CN1132971C - Method for continuous preparation of polyvinyl alcohol uniform spinning solution - Google Patents
Method for continuous preparation of polyvinyl alcohol uniform spinning solution Download PDFInfo
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- CN1132971C CN1132971C CN 00132182 CN00132182A CN1132971C CN 1132971 C CN1132971 C CN 1132971C CN 00132182 CN00132182 CN 00132182 CN 00132182 A CN00132182 A CN 00132182A CN 1132971 C CN1132971 C CN 1132971C
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Abstract
The present invention relates to a continuous preparation method for a polyvinyl alcohol uniform spinning solution, which comprises the steps that suspension liquid of polyvinyl alcohol is prepared by swelling in advance by adopting a double screw extruder through using DMSO as solutions under proper temperature, and the suspension liquid is continuously and quantitatively fed in the double screw extruder for completing swelling, dissolution, deaeration and measurement output under normal pressure and low temperature. The method combines and completes the three traditional procedures of dissolution, vacuum deaeration and spanning for preparing spinning solutions together, avoids the thermal oxidative degradation, and has the advantages of rapidity, high efficiency and energy saving.
Description
Technical field
The invention relates to a kind of continuous preparation method of polyvinyl alcohol uniform spinning solution, more particularly about the continuous preparation method of polyvinyl alcohol of high degree of polymerization uniform spinning solution.
Background technology
The continuous preparation of polyvinyl alcohol of high degree of polymerization uniform spinning solution is one of key that polyvinyl alcohol gel spun spins or wet method is spun, and it is the key factors such as mechanical property, production cost, efficient and equipment input of the influence fiber that spins directly.
Novel polyethylene alcohol (PVA) fiber (hereinafter to be referred as the K-II fiber) is a kind of novel special fibre that Japanese Network ラ レ company releases, it is with organic solvent PVA to be carried out uniform dissolution, this solution spues through spinnerets, rapid solidification cooling in coagulating bath, form the frozen glue precursor of PVA, then with extractant extract being included in solvent in the frozen glue precursor, drying and super drawing handle, and makes novel K-II fiber.
One of key of K-II fiber production is the continuous preparation and the frozen glue precursor forming process (the frozen glue precursor that promptly prepares garden shape) of uniform spinning solution.The formation of garden shape frozen glue precursor relates to the homogeneity and the high concentration of spinning solution, and the rapid cooling frozen glue in the precursor forming process is shaped.
Wet method and dry spinning in the past: be in still, to implement at first, be about to condensate and place the dissolution kettle that fills solvent, deaeration and spinning after agitating heating is dissolved to polymeric dissolving.This method has following shortcoming: (1) dissolution time is long; (2) it is low to contain polymer concentration in the obtained solution; (3) thermal oxidative degradation easily takes place in the condensate to poor stability; (4) there are a large amount of bubbles to exist in the solution, need carry out deaeration before spinning and handle; (5) whole dissolving, deaeration and spinning are batch processes; (6) production discontinuity and the equipment cleaning problem that causes by batch process.This shows that the spinning of still formula is limitation, the long flow path that it is arranged, take up an area of shortcomings such as big and energy consumption height.Especially when preparation polyvinyl alcohol of high degree of polymerization solution, because the preparation of high viscosity homogeneous solution has difficulties, and bigger obstacle is that the high viscosity solution deaeration can't carry out, and influenced the process of fiber industrialization.
