CN104492126A - De-foaming device, de-foaming method and application of polyimide spinning solution - Google Patents
De-foaming device, de-foaming method and application of polyimide spinning solution Download PDFInfo
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- CN104492126A CN104492126A CN201410842262.2A CN201410842262A CN104492126A CN 104492126 A CN104492126 A CN 104492126A CN 201410842262 A CN201410842262 A CN 201410842262A CN 104492126 A CN104492126 A CN 104492126A
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Abstract
The invention provides a de-foaming device of a polyimide spinning solution. The de-foaming device comprises a de-foaming device body, an injection opening, a vacuum module and a discharging opening, and further comprises a flow distribution module, wherein the flow distribution module is used for dispersing and de-foaming a polyimide spinning raw solution injected into the de-foaming device body. The invention provides a de-foaming method of the polyimide spinning solution, in which the de-foaming device is adopted; the flow distribution module is arranged in the de-foaming device and is used for dispersing the polyimide spinning raw solution injected into the de-foaming device body to form a thin-film-shaped spinning solution layer, and foams in the polyimide spinning raw solution are easily ascended to the surface of the solution; the de-foaming effect is enhanced under a vacuum environment, the de-foaming time is shortened and the de-foaming efficiency is improved, so that the continuous production of polymerization reaction before the de-foaming and a spinning phase after de-foaming can be realized, and the stability of fiber performances is guaranteed; and the de-foaming device is simple to operate and low in cost.
Description
Technical field
The invention belongs to the preparing technical field of high-performance fiber, specifically relate to a kind of defoaming device of polyimides spinning solution, defoaming method and application thereof.
Background technology
Polyimide fiber is a kind of high strength, high-modulus and have the high-performance fiber of polyimide material characteristic property.According to theory calculate, the modulus of the fiber synthesized by equal benzene dianhydride and p-phenylenediamine (PPD) can reach 410GPa, is only second to carbon fiber, and has very high heat endurance.Wherein, the decomposition temperature of full aromatic polyimide fiber can reach 500 DEG C, and can be used for supersonic speed aerospace field, it also has very high radioresistance and resistance to low temperature etc., and become one of material of Aero-Space first-selection, be also used as the filtering material of high-temperature medium and penetrating property material.
The preparation method of current polyimide fiber has wet spinning or dry-jet wet-spinning, and these two kinds of methods all can adopt single step spining or two step method spinning further, and in order to keep the features such as high temperature resistant, the solvent resistant of polyimide fiber, it is more extensive that two step method spins application.The method is that the polyimides acid solution that polymerisation obtains by the first step carries out spinning, obtain polyamic acid fiber, the polyimide fiber that second step polyamic acid fiber obtains through chemical imidization or thermal cyclization, the drawing of fiber is stretched can in the first step or/and carry out in second step.
And in the process of producing polyimide fiber, one of most basic factor of precursor quality depends on the deaeration effect of spinning solution.The quality of deaeration effect directly determines whether the technical process such as later stage spinning, drying, drawing-off can carry out smoothly.Can bubble be there is in spinning solution in polymerization or course of conveying, larger bubble can cause the interruption, deformation, broken end etc. of dynamic analysis of spinning by spinneret orifice, less bubble can residually by spinneret orifice cause fiber porose in the fibre, and when drawing-off, easy fracture forms lousiness, fracture of wire.When deaeration is insufficient, the drafting multiple of precursor can not improve, and does not reach due fiber number, intensity and elongation at break, finally affects the intensity of finished product precursor and polyimide fiber.So, the bubble in spinning solution thoroughly must be deviate from before spinning.But because the viscosity of spinning solution is large, bubble is deviate to acquire a certain degree of difficulty.
