CN105597580A - Solidification liquid preparation apparatus, solidification liquid preparation method, and applications of solidification liquid preparation apparatus - Google Patents
Solidification liquid preparation apparatus, solidification liquid preparation method, and applications of solidification liquid preparation apparatus Download PDFInfo
- Publication number
- CN105597580A CN105597580A CN201410582251.5A CN201410582251A CN105597580A CN 105597580 A CN105597580 A CN 105597580A CN 201410582251 A CN201410582251 A CN 201410582251A CN 105597580 A CN105597580 A CN 105597580A
- Authority
- CN
- China
- Prior art keywords
- solidification liquid
- pipeline
- storage tank
- solidification
- circulation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a solidification liquid preparation apparatus, a solidification liquid preparation method, and applications of the solidification liquid preparation apparatus. A purpose of the present invention is mainly to solve the problems of high deviation between the actual concentration and the theoretical concentration and poor solidification liquid stability of the prepared solidification liquid in the prior art. According to the present invention, the circulation apparatus of the solidification liquid is used, and comprises a purging system, a preparation system, an automatic water supplementing system, a self-circulation system and an outer circulation system, wherein the self-circulation system comprises a flow meter, a circulation pump, a pump out pipeline, a circulation pipeline, a reflux pipeline, a venturi jet pipe and a solidification liquid storage tank, the outer circulation system comprises a circulation pump, a pump out pipeline, a circulation pipeline, a solidification liquid input pipeline, a solidification bath tank, a solidification liquid output pipeline, a venturi jet pipe and a solidification liquid storage tank, and the self-circulation system and the outer circulation system can respectively and separately work. With the technical scheme of the present invention, the problems in the prior art are well solved. The preparation apparatus of the present invention can be used for the spinning process of the polyacrylonitrile-based carbon fiber protofilaments.
Description
Technical field
The present invention relates to a kind of device for formulating and compound method and application of solidification liquid, is a kind of compound method of producing the dimethyl sulfoxide (DMSO)/aqueous solution of polyacrylonitrile fibril for wet spinning specifically.
Background technology
Dimethyl sulfoxide (DMSO) (DimethylSulfoxide), as the solvent of a kind of important industrial chemicals and function admirable, has good dissolution to polymer, a large amount of spinning stages for carbon fiber production process. Dimethyl sulfoxide (DMSO) taste is slightly bitter, no color or smell, and toxicity is low, and has stronger molecular association, is a kind of very important aprotic polar solvent. The stable chemical nature of dimethyl sulfoxide (DMSO), can stable existence under acidity, alkalescence or neutrallty condition at 100 DEG C. But under constant-pressure and high-temperature, can cause it to decompose, generate micro-aldehyde, thioether and mercaptan, and have strong unhappy smell. Dimethyl sulfoxide (DMSO) is alkalescent, under acid condition, thereby owing to forming hydrogen bond in conjunction with salify with acid, can promote the decomposition of dimethyl sulphoxide solution. And under alkali condition, can slow down the decomposition rate of dimethyl sulfoxide (DMSO).
PAN base carbon fibre is a kind of artificial synthetic inorfil. It is by acrylonitrile and comonomer, the fibrous polymer obtaining after the series of process such as polymerization, spinning, pre-oxidation and carbonization are processed. In spinning process mainly there is physical change in PAN molecule, forms the fibrous precursor of white, and in preoxidation process, PAN precursor develops into that certain is heat-resisting containing oxide structure gradually, after carbonization, obtains the high carbon fiber of phosphorus content. There is the performances such as high specific strength, high ratio modulus, high temperature resistant and resistance to chemical attack due to carbon fiber, therefore its application and extensively.
The preparation of polyacrylonitrile fibril relates to the preparation of stoste and two large processes of the spinning of stoste, wherein the preparation of stoste comprises polymerization, de-single and deaeration three road procedures, the spinning of stoste comprises the filtration of stoste, measures, solidifies, hot water drawing-off, wash, oil, tens procedures such as compacting by drying, steam drafting, thermal finalization and coiling. Solidify fibre forming extremely important, it be by stoste thread to as-spun fibre change committed step. Stoste thread enters in solidification liquid (dimethyl sulfoxide (DMSO)/aqueous solution), and because the dimethyl sulfoxide (DMSO) concentration ratio solidification liquid in stoste thread is high, the dimethyl sulfoxide (DMSO) in stoste thread outwards diffuses in solidification liquid; Because the water concentration in stoste thread is lower than solidification liquid, the water in solidification liquid inwardly diffuses in stoste thread again. Double diffusion effect is separated the polymer in stoste thread, forms as-spun fibre.