U.S. Allied company discloses in 440,711 patents and has adopted double screw extruder to implement high polymerization degree PVA is carried out the method that continuous-dissolution prepares uniform spinning solution at US4.This technical process has comprised following step: (one) with PVA with evenly mix in solvent places mixing kettle, heat and make it to become the PVA slurry; (2) above-mentioned slurry is put into the dissolution kettle that has double-helical hybrid heater, implement predissolve and clamp-on double screw extruder by force; (3) the inhomogeneous solution of above-mentioned predissolve in double screw extruder, dissolve fully, quantitatively output and spinning extrude.This method makes the effect of the high shear that utilizes double screw extruder, reach quick preparation PVA uniform spinning solution, but following defective also comes out: (1) is even the even output of PVA slurry---the PVA slurry is at stirring, because slurry is inhomogeneous, cause slurry when output, to be difficult to guarantee output uniformly,, can cause that valve port stops up as the delivery valve stenostomia, it is even to cause the output slurry to contain the PVA density unevenness, finally makes dissolving back PVA concentration big fluctuation occur; (2) thermal oxidative degradation takes place in PVA in the feeding blender of double screw extruder---in view of being one, blender is with double-helical heater, slurry is in this heating for dissolving, PVA is in high temperature and contacts with air this moment, thermal oxidative degradation very easily takes place, cause degraded of the PVA degree of polymerization and molecular weight distribution to broaden, finally can influence the mechanical property of finished fiber; (3) air is sneaked into double screw extruder, making PVA that thermal oxidative degradation take place---the PVA solution after dissolving is when stirring input double screw extruder, have a certain amount of gas and sneak into simultaneously, the condition of high temperature during dissolving is disadvantageous to stablizing the PVA degree of polymerization and molecular weight distribution undoubtedly.
The Japanese Network ラ レ JP86-143 of company in 1986,439 have released the method that a kind of new double screw extruder dissolves PVA, and this technology has comprised following step: (one) carries out quantitative feeding from different spouts to double screw extruder with PVA respectively with solvent; (2) PVA and solvent are finished the overall process of swelling, dissolving under the heating of double screw extruder and high shear forces; (3) offer the deaeration mouth at the end of double screw extruder, implement bubble in the solution is removed; (4) again to solution carry, supercharging, metering output and spinning afterwards.Though this method has solved US4, also there is following defective in 440,711 feeding uniformity and the thermal oxidative degradation problems that exist:
(1) course of dissolution time weak point is restricted the uniformity and the capacity of equipment performance of dissolving---owing to feed liquid time of staying in double screw extruder is limited to by the draw ratio of double screw extruder and rotating speed.Feed liquid time of staying in screw rod is short, can not satisfy the requirement of uniform dissolution; If prolong the time of staying, influence the fan-out capability of screw rod again; (2) air is sneaked in the double screw extruder, causes the thermal oxidative degradation of PVA---and when solid PVA imported, air will enter with particle, and PVA solution needs through high-temperature digestion process, 0 afterwards
2Existence certainly will cause the thermal oxidative degradation of PVA; (3) difficulty of deaeration---double screw extruder has degassing function on the principle, yet this material that is engraved in the screw rod is a solution state, and it is high like that viscosity of sludge can not show a candle to polymer malt viscosity, so cause forming high pressure (＞20 kilograms per centimeter
2) difficulty, and when pressure discharges exhaust, solution is very easily from the overflow of deaeration mouth with overflow, solvent is overflowed with exhaust, causes the change of solution concentration; (4) difficulty set up again of solution output pressure---in view of the requirement of spinning, the spinning solution of twin-screw output should have certain pressure, just can finish spinning requirement such as the filtration of high viscosity solution, stable output, this major diameter that just needs to increase screw rod recently satisfies above-mentioned requirements.This shows that this technological process faces problems on practical application and raising productivity effect, wherein distinct issues are deaerations of high viscosity spinning solution the most.
Summary of the invention
One of purpose of the present invention overcomes PVA that prior art exists and solvent provide a kind of polyvinyl alcohol uniform spinning solution in proportion to dissolving, deaeration problem and the thermal oxidative degradation problem of inhibition PVA in course of dissolution of the difficulty of double screw extruder feeding and high concentration PVA solution continuous preparation method.
Two of purpose of the present invention is the dissolving of traditional preparation process spinning solution, vacuum defoamation and three operations of spinning to be merged finish together, has avoided the generation of thermal oxidative degradation, not only fast, efficiently but also energy-conservation.
This and other purpose of the present invention will specify and describe further and set forth by following.
In the present invention, the continuous preparation method of polyvinyl alcohol uniform spinning solution of the present invention, adopt double screw extruder, polyvinyl alcohol is carried out pre-swelling in solvent, make the suspension of polyvinyl alcohol, the degree of polymerization of described polyvinyl alcohol is 1000～6000, the concentration of polyvinyl alcohol in solution is 15～40Wt%, the swelling time of polyvinyl alcohol in solvent is 10～20 minutes, and temperature is 30～60 ℃, and the swelling multiplying power is 1.0～3.0.