Polyimides acid solution many employings batch (-type) that first step polymerisation in above-mentioned two step method obtains leaves standstill vacuum defoamation method or batch (-type) and leaves standstill normal pressure defoaming method and reach desirable wet spinning condition to make solution deaeration.It is vacuumize after polyimides acid solution being loaded several special deaeration stills to leave standstill or normal pressure leaves standstill that batch (-type) leaves standstill vacuum defoamation method or normal pressure defoaming method, the time left standstill is determined according to the polyimides acid solution amount of proceeding to, make the deaeration of solution nature, the polyimides acid solution dynamic viscosity fluctuation range obtained due to polymerisation in the method is larger, the time of standing and defoaming is difficult to grasp and time of repose is oversize, increase the risk of the polyimides acid solution auto-degradation of polymerization, equipment needs drop into multiple deaeration still, cost is higher, cannot continous way produce in polymerisation and spinning phase, the stability of fibre property also cannot be protected.
Summary of the invention
The object of the invention is to the above-mentioned deficiency overcoming prior art, provide a kind of and improve the defoaming device that deaeration efficiency, structure are simple, be easy to the polyimides spinning solution operated.
Another object of the present invention is to provide a kind of simple to operate, cost is low, efficiency is high and the defoaming method of the polyimides spinning solution that fiber quality is stable.
Another object of the present invention is to provide a kind of application process adopting the polyimides spinning solution after above-mentioned defoaming method process.
In order to realize foregoing invention object, technical scheme of the present invention is as follows:
A kind of defoaming device of polyimides spinning solution, comprise: defoaming device body, inlet, vacuum module, outlet, this defoaming device also comprises diverter module, and this diverter module is used for injecting defoaming device intrinsic polyimides spinning solution dispersion deaeration.
And the defoaming method of above-mentioned polyimides spinning solution, comprises the steps:
Obtain polyimides spinning solution;
Above-mentioned polyimides spinning solution is injected in above-mentioned defoaming device body by above-mentioned inlet; Start the vacuum module in defoaming device, arranging vacuum is 50kPa ~ 100kPa;
Above-mentioned polyimides spinning solution, through above-mentioned diverter module dispersion flows, forms the spinning liquid layer of film-form, completes vacuum defoamation;
Obtain spinnable polyimides spinning solution.
And the application process of polyimides spinning solution, adopt the polyimides spinning solution that above-mentioned defoaming device and method obtain, spinning, solidifies, washing, dry, oils, then carries out hot-imide process, obtain polyimide acid fiber.
The defoaming device of polyimide fiber spinning solution provided by the present invention and method, by arranging diverter module in defoaming device, this diverter module will inject the intrinsic polyimides spinning solution dispersion of defoaming device, form the spinning liquid layer of film-form, the bubble in polyimide fiber spinning solution is made to be easy to rise to the surface of solution, strengthen the effect of deaeration under vacuum conditions, shorten inclined heated plate, improve deaeration efficiency, thus make the spinning phase after the polymerisation before deaeration and deaeration can realize continous way production, ensure that the stability of fibre property, and this defoaming device is simple to operate, cost is low.Above-mentioned continous way defoaming method can be equally applicable to the deaeration of the contour performance fibers of aramid fiber, wide adaptability.
Accompanying drawing explanation
Fig. 1 is the structural representation of polyimides spinning solution defoaming device in the embodiment of the present invention;
Fig. 2 is the schematic flow sheet of polyimides spinning solution defoaming method in the embodiment of the present invention.
Detailed description of the invention
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment and accompanying drawing, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiments provide and a kind ofly improve the defoaming device that deaeration efficiency, structure are simple, be easy to the polyimides spinning solution operated, as shown in Figure 1, comprise: defoaming device body, inlet 1, vacuum module, outlet 5, this defoaming device also comprises diverter module 2, and this diverter module is used for injecting defoaming device intrinsic polyimides spinning solution dispersion deaeration.
Particularly, above-mentioned defoaming device is preferably continuous vacuum defoaming device.Above-mentioned inlet 1 is positioned at the top of defoaming device body, and the number of this inlet 1 is more than or equal to 2, can be but be not limited to 3,5,7,9, be preferably 3; And this inlet 1 is preferably placed at the center of defoaming device bodies top.In a preferred embodiment of the invention, the number of inlet 1 is 3, and one of them inlet 1 is positioned at the center of defoaming device bodies top, is connected with injection pump, for receiving the polyimides spinning solution injecting non-deaeration process; Two other is symmetrically distributed in the peripheral position of defoaming device bodies top centered by it.Wherein, any one inlet 1 being positioned at peripheral position is connected with outer circulation module 6, for receiving the polyimides spinning solution injecting the deaeration less effective that outer circulation module 6 refluxes; Another the inlet 1 that be positioned at peripheral position symmetrical with it is connected with injection pump, for receiving the polyimides spinning solution injecting non-deaeration process.