Stoste thread generation double diffusion, forms as-spun fibre after being separated, and this process is carried out in solidification liquid. The concentration of solidification liquid and temperature can affect double diffused speed, further affect the morphosis of as-spun fibre. Improve the concentration of solidification liquid, or reduce the temperature of solidification liquid, all can slow down the speed of double diffusion process, be conducive to like this as-spun fibre and form fine and close structure, thereby improve the mechanical property of final precursor. Improve the concentration of solidification liquid, or improve the temperature of solidification liquid, the cross section that is all conducive to as-spun fibre changes to circle.
The syntheti c route of polyacrylonitrile base carbon fiber precursors, adopts different foundations, has different sorting techniques. The solvent difference using according to spinning, can be divided into dimethyl sulfoxide method, sodium thiocyanate water solution method, nitrate method etc., according to the difference of former wire forming process, can be divided into wet method and the dry method that squirts. The polyacrylonitrile fibril that adopts at present dimethyl sulfoxide (DMSO) to produce as the wet spinning technology of solvent accounts for the overwhelming majority of output. The solidification liquid that conventional wet spinning is used, because amount of preparation is large, operates extensive, mix acutely, and the defect of equipment design aspect, therefore cause the actual concentrations of solidification liquid often low than theoretical calculating concentration, and solidification liquid muddiness, surface has the analyte of a little similar greasy dirt floating.
Patent CN201210160024 discloses a kind of polyacrylonitrile-based precursor coagulating bath solution and preparation method and application, a kind of polyacrylonitrile-based precursor coagulating bath solution is made up of dimethyl sulfoxide (DMSO), water and the 3rd component, it consists of: dimethyl sulfoxide (DMSO) and water are dimethyl sulfoxide (DMSO) by volume: water=(120-230): the content of 100, the three components in dimethyl sulphoxide aqueous solution is 0.02mol/L～0.08mol/L. Employing is prepared as follows method by dimethyl sulfoxide (DMSO) and water dimethyl sulfoxide (DMSO) by volume: water is (120-230): 100 mix, and mixes in 45～60 DEG C, obtains dimethyl sulphoxide aqueous solution; In dimethyl sulphoxide aqueous solution, add the 3rd component, the content of the 3rd component in dimethyl sulphoxide aqueous solution is 0.02mol/L～0.08mol/L, mixes and obtains polyacrylonitrile-based precursor coagulating bath solution. Still there is amount of preparation large, operate extensively, mix violent defect, cause the actual concentrations of solidification liquid often low than theoretical calculating concentration, and solidification liquid muddiness, surface has the analyte of a little similar greasy dirt floating.
Summary of the invention
One of technical problem to be solved by this invention is the actual concentrations of the solidification liquid preparation that exists in prior art and theoretical concentration deviation is large, the problem of solidification liquid poor stability. A kind of EGR of preparing solidification liquid is provided, and this device has for preparing solidification liquid the accuracy that improves preparation solidification liquid concentration, suppresses the advantage of dimethyl sulfoxide (DMSO) thermal decomposition.
Two of technical problem to be solved by this invention is to provide a kind of compound method of the solidification liquid of applying one of technical solution problem described EGR.
The application of the EGR that three of technical problem to be solved by this invention is to provide the described solidification liquid of one of a kind of technical solution problem in spinning technique.
For one of solving the problems of the technologies described above, the technical solution adopted in the present invention is as follows: a kind of EGR of solidification liquid, comprising: purging system, compounding system, self-circulation system; Wherein, described self-circulation system comprises flowmeter (21), circulating pump (7,7'), pump pipeline (11), circulation line (12), return line (13), venturi jet pipe (6) and solidification liquid storage tank (9), in described circulation line, connect at least two heat exchangers (4,4'); When the work of described self-circulation system, circulating pump pumps the liquid in solidification liquid storage tank through pumping pipeline, circulation line, return line, venturi jet pipe and turns back in solidification liquid storage tank; Described purging system through scavenging pipeline purge circulation line (16) for purge circulation line and solidification liquid intake line; Described compounding system is inputted solidification liquid storage tank through preparation pipeline (9) for preparing material.
In technique scheme, in described circulation line, be preferably connected with filter 3.
In technique scheme, for spinning technique, also preferably include external circulating system, described external circulating system preferably includes flowmeter (21), circulating pump (7,7'), pumps pipeline (11), circulation line (12), solidification liquid intake line (14), coagulating tank (8), solidification liquid output pipe (15), venturi jet pipe (6) and solidification liquid storage tank (9); When described external circulating system work, circulating pump pumps the liquid in solidification liquid storage tank through pumping pipeline, circulation line, solidification liquid intake line solidification liquid is input in coagulating tank, and the solidification liquid that coagulating tank overflows returns in solidification liquid storage tank through solidification liquid output pipe, venturi jet pipe.