Further, the continuous preparation method of polyvinyl alcohol uniform spinning solution of the present invention, adopt double screw extruder, polyvinyl alcohol is carried out pre-swelling in solvent, make the suspension of polyvinyl alcohol, the degree of polymerization of described polyvinyl alcohol is 1700～6000, the concentration of polyvinyl alcohol in solution is 15～30Wt%, the swelling time of polyvinyl alcohol in solvent is 10～20 minutes, and temperature is 30～40 ℃, and the swelling multiplying power is 1.05～2.5.
In the present invention, the solvent that is adopted is dimethyl formamide, dimethylacetylamide, dimethyl sulfoxide (DMSO), ethylene glycol and water, can use their mixture, also can use wherein a kind of separately.
The continuous preparation method of polyvinyl alcohol uniform spinning solution of the present invention, be included under low temperature and the atmospheric pressure state, with the saturated continuously feeding double screw extruder inlet of this suspension, the screwing element in the double screw extruder is formed by exporting, seal, knead and measure the multiple element of output.
In the present invention, each temperature of double screw extruder is set at: the feeding mouth temperature is that T is molten bloated below-10 ℃, and middle proparea temperature is T
Molten expanding-10 ℃～T
Molten expanding+ 20 ℃, middle back zone temperature is T
Dissolving-10 ℃～T
Dissolving+ 20 ℃, rear portion metering (outlet) temperature is T
Dissolving± 2 ℃, the screw speed of double screw extruder is 80～180 rev/mins, and suspension time of staying in double screw extruder is 3～10 minutes, and the head pressure of double screw extruder is 20 kilograms per centimeter
2More than.
Further, each temperature of double screw extruder is set at: the feeding mouth temperature is below 20 ℃, and middle proparea temperature is T
Molten expanding-T
Molten expanding+ 10 ℃, middle back zone temperature is T
Swelling-T
Dissolving+ 10 ℃, rear portion metering (outlet) temperature is T
Dissolving± 2 ℃, the screw speed of double screw extruder is 80～180 rev/mins, and the time of staying of suspension in double screw extruder is 3～5 minutes, and the head pressure of double screw extruder is 20～40 kilograms of kilograms per centimeter
2
In the continuous preparation method of polyvinyl alcohol uniform spinning solution of the present invention, at the double screw extruder inlet feeding funnel is set, the suspension of polyvinyl alcohol is exported to the feeding funnel of double screw extruder continuously saturatedly, this suspension liquid level is higher than 5～20 centimetres of double screw extruder inlet faces, overhead clearance part suspension overflows from the flash mouth, returns the storage still of suspension.
In the continuous preparation method of polyvinyl alcohol uniform spinning solution of the present invention, polyvinyl alcohol suspension is finished swelling, dissolving, deaeration and metering output in double screw extruder.The bubble of polyvinyl alcohol suspension in double screw extruder is to discharge from feeding mouth by the high pressure in screw rod.
In the present invention,, increase the suspension of PVA in solvent, thereby reach steady concentration in the output PVA suspension because PVA has been carried out pre-swelling; And at the double screw extruder inlet feeding funnel is set, double screw extruder is implemented saturated feeding, stop air to enter among the screw rod, avoid the thermal oxidative degradation of PVA in course of dissolution thereby reach; Utilize PVA course of dissolution medium viscosity to increase severely, very fast formation high pressure is discharged micro bubble from feeding mouth in screw rod, reaches the purpose of continuous-dissolution deaeration.
Method of the present invention merges the dissolving of traditional preparation process spinning solution, vacuum defoamation and three operations of spinning to be finished together, has avoided the generation of thermal oxidative degradation, not only fast, efficiently but also energy-conservation.
Among the present invention, because proportion there are differences between PVA and the solvent, its mixture non-uniform phenomenon can occur when output, cause the fluctuation of concentration of final solution.By pre-swelling to PVA, increased the suspension of PVA in solvent, but the uniformity of the output PVA content of stable suspension; Implement before also PVA part swelling process consuming time being moved to simultaneously the feeding screw rod, alleviated the burden of double screw extruder, improved the uniformity and the production efficiency of PVA solution the PVA dissolving.