Further, defoaming device also comprises injection pump and injection rate adjusting device.This injection pump is preferably gear pump, is connected with above-mentioned inlet 1, for pumping into polyimides spinning solution; This injection rate adjusting device is different according to the viscosity of polyimides spinning solution, the amount of pumping into of polyimides spinning solution is regulated, avoid affecting production efficiency very little because pumping into polyimides spinning solution, or affect deaeration effect too much because pumping into polyimides spinning solution.
Particularly, above-mentioned diverter module 2 is arranged at the intrinsic top of defoaming device, this diverter module 2 is cone mechanism, can be conical mechanism, vertical cone mechanism, the area of its bottom surface is less than the cross-sectional area of above-mentioned defoaming device, the madial wall of this bottom surface and defoaming device, at a distance of 5 ~ 10cm, is preferably at a distance of 5cm.In a preferred embodiment of the invention, this diverter module 2 preferred conical mechanism, the center inlet 1 that its summit is positioned at defoaming device bodies top near above-mentioned, its bottom surface are near outlet 5.When polyimides spinning solution is entered in defoaming device body by inlet 1 reception, under the drainage of above-mentioned tapered shunting module 2, side outer wall along diverter module 2 flows downward under gravity and forms the spinning liquid layer of film-form, should will break rapidly at the environment lower part bubble of vacuum by the spinning liquid layer in film-form, and part bubble rises to liquid surface and breaks rapidly.Observe the form of polyimide fiber spinning solution, if deaeration effect is more satisfactory, directly can shift, carry out spinning.
Particularly, the defoaming device of the embodiment of the present invention also comprises stone roller bubble module 3, and this stone roller bubble module 3 is preferably screw pump, is positioned at the intrinsic bottom of defoaming device, for extruding the bubble pulverized in above-mentioned polyimides spinning solution.
Particularly, the defoaming device of the embodiment of the present invention also comprises outer circulation module 6, outer circulation starts module 7, the first end of this outer circulation module 6 is connected with above-mentioned outlet 5, second end of outer circulation module 6 is connected with above-mentioned inlet 1, and outer circulation starts the first end that module 7 is arranged at outer circulation module 6.When above-mentioned film vacuum deaeration with after grinding bubble deaeration process, when also there is bubble in polyimides spinning solution, start module 7 by opening outer circulation, the polyimides spinning solution by outlet 5 is back to above-mentioned inlet 1 by outer circulation module 6; Re-start deaeration process.
Particularly, above-mentioned vacuum module is preferably water ring vacuum pump.
The defoaming device of the polyimide fiber spinning solution that the embodiment of the present invention provides, by arranging diverter module in defoaming device, grind bubble module, outer circulation module, this diverter module will inject the intrinsic polyimides spinning solution dispersion of defoaming device, form the spinning liquid layer of film-form, make the bubble in polyimide fiber spinning solution be easy to rise to the surface of solution, strengthen the effect of deaeration under vacuum conditions; And Combined Mining is with grinding bubble module and outer circulation module reinforcement deaeration rate, ensure the quality of polyimide fiber spinning solution, shorten inclined heated plate, improve deaeration efficiency, thus make the spinning phase after the polymerisation before deaeration and deaeration can realize continous way production, ensure that the stability of fibre property; And this defoaming device is simple to operate, cost is low.
The embodiment of the present invention additionally provides a kind of defoaming method of polyimides spinning solution, and its schematic flow sheet as shown in Figure 2, comprises the steps:
S01, obtains polyimides spinning solution; Particularly, the viscosity of this polyimides spinning solution is 5 ~ 20Pa.s, is preferably 10Pa.s;
S02, injects in above-mentioned defoaming device body by above-mentioned polyimides spinning solution by above-mentioned inlet; Start the vacuum module in defoaming device, arranging vacuum is 50kPa ~ 100kPa;
S03, above-mentioned polyimides spinning solution, through above-mentioned diverter module dispersion flows, forms the spinning liquid layer of film-form, completes vacuum defoamation;
S04, obtains spinnable polyimides spinning solution.