In technique scheme, in described solidification liquid intake line, be preferably connected with flow measurement device, more preferably flowmeter 5 and flowmeter 5'.
In technique scheme, in order to keep solidification liquid to have constant concentration in spinning process, described external circulating system also preferably includes to the automatic water-replenishing device 1 of moisturizing in the solidification liquid overflowing in coagulating tank; Concrete setting and moisturizing speed thereof can be selected according to general knowledge known in this field by those skilled in the art; In described solidification liquid output pipe, be preferably connected with static mixer 2; Moisturizing and the solidification liquid overflowing enter solidification liquid storage tank 9 after static mixer 2 mixes.
In technique scheme, described solidification liquid output pipe puts in pipeline in solidification liquid storage tank and is substantially positioned at the axial centre of storage tank; The lower edge of pipeline is less than 20 centimetres to the distance of tank bottom, more preferably 5～15 centimetres.
In technique scheme, in described circulation line, be provided with spare duct 18, spare duct 19; In case for subsequent use.
In technique scheme, described purging system preferably uses dry gas to purge, and more preferably drying nitrogen or dry air, makes to exist without moisture in purged pipeline.
In technique scheme, described solidification liquid is preferably the aqueous solution of dimethyl sulfoxide (DMSO).
For solve the problems of the technologies described above two, the technical solution used in the present invention is: a kind of compound method of solidification liquid, adopt the EGR of arbitrary described solidification liquid in technique scheme, comprise the following steps:
(a) first clean solidification liquid storage tank, circulating pump, circulation line, venturi jet pipe; After cleaning completes, water emptying is removed;
(b) use dry gas purge circulation line, make its inside not leave water;
(c) use preparation pipeline, in solidification liquid storage tank, inject the water through the required weight of preparation solidification liquid of metering by mass flowmenter;
(d) open circulating pump, regulate the flow of certain glass rotameter to start circulation, and heat exchanger is set, the temperature of controlling the solidification liquid of self-loopa is less than 40 DEG C;
(e) use preparation pipeline, in solidification liquid storage tank, inject dimethyl sulfoxide (DMSO) and the 3rd component through the required weight of preparation solidification liquid of metering by mass flowmenter, join in solidification liquid storage tank with certain flow, this flow be less than circulating pump circular flow 1/3rd;
(f) circulating pump stops after remaining in operation and being not less than 10 minutes; In the time that solidification liquid reaches predetermined concentration, the solidification liquid that obtains desired concn is for subsequent use.
In technique scheme, in the process of described preparation solidification liquid, be preferably 25～35 DEG C by the temperature of heat exchanger control solidification liquid self-loopa.
In technique scheme, in the process of described configuration solidification liquid, add the flow of dimethyl sulfoxide (DMSO) to be less than 1/3rd of self-loopa flow; It is described that to add the flow of dimethyl sulfoxide (DMSO) and the ratio optimization of self-loopa flow be 1:3～1:7.
In technique scheme, in step (f), described circulating pump time of carrying out self-loopa of remaining in operation is preferably 15～20 minutes.
For solve the problems of the technologies described above three, the technical solution used in the present invention is as follows: the application of the EGR of arbitrary described solidification liquid in spinning technique in a kind of technique scheme.
In technique scheme, adopt technical solution problem two described in compound method obtain after the solidification liquid in described step (f), open outer circulation and can carry out spinning technique.
Adopt the solution of the present invention, can improve the accuracy of preparation solidification liquid concentration, effectively suppress the thermal decomposition of dimethyl sulfoxide (DMSO), feed intake concentration and the actual concentrations difference of dimethyl sulphoxide aqueous solution are less than 0.5%, the solidification liquid preparing is transparent, good technique effect, without obvious similar greasy dirt floating thing, has been obtained in surface.
Brief description of the drawings
Fig. 1 is a kind of schematic diagram of inking device of solidification liquid.
In Fig. 1,1 is automatic water replenishing system, and 2 is static mixer, and 3 is filter, 4 and 4 ' is heat exchanger, and 21,5 and 5 ' is flowmeter, and 6 is venturi jet pipe, 7 and 7 ' is circulating pump, and 8 is coagulating tank, and 9 is coagulating bath storage tank, and 10～17 are respectively the pipeline of connection device.
Fig. 2 is the schematic diagram of the inking device to the further improved solidification liquid of the present invention.
In Fig. 2,1 is automatic water replenishing system, and 2 is static mixer, and 3 is filter, 4 and 4 ' is heat exchanger, and 5 and 5 ' is flowmeter, and 6 is venturi jet pipe, and 7 and 7 ' is circulating pump, 10～17 are respectively the pipeline of connection device, and 18 and 19 are the spare duct in circulation line, and 21 is flowmeter.