The preswollen purpose of PVA is to improve the suspension of PVA in solvent, therefore must control the swelling of PVA, and its method is the swelling multiplying power of control PVA:
The PVA suspension of ※ after to swelling adopts supercentrifuge to dry, weigh.
※ ※ to swelling after PVA dry, use 100 ℃ of dry 1hrs of methanol extraction again
PVA swelling and swelling temperature, solvent species are relevant, selected solvent and swelling temperature (Tswelling) down PVA can obtain best swelling rate, this swelling temperature can be tried to achieve by swell test or swelling DSC curve (seeing CN1050884A).
The PVA suspended substance is put into the feeding funnel of double screw extruder, make the suspension liquid level be higher than the inlet of double screw extruder, so just, played the fluid-tight effect, stoped air to enter double screw extruder, thereby suppressed the generation of the thermal oxidative degradation of thermal sensitivity PVA, alleviated the burden of solution deaeration simultaneously again.Yet, in solid, liquid, still containing minimum gas and sneak into, this part minimum gas is to depend on PVA dissolving viscosity to increase severely, and forms huge pressure in the screw rod, this part gas is inevitable to move to the low pressure direction.In order to make trace that the passage of discharge be arranged, keep low viscosity, the low temperature of suspension at the entrance of double screw extruder, the survival gas in the screw rod is discharged thus, thereby the deaeration mouth of double screw extruder end was got rid of in the past.
In order to implement the dissolving of high polymerization degree PVA, on equipment, adopted special screwing element combination (conveying, kneading, sealing and measuring element etc.); Adopt (i) feeding section to reach the abundant mixing of feed liquid on technology, selecting temperature for use is T
SwellingBelow-10 ℃.(ii) the swelling section reaches the abundant swelling of feed liquid, and selecting temperature for use is T
Swelling-T
Swelling+ 20 ℃.(iii) lysing segment reaches (the solution temperature T of dissolving fully of solution
Dissolving), selecting temperature for use is T
Dissolving-10 ℃-T
Dissolving+ 20 ℃ (iV) metering deferent segment reaches the quantitative output of solution, and selecting temperature for use is T
Dissolving± 2 ℃ reach in dissolving, the bubble in the solution are drained.
Description of drawings
Fig. 1 is a polyvinyl alcohol gel spun spinning process schematic flow sheet
In Fig. 1, symbol 1 is represented the colvent inlet, and symbol 2 is represented polyvinyl alcohol and auxiliary agent inlet, symbol 3 is represented the swelling still, and symbol 4 is represented the homogeneous still, and symbol 5 is represented the feeding funnel, symbol 6 is represented circulating pump, and symbol 7 is represented double screw extruder, and symbol 8 is represented booster pump, symbol 9 is represented filter, symbol 10 is represented measuring pump and assembly, and symbol 11 is represented the polyvinyl alcohol spinning solution, and symbol 12 is represented coagulating basin, symbol 13 is represented polyvinyl alcohol gel spun fiber, and symbol 14 is represented the Sheng Si tube.
In the present invention, certainly also should add conventional additive and auxiliary agent in some spinning productions, also need use some conventional method and operations if necessary, these steps, method and additive and auxiliary agent are known for those skilled in the art, seldom explain at this.
Below further specify the present invention by specific embodiment, in the present invention as non-refering in particular to, all deals are unit of weight, embodiment only be to the explanation of inventing, and can not limit the scope of the invention.
The specific embodiment
Embodiment 1:
PVA, auxiliary agent and the solvent DMSO of DP value 1700 are added to the (PVA: DMSO=22: 78 w/w) of (3) the swelling still from charge door (1) (2) respectively.Open and stir and the interlayer heating, make and expect in the still that temperature rise is to T
Swelling=30～35 ℃, and be incubated 20 minutes, the swelling multiplying power of PVA is 110% this moment, at once the suspension of PVA is cooled to 20～25 ℃ subsequently, and standby in the homogeneous still (4) in the middle of being transferred to.
Above-mentioned PVA suspension is put into feeding funnel (5), and keep the suspension liquid level to exceed 10 centimetres of double screw extruder (7) inlets.It is evenly mixed up and down that suspension in the funnel (5) adopts high speed agitator to carry out, and concentration is even up and down in feeding funnel (5) to keep suspension.The suspension that surpasses above-mentioned height overflows from the overfall of feeding funnel side, and is back to by circulating pump (6) and spares in the matter still (4).