Particularly, the method obtaining polyimides spinning solution is as follows:
S011, by the monomer of binary acid anhydride and diamine synthesis of polyimides;
S012, the polyimide monomers obtained by step S011 carries out low housewarming bunching in the aprotonic polar solution such as dimethyl formamide (DMF), dimethylacetylamide (DMAC), N-methyl pyrrole network alkane ketone (NMP), obtains the sub-acid solution of intermediate polyamides;
S013, the sub-acid solution of the intermediate polyamides obtained by step S012 is heated to about 300 DEG C, and intramolecular dehydration closed loop obtains polyimides spinning solution; Or, by intermediate polyamic acid solution cyclodehydration under dehydrating agent effect, obtain polyimides spinning solution, and then calorify isomerization under acid or alkali condition, obtain polyimides spinning solution.
Particularly, in above-mentioned steps S02, the charge velocity of above-mentioned polyimides spinning solution is regulated to be 50cm by injection rate adjusting device
3/ s ~ 100cm
3/ s, is preferably 100cm
3/ s; This preferred charge velocity coordinates the polyimides spinning solution of above-mentioned preferred viscosities, and avoiding affects production efficiency very little because pumping into polyimides spinning solution, or affects deaeration effect too much because pumping into polyimides spinning solution.
Further, in above-mentioned steps S02, vacuum is preferably set to 100kPa, polyimides spinning solution in step S03 is under the drainage of above-mentioned tapered shunting module 2, side outer wall along diverter module 2 flows downward under gravity and forms the spinning liquid layer of film-form, should will break rapidly at this preferred vacuum environment lower part bubble by the spinning liquid layer in film-form, and part bubble rises to liquid surface and breaks rapidly.
Further, between above-mentioned steps S03 and step S04, also comprise and grind bubble step: after vacuum defoamation process, also there is bubble when above-mentioned in polyimides spinning solution, start above-mentioned stone roller bubble module 3, the bubble remained is pulverized in extruding.
Further, between above-mentioned steps S03 and step S04, also comprising and grind outer circulation reflow step: also there is bubble through grinding after bubble process in polyimides spinning solution when above-mentioned, start above-mentioned outer circulation and start module 7, make to be drawn by the polyimides spinning solution of outlet 5 to be back to above-mentioned inlet 1 by outer circulation module 6; Re-start vacuum defoamation process.
The defoaming method of the polyimide fiber spinning solution that the embodiment of the present invention provides, by forming the spinning liquid layer of film-form, making the bubble in polyimide fiber spinning solution be easy to rise to the surface of solution, strengthening the effect of deaeration under vacuum conditions; And Combined Mining, with grinding bubble step and outer circulation reflow step, strengthens deaeration rate, ensures the quality of polyimide fiber spinning solution, shortens inclined heated plate, improves deaeration efficiency,
Embodiments provide the application process of the polyimides spinning solution of said apparatus and method acquisition, by the polyimides spinning solution obtained, spinning, solidifies, and washing is dry, oils, then carries out hot-imide process, obtain polyimide acid fiber;
Or, by the polyimides spinning solution obtained, be extruded into silk via spinneret orifice, namely carry out wet spinning, obtain polyimide acid fiber.