Further illustrate below by specific embodiment.
Detailed description of the invention
[embodiment 1]
The water of draining in filter and heat exchanger; Use dry air to purge heat exchanger, filter and part self-loopa pipeline, make its inside not leave moisture; Use the pure water mass flowmenter on preparation pipeline to measure 112 kilograms of pure water, then be transported in solidification liquid storage tank, open the valve on circulating pump and self-loopa pipeline, it is 800L/h that self-loopa flow is set, heat exchanger is set, and the temperature of controlling self-loopa fluid is 35 DEG C, uses the dimethyl sulfoxide (DMSO) mass flowmenter on preparation pipeline to measure 288 kilograms of dimethyl sulfoxide (DMSO)s, then in suction solidification liquid storage tank, it is 200L/h that mass flowmenter is carried the volume flow of dimethyl sulfoxide (DMSO); After dimethyl sulfoxide (DMSO) has been carried, circulating pump stops after continuing to turn round 20 minutes with the flow of 800L/h, dimethyl sulfoxide (DMSO)/aqueous solution in solidification liquid storage tank left standstill after 3 minutes, observe liquid level top without floating thing, solidification liquid is as clear as crystal, and the concentration of testing solidification liquid with refractometer is 71.6%.
The solidification liquid preparing, opens outer circulation and can carry out spinning technique. Spinning technique is as follows:
1, stoste preparation: by acrylonitrile (AN), itaconic acid (IA) 97:3, solid content 20% in proportion through distillation; azodiisobutyronitrile (AIBN) accounts for the 0.4wt% of comonomer; join in reactor taking dimethyl sulfoxide (DMSO) (DMSO) as solvent; under nitrogen protection; under the steady temperature of 59 DEG C, react 20 hours, obtain binary acrylonitrile copolymer spinning fluid. Then spinning solution removes after residual monomer and bubble through decompression, through the filtration of 5 μ m filtering materials, obtains acrylonitrile copolymer spinning solution. After tested, molecular weight is 80021, and molecular weight distribution is 3.34, and viscosity is 75PaS at 60 DEG C.
2, coagulation forming: spinning solution is through measuring pump metering, again after 3 μ m filter, after extruding by spinning head, enter the 1st road coagulating bath, 20 DEG C of coagulation bath temperatures, concentration is 50%, draw ratio is-30%, the 2nd road coagulating bath is 40 DEG C, and concentration is 40%, and draw ratio is 100%, the 3rd road coagulating bath is 60 DEG C, concentration is 30%, and draw ratio is 105%, obtains as-spun fibre.
3, drawing-off and washing:
After as-spun fibre solidifies by 3 roads, carry out hot water 3 road drawing-offs, 3 road hot water drawing temperatures are respectively 90 DEG C, 95 DEG C and 97 DEG C, and drafting multiple is respectively 1.5,1.5 and 1.5.. After 3 road hot water drawing-offs, strand carries out 9 road washings, adopts the mode of ladder-elevating temperature, and 1-3 road washing temperature is 50 DEG C, and 4-6 road washing temperature is 60 DEG C, and 7-9 road washing temperature is 70 DEG C, and the washing stage is not carried out drawing-off.
4, oil and compacting by drying: the fiber that step 3 is obtained carries out after 1 road oils carrying out compacting by drying, and temperature is 90 DEG C, once oils subsequently again, after oiling, carries out the 2nd road compacting by drying, and the temperature of compacting by drying is 120 DEG C.
5, steam drafting: the fiber that step 4 is obtained carries out steam drafting, the pressure of steam drafting is 0.2Mpa, draw ratio is 2 times.
6, steam heat is shaped and is received silk: the fiber that step 5 is obtained carries out the rear receipts silk of steam heat sizing, obtains high-performance carbon fibre precursor, and the pressure of steam heat sizing is 0.2Mpa.
Fiber without lousiness, without fracture of wire, there is no the phenomenon of fiber curling round the roll, the fiber number of gained precursor is 1.21dtex, filament strength is 6cN/dtex, precursor density is 1.178.