PVA suspension carries out swelling, dissolving, deaeration and metering output in the end opening inflow double screw extruder (7) of feeding funnel (5), actual conditions is:
Double screw extruder type: parallel co-rotating twin screw extruder;
2 * 34 millimeters L/D=39 of Φ, 7 joint barrels add thermal control;
The screwing element of double screw extruder: the screwing element organic assembling of carrying, knead, sealing and measuring output;
Screw speed: 100～150 rev/mins;
Feeding: normal pressure, low temperature and saturated feeding;
Screw rod barrel temperature: 20～25 ℃ of feeding sections;
30～70 ℃ of swelling sections;
80～95 ℃ of lysing segments;
93 ℃ of conveying and metering sections;
The time of staying of suspension in screw rod: about 4 minutes;
Screw rod head pressure: 〉=20 kilograms per centimeter
2
Adopt above-mentioned condition can make the uniform spinning solution of polyvinyl alcohol continuously, connect booster pump (8), filter (9), measuring pump and filament spinning component (10) [N=330f Φ=0.12mm] as outlet and can carry out continuous spinning at double screw extruder.Gained spinning solution strand (11) obtains polyvinyl alcohol gel spun fiber (13) through solidifying of coagulating basin (12), stores in containing silk tube (14).
Above-mentioned polyvinyl alcohol gel spun fiber can be made the vinal that intensity was 12.7 gram/dawn through extraction, drying and super drawing.
Embodiment 2:
With the same quadrat method of embodiment 1 make that the DP value is 2400, concentration is 20% uniform spinning solution and corresponding polyvinyl alcohol gel spun fiber.
With above-mentioned polyvinyl alcohol gel spun fiber extract, drying and super drawing can make the vinal that intensity was 13.5 gram/dawn.
Embodiment 3:
PVA, auxiliary agent and the solvent DMSO of DP value 1700 are added to the (PVA: DMSO=22: 78 w/w) of (3) the swelling still from charge door (1) (2) respectively.Open to stir and the interlayer heating, make in the still material temperature rise to T swelling=30～35 ℃, and be incubated 20 minutes, the swelling multiplying power of PVA is 110% this moment, at once the suspension of PVA is cooled to 20～25 ℃ subsequently, and homogeneous still (4) is interior standby in the middle of being transferred to.
Above-mentioned PVA suspension is put into feeding funnel (5), and keep the suspension liquid level to exceed 10 centimetres of double screw extruder (7) inlets.It is evenly mixed up and down that suspension in the funnel (5) adopts high speed agitator to carry out, and concentration is even up and down in feeding funnel (5) to keep suspension.The suspension that surpasses above-mentioned height overflows from the overfall of feeding funnel side, and is back to by circulating pump (6) and spares in the matter still (4).
PVA suspension carries out swelling, dissolving, deaeration and metering output in the end opening inflow double screw extruder (7) of feeding funnel (5), actual conditions is:
Double screw extruder type: parallel co-rotating twin screw extruder;
2 * 34 millimeters L/D=39 of Φ, 7 joint barrels add thermal control;
The screwing element of double screw extruder: the screwing element organic assembling of carrying, knead, sealing and measuring output;
Screw speed: 120 rev/mins;
Feeding: normal pressure, low temperature and saturated feeding;
Screw rod barrel temperature: 20 ℃ of feeding sections;
70 ℃ of swelling sections;
80 ℃ of lysing segments;
93 ℃ of conveying and metering sections;
The time of staying of suspension in screw rod: about 4 minutes;
Screw rod head pressure: 〉=20 kilograms per centimeter
2
Adopt above-mentioned condition can make the uniform spinning solution of polyvinyl alcohol continuously, connect booster pump (8), filter (9), measuring pump and filament spinning component (10) [N=330f Φ=0.12mm] as outlet and can carry out continuous spinning at double screw extruder.Gained spinning solution strand (11) obtains polyvinyl alcohol gel spun fiber (13) through solidifying of coagulating basin (12), stores in containing silk tube (14).
With above-mentioned polyvinyl alcohol gel spun fiber through extraction, drying and super drawing can make intensity be 12.7 the gram/and vinal.