Now in conjunction with instantiation, the defoaming method of embodiment of the present invention polyimides spinning solution and device thereof are further elaborated:
Embodiment 1
S11, obtaining viscosity is 200,000 Pa.s (centipoise) polyimides spinning solution;
S12, injects in above-mentioned defoaming device body by above-mentioned polyimides spinning solution by the inlet of continuous vacuum deaeration still; Start the vacuum module in defoaming device, arranging vacuum is 100kPa;
S13, above-mentioned polyimides spinning solution, through above-mentioned diverter module dispersion flows, forms the spinning liquid layer of film-form, completes vacuum defoamation;
S14, obtains spinnable polyimides spinning solution;
S15, proceeds to filament spinning component and carries out wet spinning, obtains the polyimide acid fiber that fiber number is 90tex;
S16, solidify through one or two road coagulating baths, by washing, dry, spinning speed according to 10m/min after oiling enters tension-adjusting gear, imported in imidizate processor by fiber, process stage by stage, one-phase hot-imide temperature is 250 DEG C, two-stage is 300 DEG C, three stages were 350 DEG C, and four stages were 400 DEG C, and the processing time is constant according to technological requirement respectively;
S17, becomes cylinder to receive silk at receipts silk machine place.
Three increment product of getting detect, and testing result is as shown in table 1 below:
Table 1
Embodiment 2
S21, obtaining viscosity is 100,000 Pa.s (centipoise) polyimides spinning solution;
S22, injects in above-mentioned defoaming device body by above-mentioned polyimides spinning solution by the inlet of continuous vacuum deaeration still; Start the vacuum module in defoaming device, arranging vacuum is 100kPa;
S23, above-mentioned polyimides spinning solution, through above-mentioned diverter module dispersion flows, forms the spinning liquid layer of film-form, completes vacuum defoamation;
S24, obtains spinnable polyimides spinning solution;
S25, proceeds to filament spinning component and carries out wet spinning, obtains the polyimide acid fiber that fiber number is 90tex;
S26, solidify through one or two road coagulating baths, by washing, dry, spinning speed according to 10m/min after oiling enters tension-adjusting gear, imported in imidizate processor by fiber, process stage by stage, one-phase hot-imide temperature is 250 DEG C, two-stage is 300 DEG C, three stages were 350 DEG C, and four stages were 400 DEG C, and the processing time is constant according to technological requirement respectively;
S27, becomes cylinder to receive silk at receipts silk machine place.
Three increment product of getting detect, and testing result is as shown in table 2 below:
Table 2
Embodiment 3
S31, obtaining viscosity is 50,000 Pa.s (centipoise) polyimides spinning solution;
S32, injects in above-mentioned defoaming device body by above-mentioned polyimides spinning solution by the inlet of continuous vacuum deaeration still; Start the vacuum module in defoaming device, arranging vacuum is 100kPa;
S33, above-mentioned polyimides spinning solution, through above-mentioned diverter module dispersion flows, forms the spinning liquid layer of film-form, completes vacuum defoamation;
S34, obtains spinnable polyimides spinning solution;
S35, proceeds to filament spinning component and carries out wet spinning, obtains the polyimide acid fiber that fiber number is 90tex;
S36, solidify through one or two road coagulating baths, by washing, dry, spinning speed according to 10m/min after oiling enters tension-adjusting gear, imported in imidizate processor by fiber, process stage by stage, one-phase hot-imide temperature is 250 DEG C, two-stage is 300 DEG C, three stages were 350 DEG C, and four stages were 400 DEG C, and the processing time is constant according to technological requirement respectively;
S37, becomes cylinder to receive silk at receipts silk machine place.
Three increment product of getting detect, and testing result is as shown in table 3 below:
Table 3
The testing result display of above embodiment, adopt the polyimides spinning solution that the polyimide fiber defoaming device of the embodiment of the present invention and method obtain, comparatively intermittent vacuum standing and defoaming method and batch (-type) normal pressure standing and defoaming method technique simpler, more convenient operation, cost is lower, and fibrous finished product qualification rate is higher, stable performance, the development for current high-performance fiber manufacturing has great importance.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the defoaming device of a polyimides spinning solution, comprise: defoaming device body, inlet, vacuum module, outlet, it is characterized in that, described defoaming device also comprises diverter module, and described diverter module is used for injecting described defoaming device intrinsic polyimides spinning solution dispersion deaeration.
2. the defoaming device of polyimides spinning solution as claimed in claim 1, it is characterized in that, described diverter module is arranged at the intrinsic top of described defoaming device, described diverter module is summit near inlet, bottom surface near the cone mechanism of outlet, and described base area is less than the cross-sectional area of described defoaming device.