[embodiment 2]
The water of draining in filter and heat exchanger; Use dry air to purge heat exchanger, filter and part self-loopa pipeline, make its inside not leave moisture; Use the pure water mass flowmenter on preparation pipeline to measure 112 kilograms of pure water, then be transported in solidification liquid storage tank, open the valve on circulating pump and self-loopa pipeline, it is 800L/h that self-loopa flow is set, heat exchanger is set, and the temperature of controlling self-loopa fluid is 35 DEG C, uses the dimethyl sulfoxide (DMSO) mass flowmenter on preparation pipeline to measure 288 kilograms of dimethyl sulfoxide (DMSO)s, then in suction solidification liquid storage tank, it is 200L/h that mass flowmenter is carried the volume flow of dimethyl sulfoxide (DMSO); After dimethyl sulfoxide (DMSO) has been carried, circulating pump stops after continuing to turn round 20 minutes with the flow of 800L/h, dimethyl sulfoxide (DMSO)/aqueous solution in solidification liquid storage tank left standstill after 3 minutes, observe liquid level top without floating thing, solidification liquid is as clear as crystal, and the concentration of testing solidification liquid with refractometer is 71.6%.
[embodiment 3]
The water of draining in filter and heat exchanger; Use dry air to purge heat exchanger, filter and part self-loopa pipeline, make its inside not leave moisture; Use the pure water mass flowmenter on preparation pipeline to measure 220 kilograms of pure water, then be transported in solidification liquid storage tank, open the valve on circulating pump and self-loopa pipeline, it is 1000L/h that self-loopa flow is set, heat exchanger is set, and the temperature of controlling self-loopa fluid is 38 DEG C, uses the dimethyl sulfoxide (DMSO) mass flowmenter on preparation pipeline to measure 180 kilograms of dimethyl sulfoxide (DMSO)s, then in suction solidification liquid storage tank, it is 300L/h that mass flowmenter is carried the volume flow of dimethyl sulfoxide (DMSO); After dimethyl sulfoxide (DMSO) has been carried, circulating pump stops after continuing to turn round 15 minutes with the flow of 1000L/h, dimethyl sulfoxide (DMSO)/aqueous solution in solidification liquid storage tank left standstill after 3 minutes, observe liquid level top without floating thing, solidification liquid is as clear as crystal, and the concentration of testing solidification liquid with refractometer is 44.6%.
[embodiment 4]
The water of draining in filter and heat exchanger; Use dry air to purge heat exchanger, filter and part self-loopa pipeline, make its inside not leave moisture; Use the pure water mass flowmenter on preparation pipeline to measure 320 kilograms of pure water, then be transported in solidification liquid storage tank, open the valve on circulating pump and self-loopa pipeline, it is 500L/h that self-loopa flow is set, heat exchanger is set, and the temperature of controlling self-loopa fluid is 40 DEG C, uses the dimethyl sulfoxide (DMSO) mass flowmenter on preparation pipeline to measure 80 kilograms of dimethyl sulfoxide (DMSO)s, then in suction solidification liquid storage tank, it is 150L/h that mass flowmenter is carried the volume flow of dimethyl sulfoxide (DMSO); After dimethyl sulfoxide (DMSO) has been carried, circulating pump stops after continuing to turn round 10 minutes with the flow of 500L/h, dimethyl sulfoxide (DMSO)/aqueous solution in solidification liquid storage tank left standstill after 3 minutes, observe liquid level top without floating thing, solidification liquid is as clear as crystal, and the concentration of testing solidification liquid with refractometer is 19.7%.
[embodiment 5]
The water of draining in filter and heat exchanger; Use dry air to purge heat exchanger, filter and part self-loopa pipeline, make its inside not leave moisture; Use the pure water mass flowmenter on preparation pipeline to measure 192 kilograms of pure water, then be transported in solidification liquid storage tank, open the valve on circulating pump and self-loopa pipeline, it is 1000L/h that self-loopa flow is set, heat exchanger is set, and the temperature of controlling self-loopa fluid is 33 DEG C, uses the dimethyl sulfoxide (DMSO) mass flowmenter on preparation pipeline to measure 408 kilograms of dimethyl sulfoxide (DMSO)s, then in suction solidification liquid storage tank, it is 300L/h that mass flowmenter is carried the volume flow of dimethyl sulfoxide (DMSO); After dimethyl sulfoxide (DMSO) has been carried, circulating pump stops after continuing to turn round 20 minutes with the flow of 1000L/h, dimethyl sulfoxide (DMSO)/aqueous solution in solidification liquid storage tank left standstill after 3 minutes, observe liquid level top without floating thing, solidification liquid is as clear as crystal, and the concentration of testing solidification liquid with refractometer is 67.6%.