Embodiment 4:
PVA, auxiliary agent and the solvent DMSO of DP value 2400 are added to the (PVA: DMSO=25: 75 w/w) of (3) the swelling still from charge door (1) (2) respectively.Open and stir and the interlayer heating, make and expect in the still that temperature rise is to T
Swelling=30～35 ℃, and be incubated 20 minutes, the swelling multiplying power of PVA is 110% this moment, at once the suspension of PVA is cooled to 20～25 ℃ subsequently, and standby in the homogeneous still (4) in the middle of being transferred to.
Above-mentioned PVA suspension is put into feeding funnel (5), and keep the suspension liquid level to exceed 10 centimetres of double screw extruder (7) inlets.It is evenly mixed up and down that suspension in the funnel (5) adopts high speed agitator to carry out, and concentration is even up and down in feeding funnel (5) to keep suspension.The suspension that surpasses above-mentioned height overflows from the overfall of feeding funnel side, and is back to by circulating pump (6) and spares in the matter still (4).
PVA suspension carries out swelling, dissolving, deaeration and metering output in the end opening inflow double screw extruder (7) of feeding funnel (5), actual conditions is:
Double screw extruder type: parallel co-rotating twin screw extruder;
2 * 34 millimeters L/D=39 of Φ, 7 joint barrels add thermal control;
The screwing element of double screw extruder: the screwing element organic assembling of carrying, knead, sealing and measuring output;
Screw speed: 150 rev/mins;
Feeding: normal pressure, low temperature and saturated feeding;
Screw rod barrel temperature: 30 ℃ of feeding sections;
80 ℃ of swelling sections;
120 ℃ of lysing segments;
125 ℃ of conveying and metering sections;
The time of staying of suspension in screw rod: about 4 minutes;
Screw rod head pressure: 〉=20 kilograms per centimeter
2
Adopt above-mentioned condition can make the uniform spinning solution of polyvinyl alcohol continuously, connect booster pump (8), filter (9), measuring pump and filament spinning component (10) [N=330f Φ=0.12mm] as outlet and can carry out continuous spinning at double screw extruder.Gained spinning solution strand (11) obtains polyvinyl alcohol gel spun fiber (13) through solidifying of coagulating basin (12), stores in containing silk tube (14).
Above-mentioned polyvinyl alcohol gel spun fiber can be made the vinal that intensity was 12.7 gram/dawn through extraction, drying and super drawing.
Reference examples 1:
The degree of polymerization and the corresponding concentration proportioning of the polyvinyl alcohol of enforcement 1,2, polyvinyl alcohol and solvent DMSO are added to simultaneously the population of double screw extruder, to polyvinyl alcohol carry out continuous-dissolution and spinning find to remove polyvinyl alcohol dissolve insufficient, the bubble of trace also appears existing in spinning solution and the polyethylene gel precursor, the spinnerets that via hole diameter is little, be easy to fracture of wire and after stretch, super drawing is difficult to carry out.
Claims (10)
1, a kind of continuous preparation method of polyvinyl alcohol uniform spinning solution, it is characterized in that adopting double screw extruder, polyvinyl alcohol is carried out pre-swelling in solvent, make the suspension of polyvinyl alcohol, the degree of polymerization of described polyvinyl alcohol is 1000～6000, and the concentration of polyvinyl alcohol in solution is 15～40Wt%, and the swelling time of polyvinyl alcohol in solvent is 10～20 minutes, temperature is 30～60 ℃, and the swelling multiplying power is 1.0～3.0.
2, the continuous preparation method of polyvinyl alcohol uniform spinning solution as claimed in claim 1, it is characterized in that adopting double screw extruder, polyvinyl alcohol is carried out pre-swelling in solvent, make the suspension of polyvinyl alcohol, the degree of polymerization of described polyvinyl alcohol is 1700～6000, and the concentration of polyvinyl alcohol in solution is 15～30Wt%, and the swelling time of polyvinyl alcohol in solvent is 10～20 minutes, temperature is 30～40 ℃, and the swelling multiplying power is 1.05～2.5.
3, the continuous preparation method of polyvinyl alcohol uniform spinning solution as claimed in claim 1 or 2, it is characterized in that described solvent is dimethyl formamide, dimethylacetylamide, dimethyl sulfoxide (DMSO), ethylene glycol and water, can use their mixture, also can use wherein a kind of separately.
