kind of equipment that is used to make the body that is formed by spinning solution that precipitation takes place, and this equipment can reduce the defective of above-mentioned original technology at least.Another object of the present invention provides a kind of technology, under the help of this technology, even under high yield and/or high spinning speed, can not stick together in the spinning process yet, and stable.
By the present invention is provided the stillpot of first section described type, first problem in the problems referred to above has unexpectedly obtained solution.The characteristics of described stillpot are, it has a cover plate, has a hole on the cover plate at least, is used for putting at least one stillpot discharge nozzle, and described cover plate is positioned at the top of described at least one coagulation liquid import and the below of described at least one coagulation liquid outlet; Its feature is that also at least one the stillpot discharge nozzle in described at least one cover plate hole will be arranged like this, promptly around described at least one stillpot discharge nozzle, forms one or more mouthfuls in cover plate, if a plurality of mouth then these mouths surround annular.
Because exist a plurality of in the stillpot usually, often being many stillpot discharge nozzles, so that described cover plate has usually is a plurality of, often is many holes that put the stillpot discharge nozzle, term hereinafter " stillpot discharge nozzle " also comprises " a stillpot discharge nozzle ", and vice versa.Those of skill in the art should be appreciated that within framework of the present invention, and the feature that does not all constitute the stillpot function of the hole count in stillpot discharge nozzle number and the cover plate that interrelates with these nozzles is not limited yet.
Spinning solution be cellulose at tertiary amine N-oxide, specifically be N-methylmorpholine N-oxide and may also have solution in the water time, stillpot of the present invention is particularly useful.Known in these situations, cellulose will be at higher temperature before spinning, is about usually under 55 ℃-130 ℃ to be dissolved in the suitable solvent, as the tertiary amine N-oxide and the water that may also have.Under the help of spinning head, make cellulose at tertiary amine N-oxide and may also have the solution in the water under scorching hot state, to extrude, and in this operation, be shaped.The solution that makes shaping like this is by collection surface, affiliated collection surface fill usually can not dissolving cellulos material, the aqueous solution for example.In this process, tertiary amine N-oxide extracts from shaping solution, the state precipitation of cellulose to be shaped.Between spinning head and collection surface, the cooling of shaping solution usually occurs in the so-called air gap.This cooling down operation can for example only have under the situation of air in environmental gas, but carries out under the help that blasts gas in addition usually, for example regulates the air of humiture.
In the present invention, stillpot has a so-called cover plate, and it structurally has one or more holes, and is corresponding with one or more stillpot discharge nozzles, and the result forms a circle opening around the stillpot discharge nozzle.Described cover plate can be a sheet metal.In the case, the stillpot discharge nozzle is installed usually like this, promptly makes and has only its top, be i.e. import, the split ring that close these nozzles and cover plate form.The position that cover plate is suitable should promptly make the top edge of it and stillpot discharge nozzle form a plane, promptly flushes with it.And stillpot discharge nozzle any part does not all extend to the top on the plane of cover plate formation.
Therefore, according to the present invention, on cover plate, there are one or more openings to form a circle around described at least one stillpot discharge nozzle.This is easy to finish in the following manner, and promptly cover plate is including (for example) the hole of some annular arrangements, and in each case, its diameter surpasses the diameter that is placed in stillpot discharge nozzle wherein.By this structure, opening (for example annulus) forms around the stillpot discharge nozzle in cover plate, perhaps is retained in the cover plate.Though be not preferred, but the hole in the cover plate also can tightly hold the stillpot discharge nozzle, simultaneously the hole of other (for example littler) can be used as opening and is centered around present stage is arranged in annular by the closed opening of stillpot discharge nozzle in cover plate, that is to say that this moment, cover plate had perforation.
The opening that forms around the stillpot discharge nozzle in the cover plate can be continuous, also can be discontinuous.The narrow annular slot around the stillpot discharge nozzle of mistake described above can be used as an example of continuous opening.But described opening is more suitable to be existed with discontinuous form.In a preferred implementation, the hole on the stillpot cover plate inwardly has at least one isolation strip along its edge to the hole center position.When arrange around the stillpot discharge nozzle in such hole, just formed a circle opening around this nozzle, and be interrupted by the isolation strip.
Be more preferably, in each case, there are 6 isolation strip of pointing to inside along bore edges to the center, hole in the hole on the cover plate, and these isolation strip differ 60 ° each other.For circular hole, these isolation strip form garland shape structures, and when all isolation strip isometric (preferably isometric), this structure forms smaller " interior " hole of diameter again.To be installed in this ring inner and when being positioned at the ring center when the stillpot discharge nozzle, when promptly being close to all isolation strip, around the stillpot discharge nozzle and pass cover plate and formed six openings that narrow annular channel is formed.
When settling cover plate and stillpot discharge nozzle, make them when stillpot is worked, be immersed in the coagulation liquid.This means spinning solution before the import that arrives the stillpot discharge nozzle, earlier by one section preset distance of coagulation liquid.The exhaust position of coagulation liquid is above cover plate.Therefore, coagulation liquid leaves stillpot basically on cover plate.Certainly, the part flocculating agent is also by the discharging of stillpot discharge nozzle.For stillpot of the present invention, the level of coagulation liquid should be regulated by at least one overflow baffle (wasteway) on emission point, and what it was regulated is the height of filling in of coagulation liquid.In a suitable embodiment, stillpot has (for example) rectangular shape with four sidewalls, and wherein two relative sidewalls (to call longitudinal side wall in the following text) are longer than two opposing sidewalls in addition.For instance, if two longitudinal side walls are lower than other two sidewalls, then discharge from the sidewall that hangs down some and carry out, the height of longitudinal side wall has determined the level of coagulation liquid, and promptly longitudinal side wall serves as the overflow base plate.Certainly, the amount of the coagulation liquid of overflow can collect and utilize again.For instance, this can be circulated back in the stillpot by suitable overflow launder and coagulation liquid and realize.Certainly, in the case, need guarantee that the coagulation liquid composition of being scheduled to remains unchanged, described composition is water and N-methylmorpholine N-hopcalite normally., one or more components in the recycled material also can need enrichment or minimizing before returning stillpot entering.
The height of overflow baffle better can be regulated, and this can be undertaken by the corresponding sidewall of (for example) exchange.The height of overflow baffle, and then the level of coagulation liquid at first depends on the cellulose body and the spinning condition that will be shaped.Therefore, for instance, linear density (fiber number) and spinning speed are influential to the production of yarn or multifilament.
In another specific implementations of stillpot, overflow baffle has zigzag fashion.As a result, coagulation liquid is more even along the discharging of the whole length direction of stillpot.
According to the present invention, the import of coagulation liquid is positioned at the below of cover plate.The import of coagulation liquid is positioned at the result that the below of cover plate and outlet be positioned at the cover plate top, and the position of described import and export can be set by overflow baffle, and coagulation liquid can be set from bottom to top at the flow circuits of stillpot inside.In this process, coagulation liquid stream leaves by the opening on the cover plate, and described opening circularizes arrangement around the stillpot nozzle, for example, leaves by narrow annular channel.Because waiting to precipitate body runs into coagulation liquid from above, before arriving the stillpot nozzle inlet, cover one section preset distance then, so coagulation liquid flows through one section preset distance towards the body that will precipitate in coagulation liquid inside.In other words, stillpot of the present invention is the adverse current stillpot, and wherein the flow direction of coagulation liquid is opposite with the flow direction that enters body wherein, for example, is being positioned at or near the import that body enters the stillpot discharge nozzle, is flowing to about 180 ° of calculating deflection with this at least.With regard to the body quality of precipitation and precipitation, adverse current has caused tangible improvement.Can think, because the existence of this adverse current, the phenomenon that forms eddy current (jet flow) in the body that will precipitate enters the coagulation liquid of porch of stillpot can be avoided or alleviate, this so that can prevent in body inside, for example between many monofilament of single line, stick together.With at a high speed, as 100-1500 rice/minute, be preferably 500-1000 rice/minute, more be preferably 800-1200 rice/minute the speed spinning, be preferably when spinning multifilament threads with high linear density (fiber number), this favourable effect is especially remarkable.Owing to this reason, stillpot of the present invention is specially adapted to high speed spinning.
Coagulation liquid should enter stillpot by distributing pipe, and described distributing pipe is positioned at the cover plate below, and (for example) is parallel to the longitudinal side wall of stillpot.These distributing pipes are equipped with several little outlet openings on whole pipe length, coagulation liquid is discharged by these little outlet openings.This makes the coagulation liquid discharging evenly.Distributing pipe should extend on the whole length of stillpot, and outlet opening should evenly distribute on the whole length of pipe.
In a preferred embodiment, distributing pipe is settled like this, makes open pore to become the direction of (for example) 45 to be tilted to down with the stillpot bottom.This can produce in stillpot of the present invention more effectively and flow.On the whole length of stillpot, in stillpot, add coagulation liquid indirectly, further guaranteed coagulation liquid with regard to temperature and additive (for example NMMO), the even distribution on whole stillpot length direction by distributing pipe.In addition, the contingent folder that twines of yarn also can be eliminated.Coagulation liquid also should enter the stillpot discharge nozzle from both direction, for example the direction of two symmetries.For example, by adopting two distributing pipes, every is parallel to the stillpot longitudinal side wall, and is parallel to row's stillpot discharge nozzle, can strengthen above-mentioned effect.This can make the coagulation liquid that enters stillpot more even, and can prevent turbulent flow.
The stillpot discharge nozzle of stillpot of the present invention can be connected on the base plate of stillpot, and be preferably movable.Charging aperture is positioned at the coagulation liquid the inside, and floss hole is embedded on the base plate, thereby can precipitate good body (for example silk) from the stillpot discharging, and reels they collections by (for example).Certainly, along with settled body ejects from stillpot, some coagulation liquids also are brought out, for example owing to it sticks on the silk of discharge.For reclaim these coagulation liquids also/or make dry run easier, the coagulation liquid that should will stick on the body is separated above it.This can accomplish, for example body is pulled out sideling from the stillpot discharge nozzle.This discharging modes can make adhesive liquor separate, and return stillpot.
The stillpot discharge nozzle can be used a kind of inert material, for example metal or ceramic material manufacturing.Studies show that,, carry out unglazed chromium plating then, obtain so-called " tangerine peel " structure, will be particularly conducive to from body so and more leniently adhesive liquor be separated if the discharge nozzle of stillpot of the present invention is made with high-grade steel (stainless steel).
The base plate of stillpot of the present invention can out-of-flatness.For example, be arranged in a row when the stillpot discharge nozzle is parallel to stillpot direction radially on edge, stillpot base plate middle part, then this base plate central region should be higher than the zone of base plate both sides, i.e. its more close cover plate.And this two zones in the back can be installed distributing pipe easily.This design advantageous particularly, because the trough degree of depth consequently, promptly the degree of depth of the coagulation liquid of the body that is formed by spinning solution by wherein can keep lower.Particularly advantageous is that the degree of depth of the coagulation liquid of stillpot discharge nozzle below more is preferably about 10-20mm only for about 10-40mm.We are surprised to find, no matter body passes through coagulation liquid with which kind of speed, the low like this degree of depth all can significantly reduce the formation of eddy current.Consequently, body can better contact with coagulation liquid, thereby significantly improves filling effect.Same because the stillpot degree of depth is more shallow, when spinning speed was higher, friction loss was also lower.
In addition, the cover plate of stillpot of the present invention should further comprise (at least one) other hole, and these holes are connected with the stillpot base plate by small-bore pipeline (capillary).These extra holes can be used as so-called " emergency exit " on the cover plate.These emergency exits on the cover plate are connected with the capillary in being installed in stillpot, and its top edge flushes with cover plate, and does not form other hole in this process.These capillaries make the stillpot bottom to forming straight clear passage between the opening.On the cover plate these extra holes and the capillary that is attached thereto when the precipitation beginning of great use, for example when repiece, so as in the first step as far as possible fast and reposefully with one one line drawing by whole stillpot.Separated time subsequently, and pass the stillpot discharge nozzle respectively.If at the spinneret duration of work, one or several position fluctuation of service that spins is arranged, the multifilament in then corresponding line or the single line can be discharged by these emergency exits.Can prevent the obstruction of stillpot discharge nozzle like this.After the repiece, perhaps no the time, capillary can seal, and for example seals from below with the taper rubber stopper.
The present invention also provides the method for preparing the cellulose body, in the method, cellulose is at tertiary amine N-oxide and may also have the solution in the water to be shaped in the condition of high temperature, the solution that is shaped is clamp-oned in the gas medium of being scheduled in the gas phase zone (gap), and the shaping solution that will extrude subsequently feeds coagulation liquid, precipitates, it is characterized in that, in precipitation process, the flow direction of coagulation liquid is opposite with the flow direction of shaping solution, is like this in the import department that shaping solution enters coagulation liquid at least.
In precipitation process, the flow direction of coagulation liquid is even and effective with the opposite precipitation that makes of the flow direction of the shaped fibers cellulose solution that will precipitate, and this character for the gained body has positive impact.All the more so for the character of spinning the formed line of cellulose fiber peacekeeping silk (fiber) with this counter-current process.
The described process that is settled out the cellulose body should utilize stillpot of the present invention to carry out.
If the cellulose body with prepared of the present invention is cellulose fibre or silk, these fibers or silk should be handled with known method after leaving stillpot so, for example clean, apply finishing agent, drying and coiling.
After cellulose fibre or silk left stillpot, during as stillpot of the present invention, the suitable especially floss hole EDGE CONTACT that turns to side and at least one stillpot discharge nozzle was earlier further handled then.The side direction transfer of cellulose fibre or silk is more suitable to be carried out like this, and promptly they overflow the floss hole edge of one or more stillpot discharge nozzles.In this way, can remove the coagulation liquid that adheres to and carry secretly preferably.
Generally speaking, the inventive method can to the line that might form carry out homogeneous precipitation (cohesion).The line of gained has physics, optics and weaving character highly uniformly.The inventive method especially can be preferably the multifilament threads with high linear density and carry out high-speed spinning silk, described speed be 100-1500 rice/minute, be preferably 500-1000 rice/minute, more be preferably 800-1200 rice/minute.
A special benefits of stillpot of the present invention and the inventive method is, the product that spinning obtains is because picked-up (absorption) dyestuff is even unusually, prolongedly do not take off.In the fabric, particularly woven fabric made by this silk, this effect is especially obvious, because the striped above them greatly reduces, the trend that forms striped also greatly reduces.This positive result is attributable to the particular geometries of stillpot, what deserves to be mentioned is that especially the stillpot degree of depth at stillpot discharge nozzle place is more shallow.The less stillpot degree of depth has obviously been brought above-mentioned benefit really, and this is unexpected fully, because this effect can't be predicted.
Description of drawings
Further set forth the present invention below in conjunction with accompanying drawing and some examples.In these accompanying drawings, Fig. 1 is the cross-sectional of a suitable example of stillpot of the present invention, and Fig. 2 is the diagrammatic side views of zigzag overflow baffle, and Fig. 3 is the top plan view sketch of cover plate.
Stillpot be positioned at spinning head 1 and air gap 2 below.By a set screw, stillpot can be regulated, itself and be that height between the spinning head 1 is a distance.By this method, can regulate the length of air gap 2, i.e. distance between spinning head 1 and the stillpot.
In embodiment illustrated in fig. 1, the length of stillpot is about 1000mm, and width is about 250mm.At the two ends of stillpot length direction, a removable zigzag overflow baffle 5 and an overflow launder 12 are arranged respectively.In a narrow side of stillpot, a joint for coagulation liquid 4 feeding lines is arranged.Feeding line is positioned at the middle part, seals distributing pipe 8 by being encircled by O-shape of a three-way pipe and two insertions, and liquid distributes in the both sides of stillpot length direction.The external diameter of two distributing pipes 8 is 20mm, installs along being parallel to the stillpot length direction.They respectively have 40 discharge openings, so that coagulation liquid 4 is evenly distributed on the whole length direction of stillpot.When inserting distributing pipe 8, make discharge opening with direction directed downwards from the horizontal by 45.The back of the body end of distributing pipe 8, promptly opposite with inserting that face of a three-way pipe end is sealed with stopper, and uses the polytetrafluoroethylene (PTFE) rubber belt sealing.What be positioned at the stillpot middle part is stillpot discharge nozzle 10, and it is parallel to the length direction of stillpot.Every fiber (line of being made up of multifilament 3) 11 is from spinning head 1, by stillpot discharge nozzle 10.Stillpot discharge nozzle 10 can be removed, and fixing with O-shape ring in the time of in being used in stillpot, the direction along trough seals simultaneously.Stillpot discharge nozzle 10 usefulness stainless steels are made matt chromium plating, and matt chromium plating is to make its surface have " tangerine peel " structure.