[embodiment 6]
The water of draining in filter and heat exchanger; Use dry air to purge heat exchanger, filter and part self-loopa pipeline, make its inside not leave moisture; Use the pure water mass flowmenter on preparation pipeline to measure 378 kilograms of pure water, then be transported in solidification liquid storage tank, open the valve on circulating pump and self-loopa pipeline, it is 1000L/h that self-loopa flow is set, heat exchanger is set, and the temperature of controlling self-loopa fluid is 40 DEG C, uses the dimethyl sulfoxide (DMSO) mass flowmenter on preparation pipeline to measure 222 kilograms of dimethyl sulfoxide (DMSO)s, then in suction solidification liquid storage tank, it is 300L/h that mass flowmenter is carried the volume flow of dimethyl sulfoxide (DMSO); After dimethyl sulfoxide (DMSO) has been carried, circulating pump stops after continuing to turn round 20 minutes with the flow of 1000L/h, dimethyl sulfoxide (DMSO)/aqueous solution in solidification liquid storage tank left standstill after 3 minutes, observe liquid level top without floating thing, solidification liquid is as clear as crystal, and the concentration of testing solidification liquid with refractometer is 36.7%.
[embodiment 7]
The water of draining in filter and heat exchanger; Use dry air to purge heat exchanger, filter and part self-loopa pipeline, make its inside not leave moisture; Use the pure water mass flowmenter on preparation pipeline to measure 426 kilograms of pure water, then be transported in solidification liquid storage tank, open the valve on circulating pump and self-loopa pipeline, it is 1000L/h that self-loopa flow is set, heat exchanger is set, and the temperature of controlling self-loopa fluid is 35 DEG C, uses the dimethyl sulfoxide (DMSO) mass flowmenter on preparation pipeline to measure 174 kilograms of dimethyl sulfoxide (DMSO)s, then in suction solidification liquid storage tank, it is 300L/h that mass flowmenter is carried the volume flow of dimethyl sulfoxide (DMSO); After dimethyl sulfoxide (DMSO) has been carried, circulating pump stops after continuing to turn round 15 minutes with the flow of 1000L/h, dimethyl sulfoxide (DMSO)/aqueous solution in solidification liquid storage tank left standstill after 3 minutes, observe liquid level top without floating thing, solidification liquid is as clear as crystal, and the concentration of testing solidification liquid with refractometer is 28.6%.
[comparative example]
Cleaned after the EGR of solidification liquid, the water in emptying storage tank, does not consider the residual water in filter and heat exchanger; Do not use dry air to purge heat exchanger, filter and part self-loopa pipeline; The pipeline part in solidification liquid storage tank is stretched in self-loopa and outer circulation, and the lower edge of pipeline is positioned at solidifies liquid level top; Self-loopa pipeline end is without venturi jet pipe; Use the dimethyl sulfoxide (DMSO) mass flowmenter on preparation pipeline to measure 288 kilograms of dimethyl sulfoxide (DMSO)s, squeezed in solidification liquid storage tank, use the pure water mass flowmenter on preparation pipeline to measure 112 kilograms of pure water, squeezed in solidification liquid storage tank, open the valve on self-loopa pipeline, the pipeline of self-loopa is without filter and heat exchanger, ON cycle pump, and self-loopa flow is 6.5m3/ h, after 20 minutes, close circulating pump, dimethyl sulfoxide (DMSO)/aqueous solution in solidification liquid storage tank left standstill after 5 minutes, observing liquid level top has the catabolite of the similar oily of dense distribution, there is offending odor dispersion liquid level top, body color micro emulsion is white, muddiness, and the concentration of testing solidification liquid with refractometer is 68.6%.
Can be found out by comparative example and embodiment, adopt the solution of the present invention, can improve the accuracy of preparation solidification liquid concentration, effectively suppress the thermal decomposition of dimethyl sulfoxide (DMSO), feed intake concentration and the actual concentrations difference of dimethyl sulphoxide aqueous solution are less than 0.5%, the solidification liquid preparing is transparent, and good technique effect, without obvious similar greasy dirt floating thing, has been obtained in surface.
Claims (10)
1. an EGR for solidification liquid, comprising: purging system, compounding system, self-circulation system; Wherein, described fromThe circulatory system comprises flowmeter (21), circulating pump (7,7'), pumps pipeline (11), circulation line (12), refluxPipeline (13), venturi jet pipe (6) and solidification liquid storage tank (9), connect at least two heat exchange in described circulation lineDevice (4,4'); When described self-circulation system work, circulating pump pumps the liquid in solidification liquid storage tank through pumping pipeline, followingEndless tube road, return line, venturi jet pipe turn back in solidification liquid storage tank; Described purging system is used for blowing through scavenging pipelineSweep circulation line and solidification liquid intake line; Described compounding system is through preparing pipeline (9) for the input of preparation material is solidifiedLiquid storage tank.
2. the EGR of solidification liquid according to claim 1, is characterized in that being also connected with in described circulation lineFilter (3).