4, the continuous preparation method of polyvinyl alcohol uniform spinning solution as claimed in claim 1 or 2, it is characterized in that under low temperature and atmospheric pressure state, with the saturated continuously feeding double screw extruder inlet of this suspension, the screwing element in the double screw extruder is formed by exporting, seal, knead and measure the multiple element of output.
5, the continuous preparation method of polyvinyl alcohol uniform spinning solution as claimed in claim 4, it is characterized in that each temperature of double screw extruder is set at: the feeding mouth temperature is T
Molten expandingBelow-10 ℃, middle proparea temperature is T
Molten expanding-10 ℃～T
Molten expanding+ 20 ℃, middle back zone temperature is T
Swelling-10 ℃～T
Dissolving+ 20 ℃, rear portion metering (outlet) temperature is T
Dissolving± 2 ℃, the screw speed of double screw extruder is 80～180 rev/mins, and suspension time of staying in double screw extruder is 3～10 minutes, and the head pressure of double screw extruder is 20 kilograms per centimeter
2More than.
6, the continuous preparation method of polyvinyl alcohol uniform spinning solution as claimed in claim 4, it is characterized in that the multi-section temperature of double screw extruder is set at: the feeding mouth temperature is below 20 ℃, middle proparea temperature is T
Swelling-T
Molten expanding+ 10 ℃, middle back zone temperature is T
Dissolving-T
Dissolving+ 10 ℃, rear portion metering (outlet) temperature is T
Dissolving± 2 ℃, the screw speed of double screw extruder is 80～180 rev/mins, and the time of staying of suspension in double screw extruder is 3～5 minutes, and the head pressure of double screw extruder is 20～40 kilograms of kilograms per centimeter
2
7, the continuous preparation method of polyvinyl alcohol uniform spinning solution as claimed in claim 1 or 2 is characterized in that at the double screw extruder inlet feeding funnel being set.
8, the continuous preparation method of polyvinyl alcohol uniform spinning solution as claimed in claim 7, the suspension that it is characterized in that polyvinyl alcohol is exported to the feeding funnel of double screw extruder continuously saturatedly, this suspension liquid level is higher than 5～20 centimetres of double screw extruder inlet faces, overhead clearance part suspension overflows from the flash mouth, returns the storage still of suspension.
9, the continuous preparation method of polyvinyl alcohol uniform spinning solution as claimed in claim 1 or 2 is characterized in that polyvinyl alcohol suspension finishes swelling, dissolving, deaeration and metering output in double screw extruder.
10, the continuous preparation method of polyvinyl alcohol uniform spinning solution as claimed in claim 1 or 2 is characterized in that the bubble of polyvinyl alcohol suspension in double screw extruder is to discharge from feeding mouth by the high pressure in screw rod.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00132182 CN1132971C (en) | 2000-12-20 | 2000-12-20 | Method for continuous preparation of polyvinyl alcohol uniform spinning solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00132182 CN1132971C (en) | 2000-12-20 | 2000-12-20 | Method for continuous preparation of polyvinyl alcohol uniform spinning solution |
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| Publication Number | Publication Date |
|---|---|
| CN1358886A CN1358886A (en) | 2002-07-17 |
| CN1132971C true CN1132971C (en) | 2003-12-31 |
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| CN 00132182 Expired - Fee Related CN1132971C (en) | 2000-12-20 | 2000-12-20 | Method for continuous preparation of polyvinyl alcohol uniform spinning solution |
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| EP1677964A1 (en) | 2003-10-29 | 2006-07-12 | Prysmian Cavi e Sistemi Energia S.r.l. | Process for manufacturing a water-resistant telecommunication cable |
| CN108977938A (en) * | 2018-06-05 | 2018-12-11 | 中国石油化工股份有限公司 | The method that sodium sulfocyanate method prepares polyacrylonitrile powder lot dispersing slurry |
| CN109680346B (en) * | 2018-12-08 | 2021-07-06 | 英鸿纳米科技股份有限公司 | Feeding mechanism of feeding robot for nanofiber production |
| CN113403694B (en) * | 2021-06-29 | 2022-08-12 | 东华大学 | Preparation method and application of PVA high-solid-content spinning solution |
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