A cover plate 6 with holes is arranged in the stillpot, and stillpot discharge nozzle 10 is installed in the hole.Cover plate flushes with the top edge of stillpot discharge nozzle 10.In addition, also have 6 holes on the cover plate, promptly so-called urgent discharge opening.
Urgent discharge opening on the cover plate 6 is connected with capillary 7, and capillary is installed in the stillpot, and its top edge flushes with cover plate 6.Capillary 7 is parallel with the stillpot discharge nozzle.Below stillpot, promptly some holes are arranged in the stillpot bottom, make capillary 7 can freely pass through trough.If do not need these urgent discharging capillaries 7, can they be sealed with taper rubber stopper 9.These urgent discharging capillaries 7 have been welded on the stillpot bottom.
Figure 2 shows that the diagrammatic side views of overflow baffle 5 among Fig. 1.The zigzag fashion of flow-stopping plate is high-visible, and this shape can make the overflow of flocculating agent very even.
Figure 3 shows that the plan view from above of cover plate 6 among Fig. 1.In this figure, at first can see some holes 13 of stillpot discharge nozzle 10 usefulness.Each hole 13 all shows 6 isolation strip 14 in addition, and they apart 60 °.These isolation strip are pointed to inboard, so just make hole 13 have definite internal diameter.Stillpot discharge nozzle 10 and the strict coupling of the internal diameter in hole 13.In addition, Fig. 3 also show with Fig. 1 in the urgent discharge opening 15 of urgent discharging capillary 7 usefulness.
The top edge of these urgent discharge openings 15 has carried out flat bore hole with 45 ° of directions, to avoid forming sharp-pointed edge.Two types hole 13 and 15 distributes by this way on the cover plate 6, and promptly always there is an outlet opening 15 centre in the hole 13 of two stillpot discharge nozzle 10 usefulness, that is to say, per two fibers 11 always have an emergency exit.
Stillpot shown in Figure 1 is a kind of adverse current stillpot, and promptly the flow direction of coagulation liquid 4 shown in the arrow becomes 180 ° with the flow direction of fiber that enters this coagulation liquid or monofilament among Fig. 1.
Coagulation liquid is by container (reservoir) circulation.This circulating device comprise consistency controller, pump, the band temperature controller of a container, control coagulation liquid 4 each concentration of component heat exchanger, filtration system, be used to set the flowmeter and the stillpot of volume required stream.Unnecessary coagulation liquid is made up of the coagulation liquid overflow 12 of stillpot and the coagulation liquid of removing from fiber 11 4, and it flow back in the container again.Stillpot circulation is in the constant temperature current downflow that is set at 5 °-30 ℃.Because wet fiber 11 is also often taken away some coagulation liquids of failing to extract 4 after leaving stillpot, this loss in the stillpot circulation must compensate.In addition, because (for example) NMMO is diffused into the coagulation liquid from filament, in coagulation liquid, assembled NMMO.Replenish any component (as water) in the stillpot, owing to being taken out of the loss that causes, and keep required NMMO concentration, can be undertaken by the NMMO consistency controller with compensation.Certainly, also can add other additives by this way, for example be used for avoiding the gathering or the sedimentation of body, perhaps change the character of body.
As previously described, in practical operation, the silk 3 one by one of each fiber 11 from top to bottom enters in the coagulation liquid 4 separately, and tiltedly pull process stillpot discharge nozzle 10 is dipped down---so that remove coagulation liquid 4 from fiber 11.In addition,, can bathe the surface by settlement, can guarantee like this that promptly precipitating bath has even, constant height in whole precipitating bath surface range, and turbulent flow can not occur by the cover plate 6 that will place stillpot.