3. the EGR of solidification liquid according to claim 1 and 2, is characterized in that the EGR of described solidification liquidAlso comprise external circulating system, described external circulating system comprises flowmeter (21), circulating pump (7,7'), pumps pipeline (11),Circulation line (12), solidification liquid intake line (14), coagulating tank (8), solidification liquid output pipe (15), literary compositionJet pipe in mound (6) and solidification liquid storage tank (9); When the work of described external circulating system, circulating pump is by solidification liquid storage tankLiquid pumps through pumping pipeline, circulation line, solidification liquid intake line solidification liquid is input in coagulating tank, coagulating tankThe solidification liquid overflowing returns in solidification liquid storage tank through solidification liquid output pipe, venturi jet pipe.
4. the EGR of a kind of solidification liquid according to claim 3, is characterized in that in described solidification liquid intake lineBe connected with flow measurement device.
5. the EGR of a kind of solidification liquid according to claim 3, is characterized in that in described solidification liquid output pipeBe connected with static mixer (2).
6. the EGR of a kind of solidification liquid according to claim 3, is characterized in that described external circulating system also comprisesFor the automatic water-replenishing device of moisturizing in the solidification liquid overflowing to coagulating tank.
7. the EGR of a kind of solidification liquid according to claim 3, is characterized in that in described solidification liquid intake lineBeing connected with flow measurement device is flowmeter (5,5').
8. the EGR of solidification liquid according to claim 3, is characterized in that described solidification liquid output pipe puts in solidifyingPipeline in solid-liquid storage tank is positioned at the axial centre of storage tank substantially, and the lower edge of pipeline is less than 20 centimetres to the distance of tank bottom.
9. a compound method for solidification liquid, adopts the EGR of the arbitrary described solidification liquid of claim 1～8, comprise withLower step:
(a) first clean solidification liquid storage tank, circulating pump, circulation line, venturi jet pipe; After cleaning completes, water is putSky is removed;
(b) use dry gas purge circulation line, make its inside not leave water;
(c) use preparation pipeline, required toward injecting through the preparation solidification liquid of metering in solidification liquid storage tank by mass flowmenterThe water of weight;
(d) open circulating pump, regulate the flow of certain glass rotameter to start circulation, and heat exchanger is set, controlThe temperature of the solidification liquid of self-loopa is less than 40 DEG C;
(e) use preparation pipeline, required toward injecting through the preparation solidification liquid of metering in solidification liquid storage tank by mass flowmenterThe dimethyl sulfoxide (DMSO) of weight and the 3rd component, join in solidification liquid storage tank with certain flow, and this flow is less than following of circulating pump/ 3rd of a circulation; The pH value conditioning agent that the 3rd component is solidification liquid, or a class thing of raising solidification liquid stabilityMatter, or both combinations, but be not limited to both;
(f) after described dimethyl sulfoxide (DMSO) all adds, circulating pump remains in operation and carries out self-loopa, continues the time of self-loopaBe not less than 10 minutes; Use refractometer to measure the concentration of solidification liquid, obtain certain density solidification liquid for subsequent use.
10. the application of the EGR of the arbitrary described solidification liquid of claim 1～8 in spinning technique.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410582251.5A CN105597580B (en) | 2014-10-27 | 2014-10-27 | The device for formulating and compound method of solidification liquid and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410582251.5A CN105597580B (en) | 2014-10-27 | 2014-10-27 | The device for formulating and compound method of solidification liquid and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105597580A true CN105597580A (en) | 2016-05-25 |
| CN105597580B CN105597580B (en) | 2018-04-06 |
Family
ID=55978250
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410582251.5A Active CN105597580B (en) | 2014-10-27 | 2014-10-27 | The device for formulating and compound method of solidification liquid and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105597580B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112877799A (en) * | 2020-12-31 | 2021-06-01 | 荣成碳纤维科技有限公司 | Method and system for producing carbon fiber dry-jet wet-spun precursor |
| CN113215668A (en) * | 2021-04-16 | 2021-08-06 | 山西钢科碳材料有限公司 | Polyacrylonitrile nascent fiber, polyacrylonitrile fiber and preparation method thereof |