3. the defoaming device of polyimides spinning solution as claimed in claim 1, is characterized in that, the bottom surface of described cone mechanism and the sidewall of described defoaming device are at a distance of 5 ~ 10cm.
4. the defoaming device of the polyimides spinning solution as described in any one of claims 1 to 3, is characterized in that, described defoaming device also comprises stone roller bubble module, and described stone roller bubble module is for grinding brokenly bubble in described polyimides spinning solution.
5. the defoaming device of the polyimides spinning solution as described in any one of claims 1 to 3, it is characterized in that, described defoaming device also comprises outer circulation module, outer circulation starts module, the first end of described outer circulation module is connected with described outlet, and the second end of described outer circulation module is connected with described inlet; Described outer circulation starts module installation in the first end of described outer circulation module.
6. the defoaming device of the polyimides spinning solution as described in any one of claims 1 to 3, is characterized in that, described defoaming device also comprises injection pump and injection rate adjusting device.
7. a defoaming method for polyimides spinning solution, comprises the steps:
Obtain polyimides spinning solution;
Described polyimides spinning solution is injected in described defoaming device body by described inlet; Start the vacuum module in defoaming device, arranging vacuum is 50kPa ~ 100kPa;
Described polyimides spinning solution, through described diverter module dispersion flows, forms the spinning liquid layer of film-form, completes vacuum defoamation;
Obtain spinnable polyimides spinning solution.
8. the defoaming method of polyimides spinning solution as claimed in claim 7, it is characterized in that, described film-form spinning solution layer thickness is 0.1mm ~ 2mm.
9. the defoaming method of polyimides spinning solution as claimed in claim 7, it is characterized in that, the charge velocity of described polyimides spinning solution is 50cm
3/ s ~ 100cm
3/ s.
10. the application process of a polyimides spinning solution, adopt the polyimides spinning solution that the defoaming device described in any one of claim 1 ~ 6 and the defoaming method described in any one of claim 7 ~ 9 obtain, spinning, solidify, washing, dry, oil, then carry out hot-imide process, obtain polyimide acid fiber.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108339295A (en) * | 2017-01-25 | 2018-07-31 | 京东方科技集团股份有限公司 | Defoaming device and method |
| CN108588873A (en) * | 2018-03-23 | 2018-09-28 | 海盐海利环保纤维有限公司 | A kind of manifold defoaming device and bubble removing method for producing regenerated fiber |
| CN109537066A (en) * | 2018-12-19 | 2019-03-29 | 四川辉腾科技股份有限公司 | A kind of defoaming device and defoaming method for aramid IIII fiber spinning solution |
| CN113617064A (en) * | 2020-05-09 | 2021-11-09 | 中国石油化工股份有限公司 | Continuous defoaming device for high-viscosity fluid, application of continuous defoaming device and defoaming method for polyamide acid spinning solution |
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2014
- 2014-12-30 CN CN201410842262.2A patent/CN104492126A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108339295A (en) * | 2017-01-25 | 2018-07-31 | 京东方科技集团股份有限公司 | Defoaming device and method |
| WO2018137342A1 (en) * | 2017-01-25 | 2018-08-02 | Boe Technology Group Co., Ltd. | Defoaming device and method |
| CN108339295B (en) * | 2017-01-25 | 2019-10-25 | 京东方科技集团股份有限公司 | Defoaming device and method |
| US10744423B2 (en) | 2017-01-25 | 2020-08-18 | Boe Technology Group Co., Ltd. | Defoaming device and method |
| CN108588873A (en) * | 2018-03-23 | 2018-09-28 | 海盐海利环保纤维有限公司 | A kind of manifold defoaming device and bubble removing method for producing regenerated fiber |
| CN109537066A (en) * | 2018-12-19 | 2019-03-29 | 四川辉腾科技股份有限公司 | A kind of defoaming device and defoaming method for aramid IIII fiber spinning solution |
| CN113617064A (en) * | 2020-05-09 | 2021-11-09 | 中国石油化工股份有限公司 | Continuous defoaming device for high-viscosity fluid, application of continuous defoaming device and defoaming method for polyamide acid spinning solution |
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