Claims (15)
1. can put the stillpot of coagulation liquid, the body that it forms from spinning solution in order to precipitation, described stillpot has base plate and at least one to be contained in stillpot discharge nozzle on the base plate, described at least one discharge nozzle has an import and is positioned at the outlet on opposite, so that the body that is formed by spinning solution passes through; Described stillpot also has at least one coagulation liquid import and the outlet of at least one coagulation liquid, it is characterized in that, described stillpot has cover plate, has a hole on the cover plate at least, be used for putting at least one stillpot discharge nozzle, described cover plate is positioned at the top of described at least one coagulation liquid import and the below of described at least one coagulation liquid outlet; At least one stillpot discharge nozzle in described at least one cover plate hole will be arranged like this: promptly in the annular of described at least one stillpot discharge nozzle, form one or more holes in cover plate.
2. the described stillpot of claim 1, it is characterized in that spinning solution be cellulose at tertiary amine N-oxide, better be solution in the N-methylmorpholine N-oxide and the water that can have.
3. claim 1 or 2 described stillpots is characterized in that at least one the stillpot discharge nozzle in described at least one cover plate hole is settled like this, make the import of at least one stillpot discharge nozzle flush with the cover plate plane.
4. each described stillpot of claim 1-3 is characterized in that at least one hole on the described cover plate inwardly has at least one isolation strip along its edge to the hole center position.
5. the described stillpot of claim 4 is characterized in that there are 6 isolation strip of pointing to the inboard along bore edges to the center, hole, apart 60 ° of these isolation strip at least one hole on the cover plate.
6. each described stillpot of claim 1-5 when it is characterized in that from stillpot discharging coagulation liquid, has the height of filling in of an overflow baffle control coagulation liquid at least.
7. the described stillpot of claim 4 is characterized in that described at least one overflow baffle is zigzag.
8. each described stillpot of claim 1-7 is characterized in that described at least one stillpot discharge nozzle made by stainless steel, carries out unglazed chromium plating subsequently.
9. each described stillpot of claim 1-8 is characterized in that described cover plate has at least one extra hole, and they are connected with the stillpot base plate by capillary.
10. each described stillpot of claim 1-9 is in the application of spinning in the multifilament fiber, its spinning speed be 100-1500 rice/minute, be preferably 800-1200 rice/minute.
11. prepare the method for cellulose body, in the method, hot shaping in the solution of cellulose in the tertiary amine N-oxide and the water that can have, the solution that is shaped is clamp-oned in the gas medium of being scheduled in the gas phase zone gap, and the shaping solution that will extrude subsequently feeds coagulation liquid, so that precipitate, it is characterized in that, in precipitation process, the flow direction of coagulation liquid is opposite with the flow direction of moulding solution, is like this in the import department that shaping solution enters coagulation liquid at least.
12. the described method of claim 11 is characterized in that the cellulose body is deposited in the stillpot and carries out in each described stillpot of claim 1-9.
13. the described method of claim 12 is characterized in that described cellulose body is cellulose fibre or silk, they also will further be handled after leaving stillpot.
14. the described method of claim 13 is characterized in that leaving the cellulose fibre or the silk of stillpot, turns to the floss hole EDGE CONTACT of side and at least one stillpot discharge nozzle earlier, further processing then.
15. each described method of claim 11-14, the speed of spinning that it is characterized in that multifilament threads be 100-1500 rice/minute, be preferably 800-1200 rice/minute.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10139679.1 | 2001-08-11 | ||
| DE10139679 | 2001-08-11 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1539032A true CN1539032A (en) | 2004-10-20 |
| CN1325704C CN1325704C (en) | 2007-07-11 |
Family
ID=7695276
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB028155386A Expired - Lifetime CN1325704C (en) | 2001-08-11 | 2002-08-09 | Precipitating bath |
Country Status (7)
| Country | Link |
|---|---|
| EP (1) | EP1425441B1 (en) |
| KR (1) | KR100903075B1 (en) |
| CN (1) | CN1325704C (en) |
| AT (1) | ATE347627T1 (en) |
| DE (1) | DE60216617T2 (en) |
| TW (1) | TW577940B (en) |
| WO (1) | WO2003014432A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113737390A (en) * | 2021-08-27 | 2021-12-03 | 武汉南望环保技术研究有限责任公司 | Production process and production system of regenerated cellulose fiber short fiber spunlace non-woven fabric |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101562080B1 (en) | 2011-06-23 | 2015-10-20 | 코오롱인더스트리 주식회사 | Coagulation Appartus for Spinning |
| EP2719801A1 (en) * | 2012-10-10 | 2014-04-16 | Aurotec GmbH | Spinning bath and method for solidifying a moulded part |
| EP3467161A1 (en) | 2017-10-06 | 2019-04-10 | Lenzing Aktiengesellschaft | Lyocell type cellulose filament production process |
| KR20200059291A (en) | 2017-10-06 | 2020-05-28 | 렌징 악티엔게젤샤프트 | Flame retardant lyocell filament |
| EP3505659A1 (en) | 2018-08-30 | 2019-07-03 | Aurotec GmbH | Method and device for filament spinning with inflection |
| EP3674454A1 (en) | 2018-12-28 | 2020-07-01 | Lenzing Aktiengesellschaft | Cellulose filament process |
| EP3747295A1 (en) | 2020-01-21 | 2020-12-09 | Lenzing Aktiengesellschaft | Footwear that contains a lyocell continuous filament yarn |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0118088B1 (en) * | 1983-02-28 | 1986-11-26 | Asahi Kasei Kogyo Kabushiki Kaisha | Process and apparatus for preparation of polyparaphenylene terephthalamide fibers |
| US4531456A (en) * | 1984-09-26 | 1985-07-30 | Fmc Corporation | Liquid distribution trough |
| US5417909A (en) * | 1992-06-16 | 1995-05-23 | Thuringisches Institut Fur Textil- Und Kunststoff-Forschung E.V. | Process for manufacturing molded articles of cellulose |
| AT399729B (en) * | 1993-07-01 | 1995-07-25 | Chemiefaser Lenzing Ag | METHOD FOR PRODUCING CELLULOSIC FIBERS AND DEVICE FOR IMPLEMENTING THE METHOD AND THE USE THEREOF |
| GB9500387D0 (en) * | 1995-01-10 | 1995-03-01 | Courtaulds Fibres Ltd | Manufacture of extruded articles |
| DE19512053C1 (en) * | 1995-03-31 | 1996-10-24 | Akzo Nobel Nv | Process for the production of cellulosic fibers |
| CN1076405C (en) * | 1996-10-25 | 2001-12-19 | 纳幕尔杜邦公司 | Process for making high tenacity aramid fibers |
| DE19954152C2 (en) * | 1999-11-10 | 2001-08-09 | Thueringisches Inst Textil | Method and device for producing cellulose fibers and cellulose filament yarns |
-
2002
- 2002-08-09 WO PCT/EP2002/009820 patent/WO2003014432A1/en active IP Right Grant
- 2002-08-09 DE DE60216617T patent/DE60216617T2/en not_active Expired - Lifetime
- 2002-08-09 TW TW091118336A patent/TW577940B/en not_active IP Right Cessation
- 2002-08-09 EP EP02772260A patent/EP1425441B1/en not_active Expired - Lifetime
- 2002-08-09 CN CNB028155386A patent/CN1325704C/en not_active Expired - Lifetime
- 2002-08-09 KR KR1020047001687A patent/KR100903075B1/en active IP Right Grant
- 2002-08-09 AT AT02772260T patent/ATE347627T1/en not_active IP Right Cessation
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113737390A (en) * | 2021-08-27 | 2021-12-03 | 武汉南望环保技术研究有限责任公司 | Production process and production system of regenerated cellulose fiber short fiber spunlace non-woven fabric |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1425441A1 (en) | 2004-06-09 |
| EP1425441B1 (en) | 2006-12-06 |
| KR20040026702A (en) | 2004-03-31 |
| DE60216617D1 (en) | 2007-01-18 |
| TW577940B (en) | 2004-03-01 |
| WO2003014432A1 (en) | 2003-02-20 |
| CN1325704C (en) | 2007-07-11 |
| ATE347627T1 (en) | 2006-12-15 |
| KR100903075B1 (en) | 2009-06-18 |
| DE60216617T2 (en) | 2007-09-27 |
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