| US11934822B2 (en) | 2022-04-07 | 2024-03-19 | Ford Global Technologies, Llc | Systems and methods for connected vehicle enhancements |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003060207A1 (en) * | 2002-01-09 | 2003-07-24 | E. I. Du Pont De Nemours And Company | Polypeptide fibers and processes for making them |
| CN101967689A (en) * | 2010-09-30 | 2011-02-09 | 中国科学院宁波材料技术与工程研究所 | Method and device for controlling multi-level coagulation bath concentration for spinning polyacrylonitrile protofilament |
| CN101988216A (en) * | 2009-08-04 | 2011-03-23 | 上海太平洋纺织机械成套设备有限公司 | Method for circularly preparing solvents in Lyocell fiber preparation process |
| CN202830261U (en) * | 2012-07-26 | 2013-03-27 | 中国石油天然气股份有限公司 | Polyacrylonitrile precursor coagulating bath circulation current stabilizer |
-
2014
- 2014-10-27 CN CN201410582251.5A patent/CN105597580B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003060207A1 (en) * | 2002-01-09 | 2003-07-24 | E. I. Du Pont De Nemours And Company | Polypeptide fibers and processes for making them |
| CN101988216A (en) * | 2009-08-04 | 2011-03-23 | 上海太平洋纺织机械成套设备有限公司 | Method for circularly preparing solvents in Lyocell fiber preparation process |
| CN101967689A (en) * | 2010-09-30 | 2011-02-09 | 中国科学院宁波材料技术与工程研究所 | Method and device for controlling multi-level coagulation bath concentration for spinning polyacrylonitrile protofilament |
| CN202830261U (en) * | 2012-07-26 | 2013-03-27 | 中国石油天然气股份有限公司 | Polyacrylonitrile precursor coagulating bath circulation current stabilizer |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112877799A (en) * | 2020-12-31 | 2021-06-01 | 荣成碳纤维科技有限公司 | Method and system for producing carbon fiber dry-jet wet-spun precursor |
| CN112877799B (en) * | 2020-12-31 | 2022-03-11 | 荣成碳纤维科技有限公司 | Method and system for producing carbon fiber dry-jet wet-spun precursor |
| CN113215668A (en) * | 2021-04-16 | 2021-08-06 | 山西钢科碳材料有限公司 | Polyacrylonitrile nascent fiber, polyacrylonitrile fiber and preparation method thereof |
| CN113215668B (en) * | 2021-04-16 | 2022-11-11 | 山西钢科碳材料有限公司 | Polyacrylonitrile nascent fiber, polyacrylonitrile fiber and preparation method thereof |
| US11934822B2 (en) | 2022-04-07 | 2024-03-19 | Ford Global Technologies, Llc | Systems and methods for connected vehicle enhancements |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105597580B (en) | 2018-04-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101837248B (en) | Production method of cellosilk enhanced compound hollow fiber membrane | |
| CN101724922B (en) | Method for preparing high-strength polyacrylonitrile-based precursor for carbon fiber | |
| CN105597580A (en) | Solidification liquid preparation apparatus, solidification liquid preparation method, and applications of solidification liquid preparation apparatus | |
| CN103080390A (en) | Lignin/polyacrylonitrile-containing dopes, fibers, and methods of making same | |
| CN101760791A (en) | Method for preparing high-performance polyacrylonitrile-based carbon fiber protofilament through dry spraying and wet spinning | |
| CN107059150B (en) | A kind of preparation method of high intensity regenerated fibroin fiber | |
| CN103103631A (en) | Method for preparing polyacrylonitrile carbon fiber precursor | |
| CN109082730A (en) | Major diameter polyacrylonitrile-based carbon fibre and preparation method thereof | |
| CN106012103A (en) | Method for preparing high-strength alginate fiber | |
| CN105420827B (en) | A kind of method and device of vertical wet spinning | |
| CN103774253B (en) | A kind of wet spinning shaped device | |
| CN111041583B (en) | Large-tow PAN (polyacrylonitrile) -based carbon fiber precursor mass and heat transfer device and method | |
| CN101967689B (en) | Method and device for controlling multi-level coagulation bath concentration for spinning polyacrylonitrile protofilament | |
| CN104480548A (en) | Wet spinning solidification method and wet spinning solidification device | |
| CN103276466B (en) | A kind of preparation method of polytetrafluoroethylene fibre | |
| CN105568413B (en) | A kind of lignin-base doughnut and preparation method thereof | |
| CN103668532A (en) | Method for preparing anti-pilling acrylic fibers from acrylonitrile and vinyl acetate | |
| CN102851775B (en) | Preparation method of pupa protein cellulose composite viscose filament yarn | |
| CN106939439B (en) | Solidification forming method of continuous shallow trench polyacrylonitrile carbon fiber precursor | |
| CN104611787A (en) | Oil agent for polyacrylonitrile-based carbon fiber precursor manufacturing, manufacturing and use method thereof | |
| CN104532395A (en) | Preparation method of macromolecular hydrogen bond compound fiber | |
| JP5299358B2 (en) | Method for producing fiber by wet spinning | |
| CN205295553U (en) | III solidification liquids of aramid fiber regulation and control device | |
| CN204311167U (en) | A kind of pilot scale line acid bath mixing system | |
| CN103668531A (en) | Method for preparing anti-pilling acrylic fibers from acrylonitrile and vinyl chloride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |