CN112830985A - One-step demonomerization and defoaming carbon fiber production method and equipment - Google Patents
One-step demonomerization and defoaming carbon fiber production method and equipment Download PDFInfo
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- CN112830985A CN112830985A CN202011634218.4A CN202011634218A CN112830985A CN 112830985 A CN112830985 A CN 112830985A CN 202011634218 A CN202011634218 A CN 202011634218A CN 112830985 A CN112830985 A CN 112830985A
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 28
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 28
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000007380 fibre production Methods 0.000 title claims abstract description 19
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 543
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 92
- 239000006185 dispersion Substances 0.000 claims abstract description 86
- 238000006243 chemical reaction Methods 0.000 claims abstract description 81
- 239000007788 liquid Substances 0.000 claims abstract description 67
- 239000000945 filler Substances 0.000 claims abstract description 50
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 238000009826 distribution Methods 0.000 claims description 52
- 239000011521 glass Substances 0.000 claims description 36
- 239000000178 monomer Substances 0.000 claims description 25
- 229920000642 polymer Polymers 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 27
- 230000015572 biosynthetic process Effects 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 239000003292 glue Substances 0.000 description 5
- 238000005070 sampling Methods 0.000 description 5
- 238000010924 continuous production Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F20/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F20/02—Monocarboxylic acids having less than ten carbon atoms, Derivatives thereof
- C08F20/42—Nitriles
- C08F20/44—Acrylonitrile
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0422—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing S-atoms
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- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/06—Flash distillation
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- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/002—Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
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- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/02—Feed or outlet devices therefor
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- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
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- C08F2/00—Processes of polymerisation
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- C08F2/00—Processes of polymerisation
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention provides a method and equipment for producing carbon fibers by one-step demonomerization and debubbling, which comprises a reaction kettle, a reboiler and a vacuumizing device, wherein the vacuumizing device is connected with the reaction kettle; the reation kettle top is equipped with the polymer liquid inlet pipe, be equipped with the feeding distributing pipe in the reation kettle, the feeding distributing pipe below is equipped with the feeding distributing tray, the feeding distributing tray below is equipped with filler, the filler below is equipped with diverging device, be equipped with DMSO steam dispersion dish in the reation kettle, the reboiler below is equipped with the DMSO inlet pipe, be equipped with DMSO material loading dispersing pipe in the reboiler, still be equipped with steam inlet on the reboiler, be equipped with the demister in the reboiler, the reboiler with be equipped with the DMSO steam pipe between the reation kettle. The method solves the technical problems of poor quality of polymerization liquid and low production efficiency caused by the fact that demonomerization and debubbling are required to be completed in two steps in the existing carbon fiber production process. The invention can be widely applied to the demonomerization and defoaming process of the carbon fiber.
Description
Technical Field
The invention relates to a carbon fiber production method and equipment thereof, in particular to a carbon fiber production method and equipment thereof for one-step demonomerization and defoaming.
Background
In the domestic carbon fiber production process, the polymerization process demonomerization and defoaming are generally operated by adopting a two-step method. In the polymerization process of carbon fiber production by taking DMSO as a solvent, the conversion rate is low, about 10% of AN monomer contained in a polymerization solution is unreacted, and the residual AN monomer needs to be removed for the second time under a vacuum condition, so that the residual amount of the monomer in the polymerization solution can be reduced to 100-300 PPM, and the spinning polymerization solution is formed.
In addition, bubbles are generated in the polymerization reaction process, the bubbles are not easy to remove, and the residual bubbles can cause filament breakage and influence the quality of carbon fibers, so the polymerization solution also needs to be subjected to defoaming treatment.
In many domestic enterprises, in order to improve the demonomerization and defoaming efficiency of the polymerization stock solution, an additional auxiliary means is tried, but the two procedures of demonomerization and defoaming are carried out under the long-term vacuum condition, so that the solvent on the surface of the polymerization solution is easy to remove, and the polymerization solution gradually becomes gelled or generates gel, thereby influencing the quality of the polymerization solution. For example, the thin film evaporator has a complex structure, inevitably has dead corners, and is easy to produce dry gel at a plurality of positions in the equipment.
Many enterprises also improve the demonomerization and defoaming effects by specially designed internal parts of the demonomerization and defoaming kettles, such as three layers of umbrella disks, even the number of layers of the umbrella disks is increased to 5 layers to improve the demonomerization and defoaming effects, but the mode can not avoid the generation of gel, and simultaneously, the uniformity of the polymerization solution is poor due to the structure reason; moreover, since the film formation area is uncertain and the thickness has a critical value, high-load production cannot be realized. In summary, the existing technical scheme for demonomerizing and defoaming in the polymerization process of carbon fiber production adopts a two-step method, and has the following disadvantages:
(1) the surface of the polymerization liquid is easy to dry or generate gel when the polymerization liquid is operated under the vacuum condition for a long time;
(2) the monomer content and the concentration of the polymerization solution after the polymer solution is demonomerized and defoamed are difficult to be controlled quantitatively;
(3) the monomer of the polymerization liquid can not be completely removed and has poor uniformity;
(4) intermittent operation is needed, high-load and continuous production is difficult to realize, and the production efficiency is limited.
Disclosure of Invention
Aiming at the technical problems of poor quality of a polymerization liquid and low production efficiency caused by the fact that demonomerization and defoaming are required to be completed in two steps in the existing carbon fiber production process, the invention provides a high-quality and high-efficiency production method of demonomerization and defoaming by one step and equipment thereof, which can greatly reduce the monomer content in the polymerization liquid, realize high-load continuous production and avoid the quality problems of gel and the like.
Therefore, the technical scheme of the invention is that the carbon fiber production equipment with one-step demonomerization and debubbling comprises a reaction kettle, a reboiler and a vacuumizing device, wherein the vacuumizing device is connected with the reaction kettle; a polymerization liquid feeding pipe is arranged at the top end of the reaction kettle, a feeding distribution pipe is arranged in the reaction kettle and is connected with the polymerization liquid feeding pipe, a feeding distribution disc is arranged below the feeding distribution pipe, filler is arranged below the feeding distribution disc, a flow distribution device is arranged below the filler, a DMSO steam dispersion disc is arranged in the reaction kettle and is positioned above liquid in the reaction kettle and below the flow distribution device; the device is characterized in that a DMSO feeding pipe is arranged below the reboiler, a DMSO feeding dispersion pipe is arranged in the reboiler, the DMSO feeding pipe is connected with the DMSO feeding dispersion pipe, a steam inlet is further formed in the reboiler, a demister is arranged in the reboiler, the demister is arranged above the DMSO feeding dispersion pipe, the steam inlet is formed in the upper portion of the DMSO feeding dispersion pipe, a DMSO steam pipe is arranged between the reboiler and the reaction kettle, and the DMSO steam pipe is connected with the DMSO steam dispersion disc.
Preferably, the feeding distribution pipe is uniformly distributed in the reaction kettle, the filler is a wire mesh filler, the flow dividing device is a cone with a downward cone tip, and the cone is uniformly distributed below the wire mesh filler.
Preferably, the reaction kettle adopts a tapered structure with a wide upper part and a narrow lower part, and a discharge pipe is arranged at the bottom end of the reaction kettle.
Preferably, the reaction kettle is provided with a sight glass, and the sight glass comprises a top sight glass, a middle sight glass and a bottom sight glass; a reboiler viewing mirror is arranged on the reboiler, and the reboiler viewing mirror is arranged above the DMSO feeding dispersion pipe and below the demister.
Preferably, a condensate outlet pipe is arranged on the reboiler, the condensate outlet pipe is arranged at the lower part of the DMSO feeding dispersion pipe, and the condensate outlet pipe is connected with the DMSO feeding dispersion pipe.
A production method of carbon fiber with one-step demonomerization and deaeration comprises the following specific steps:
(1) starting a vacuumizing device to reduce the pressure in the reaction kettle, and stopping the vacuumizing device when the pressure in the reaction kettle is reduced to 0.1-50 KPa;
(2) the polymerization liquid enters a feeding distribution pipe in the reaction kettle through a polymerization liquid feeding pipe, enters a feeding distribution disc through the feeding distribution pipe, enters the silk screen filler through the feeding distribution disc, and descends through the silk screen filler through the cone;
(3) DMSO enters a DMSO feeding dispersion pipe in a reboiler through a DMSO feeding pipe, after the DMSO feeding dispersion pipe is filled with DMSO, steam is introduced through a steam inlet on the reboiler to heat the DMSO feeding dispersion pipe, DMSO in the DMSO feeding dispersion pipe is flashed into gas under a vacuum condition, the DMSO steam enters a DMSO steam pipe through a demister, and then further enters a DMSO steam dispersion disc in a reaction kettle;
(4) and (3) allowing DMSO steam to enter the reaction kettle through the DMSO steam dispersion plate and move upwards under the action of vacuum, and allowing the DMSO steam to reversely disperse and contact the polymerization solution in the step (2) to complete the demonomerization and debubbling process.
Preferably, in the step (4), under the action of vacuum, DMSO vapor infiltrates the cone, the silk-screen packing and the feeding distribution disc upwards, and the DMSO vapor is in counter-dispersion contact with the polymerization solution.
Preferably, sampling and detecting from a discharge pipe at the bottom end of the reaction kettle to measure the content of the monomer AN in the polymerization liquid.
Preferably, the feeding amount of the polymerization liquid is 400-5500kg/hr, and the feeding amount of the DMSO feeding pipe is 10-30% of the feeding amount of the polymerization liquid feeding pipe.
The beneficial effects of the invention are that,
(1) the polymerization liquid passes through a feeding distribution pipe, a feeding distribution disc and a wire mesh-shaped filler to obtain considerable demonomerization-defoaming mass transfer surface area, and passes through a cone below a filler layer to form filamentous polymerization liquid to flow downwards to be fully contacted with DMSO steam, so that high-efficiency demonomerization-defoaming mass transfer is carried out, monomers are removed, and bubbles are removed;
(2) the reaction kettle is set to be in a cone shape with a wide upper part and a narrow lower part, so that the contact area between the polymerization liquid and the reaction kettle after passing through the filler is favorably reduced, the flash evaporated DMSO steam enters the wire mesh filler from the DMSO steam dispersion disc in a cone dispersion mode, and the DMSO steam soaks the filler, the feeding distribution disc, the feeding distribution pipe and other tower internals in the reaction kettle, so that the generation of gel can be effectively prevented;
(3) the cone with the downward cone tip is uniformly distributed below the screen-shaped filler, so that the polymerization liquid passing through the screen-shaped filler flows down from the cone in a filament shape, high-efficiency demonomerization-defoaming is realized, the monomer content and the concentration of the polymerization liquid after the demonomerization-defoaming of the polymerization liquid can be quantitatively controlled through DMSO steam regulation, and the generation of gel is effectively prevented;
(4) the flash evaporation state of the DMSO can be observed at any time through a reboiler sight glass, and the DMSO passes through a demister after being flashed, so that the nonuniformity of DMSO steam is prevented; the glue formation phenomenon in the reaction kettle is observed through a top sight glass, a middle sight glass and a bottom sight glass of the reaction kettle so as to ensure the demonomerization and defoaming quality of the polymerization liquid;
(5) by adopting the technical scheme, the polymerization solution with the monomer AN content of 0-50ppm can be obtained, the uniformity is good, high-load and continuous production can be realized, and the production efficiency is greatly improved.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
The symbols in the drawings illustrate that:
a DMSO vapor dispersion plate; 2. polymerizing liquid; 3. a cone; 4. a wire mesh filler; 5. a reaction kettle; 6. a feed distribution pipe; 7. a vacuum pumping port; 8. a polymerization liquid feeding pipe; 9. a top view mirror; 10. a feed distribution tray; 11. a middle view mirror; 12. a bottom view mirror; 13. a discharge port; 14. a reboiler sight glass; 15. a condensate outlet; 16. a reboiler; DMSO feed tube; a DMSO feeding dispersion pipe; 19. a steam inlet; 20. a demister; DMSO steam tube.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
As shown in fig. 1, a carbon fiber production facility of defoaming is taken off to one-step process, including reation kettle 5, reboiler 16 and evacuating device, evacuating device is connected through evacuation mouth 7 with reation kettle 5, reation kettle 5 top is equipped with polymer liquid inlet pipe 8, reation kettle 5 inside is equipped with the feeding distributing pipe 6 of equipartition, feeding distributing pipe 6 is connected with polymer liquid inlet pipe 8, feeding distributing pipe 6 below is equipped with feeding distributing disk 10, feeding distributing disk 10 below is equipped with silk screen filler 4, silk screen filler 4 supports fixedly through the support, silk screen filler 4 below equipartition is equipped with 150 ~ 350 downward cones of awl point 3, cone 3 also fixes on the support. Be equipped with the DMSO steam dispersion dish 1 of equipartition in reation kettle 5, DMSO steam dispersion dish 1 is located reation kettle 5 interior liquid top and in the below of cone 3. A DMSO feeding pipe 17 is arranged below the reboiler 16 and used for DMSO feeding, a DMSO feeding dispersion pipe 18 is arranged in the reboiler 16, the DMSO feeding pipe 17 is connected with the DMSO feeding dispersion pipe 18, a demister 20 is arranged above the DMSO feeding dispersion pipe 18 in the reboiler 16, a steam inlet 19 is further arranged on the reboiler 16 and is arranged on the upper portion of the DMSO feeding dispersion pipe 18, a DMSO steam pipe 21 is arranged between the reboiler 16 and the reaction kettle 5, and the DMSO steam pipe 21 is connected with the DMSO steam dispersion disc 1.
A production method of carbon fiber with one-step demonomerization and deaeration comprises the following specific steps:
(1) starting a vacuumizing device to reduce the pressure in the reaction kettle 5 until the pressure is reduced to 0.1 KPa;
(2) the polymerization liquid 2 is pumped into a feeding distribution pipe 6 in a reaction kettle 5 by a pump through a polymerization liquid feeding pipe 8, the flow rate of the polymerization liquid is 5500kg/hr, the concentration of a monomer is 10 percent, the polymerization liquid is uniformly distributed on the feeding distribution disc 10 through 12 to 28 feeding distribution pipes 6, enters a silk screen-shaped filler 4 through the feeding distribution disc 10, goes down through a cone 3 through the silk screen-shaped filler 4 to obtain considerable demonomerization-defoaming mass transfer surface area, and flows downwards through a cone 3 below the silk screen-shaped filler 4 to form a filament-shaped polymerization liquid with the diameter of 0.5mm to 5 mm; a top sight glass 9, a middle sight glass 11 and a bottom sight glass 12 are arranged on the reaction kettle 5, and the glue formation phenomenon in the reaction kettle 5 is observed through the sight glass of the reaction kettle 5 so as to ensure the demonomerization and defoaming quality of the polymerization liquid;
(3) DMSO is slowly delivered to a DMSO feed dispersion pipe 18 in a reboiler 16 through a DMSO feed pipe 17, the flow rate is 25% of the flow rate of the polymer; a reboiler viewing mirror 14 is arranged on the reboiler 16, the reboiler viewing mirror 14 is arranged above the DMSO feeding dispersion pipe 18 and below the demister 20, the liquid level is observed through the reboiler viewing mirror 14, the DMSO feeding dispersion pipe 18 is ensured to be filled with DMSO, then steam is introduced through a steam inlet 19 on the reboiler 16 for heating, DMSO in the DMSO feeding dispersion pipe 18 is flashed into gas under the vacuum condition, and DMSO steam enters a DMSO steam pipe 21 through the demister 20 and then enters the DMSO steam dispersion disc 1 in the reaction kettle 5; a condensate outlet pipe 15 is arranged on the reboiler 16, the condensate outlet pipe 15 is arranged at the lower part of the DMSO feeding dispersion pipe 18, the condensate outlet pipe 15 is connected with the DMSO feeding dispersion pipe 18, and steam condensate is discharged from the steam condensate outlet pipe 15; the flash evaporation state of DMSO is observed at any time through a reboiler sight glass 14, and the DMSO passes through a demister 20 after being flashed, so that the nonuniformity of DMSO steam is prevented; through DMSO steam regulation, the monomer content and the concentration of the polymerization solution after the polymerization solution is demonomerized and defoamed can be quantitatively controlled, and the generation of gel is effectively prevented;
(4) DMSO steam enters a reaction kettle 5 through a DMSO steam dispersion plate 1 and goes upward under the action of vacuum, the DMSO steam upwards infiltrates a cone 3, a wire mesh-shaped filler 4 and a feeding distribution plate 10, the DMSO steam and a polymerization solution 2 are in reverse dispersion contact on the above components and in a space between the wire mesh-shaped filler 4 and the DMSO steam dispersion plate 1, and the demonomerization and debubbling process is completed;
(5) the bottom end of the reaction kettle 5 is provided with a discharge pipe 13, and the AN content of the monomer in the polymerization liquid is measured to be 8ppm by sampling and detecting from the discharge pipe 13.
Example 2
Compared with the embodiment 1, the difference of the embodiment is that a carbon fiber production method with one-step demonomerization and deaeration comprises the following specific steps:
(1) starting a vacuumizing device to reduce the pressure in the reaction kettle 5 until the pressure is reduced to 0.8 KPa;
(2) the polymerization liquid 2 is pumped into a feeding distribution pipe 6 in a reaction kettle 5 by a pump through a polymerization liquid feeding pipe 8, the flow rate of the polymerization liquid is 3800kg/hr, the concentration of a monomer is 10%, the polymerization liquid is uniformly distributed on a feeding distribution disc 10 through 12-28 feeding distribution pipes 6, enters a silk screen-shaped filler 4 through the feeding distribution disc 10, descends through a cone 3 through the silk screen-shaped filler 4 to obtain a considerable demonomerization-defoaming mass transfer surface area, and flows downwards through a cone 3 below the silk screen-shaped filler 4 to form a filament-shaped polymerization liquid with the diameter of 0.5-5 mm; a top sight glass 9, a middle sight glass 11 and a bottom sight glass 12 are arranged on the reaction kettle 5, and the glue formation phenomenon in the reaction kettle 5 is observed through the sight glass of the reaction kettle 5 so as to ensure the demonomerization and defoaming quality of the polymerization liquid;
(3) DMSO is slowly delivered to a DMSO feed dispersion pipe 18 in a reboiler 16 through a DMSO feed pipe 17, the flow rate is 25% of the flow rate of the polymer; a reboiler viewing mirror 14 is arranged on the reboiler 16, the reboiler viewing mirror 14 is arranged above the DMSO feeding dispersion pipe 18 and below the demister 20, the liquid level is observed through the reboiler viewing mirror 14, the DMSO feeding dispersion pipe 18 is ensured to be filled with DMSO, then steam is introduced through a steam inlet 19 on the reboiler 16 for heating, DMSO in the DMSO feeding dispersion pipe 18 is flashed into gas under the vacuum condition, and DMSO steam enters a DMSO steam pipe 21 through the demister 20 and then enters the DMSO steam dispersion disc 1 in the reaction kettle 5; a condensate outlet pipe 15 is arranged on the reboiler 16, the condensate outlet pipe 15 is arranged at the lower part of the DMSO feeding dispersion pipe 18, the condensate outlet pipe 15 is connected with the DMSO feeding dispersion pipe 18, and steam condensate is discharged from the steam condensate outlet pipe 15; the flash evaporation state of DMSO is observed at any time through a reboiler sight glass 14, and the DMSO passes through a demister 20 after being flashed, so that the nonuniformity of DMSO steam is prevented; through DMSO steam regulation, the monomer content and the concentration of the polymerization solution after the polymerization solution is demonomerized and defoamed can be quantitatively controlled, and the generation of gel is effectively prevented;
(4) DMSO steam enters a reaction kettle 5 through a DMSO steam dispersion plate 1 and goes upward under the action of vacuum, the DMSO steam upwards infiltrates a cone 3, a wire mesh-shaped filler 4 and a feeding distribution plate 10, the DMSO steam and a polymerization solution 2 are in reverse dispersion contact on the above components and in a space between the wire mesh-shaped filler 4 and the DMSO steam dispersion plate 1, and the demonomerization and debubbling process is completed;
(5) the bottom end of the reaction kettle 5 is provided with a discharge pipe 13, and the AN content of the monomer in the polymerization liquid is measured to be 9ppm by sampling and detecting from the discharge pipe 13.
Example 3
Compared with the embodiment 1, the difference of the embodiment is that a carbon fiber production method with one-step demonomerization and deaeration comprises the following specific steps:
(1) starting a vacuumizing device to reduce the pressure in the reaction kettle 5 until the pressure is reduced to 5 KPa;
(2) the polymerization liquid 2 is pumped into a feeding distribution pipe 6 in a reaction kettle 5 by a pump through a polymerization liquid feeding pipe 8, the flow rate of the polymerization liquid is 2300kg/hr, the concentration of a monomer is 10 percent, the polymerization liquid is uniformly distributed on a feeding distribution disc 10 through 12-28 feeding distribution pipes 6, enters a silk screen-shaped filler 4 through the feeding distribution disc 10, descends through a cone 3 through the silk screen-shaped filler 4 to obtain a considerable demonomerization-deaeration mass transfer surface area, and flows downwards through a cone 3 below the silk screen-shaped filler 4 to form a thin-thread polymerization liquid with the diameter of 0.5-5 mm; a top sight glass 9, a middle sight glass 11 and a bottom sight glass 12 are arranged on the reaction kettle 5, and the glue formation phenomenon in the reaction kettle 5 is observed through the sight glass of the reaction kettle 5 so as to ensure the demonomerization and defoaming quality of the polymerization liquid;
(3) DMSO is slowly delivered to a DMSO feeding dispersion pipe 18 in a reboiler 16 through a DMSO feeding pipe 17, and the flow rate is 23% of the flow rate of the polymer; a reboiler viewing mirror 14 is arranged on the reboiler 16, the reboiler viewing mirror 14 is arranged above the DMSO feeding dispersion pipe 18 and below the demister 20, the liquid level is observed through the reboiler viewing mirror 14, the DMSO feeding dispersion pipe 18 is ensured to be filled with DMSO, then steam is introduced through a steam inlet 19 on the reboiler 16 for heating, DMSO in the DMSO feeding dispersion pipe 18 is flashed into gas under the vacuum condition, and DMSO steam enters a DMSO steam pipe 21 through the demister 20 and then enters the DMSO steam dispersion disc 1 in the reaction kettle 5; a condensate outlet pipe 15 is arranged on the reboiler 16, the condensate outlet pipe 15 is arranged at the lower part of the DMSO feeding dispersion pipe 18, the condensate outlet pipe 15 is connected with the DMSO feeding dispersion pipe 18, and steam condensate is discharged from the steam condensate outlet pipe 15; the flash evaporation state of DMSO is observed at any time through a reboiler sight glass 14, and the DMSO passes through a demister 20 after being flashed, so that the nonuniformity of DMSO steam is prevented; through DMSO steam regulation, the monomer content and the concentration of the polymerization solution after the polymerization solution is demonomerized and defoamed can be quantitatively controlled, and the generation of gel is effectively prevented;
(4) DMSO steam enters a reaction kettle 5 through a DMSO steam dispersion plate 1 and goes upward under the action of vacuum, the DMSO steam upwards infiltrates a cone 3, a wire mesh-shaped filler 4 and a feeding distribution plate 10, the DMSO steam and a polymerization solution 2 are in reverse dispersion contact on the above components and in a space between the wire mesh-shaped filler 4 and the DMSO steam dispersion plate 1, and the demonomerization and debubbling process is completed;
(5) the bottom end of the reaction kettle 5 is provided with a discharge pipe 13, and the AN content of the monomer in the polymerization liquid is 10ppm by sampling and detecting from the discharge pipe 13.
Example 4
Compared with the embodiment 1, the difference of the embodiment is that a carbon fiber production method with one-step demonomerization and deaeration comprises the following specific steps:
(1) starting a vacuumizing device to reduce the pressure in the reaction kettle 5 until the pressure is reduced to 50 KPa;
(2) the polymerization liquid 2 is pumped into a feeding distribution pipe 6 in a reaction kettle 5 by a pump through a polymerization liquid feeding pipe 8, the flow rate of the polymerization liquid is 400kg/hr, the concentration of a monomer is 10 percent, the polymerization liquid is uniformly distributed on a feeding distribution disc 10 through 12-28 feeding distribution pipes 6, enters a silk screen-shaped filler 4 through the feeding distribution disc 10, descends through a cone 3 through the silk screen-shaped filler 4 to obtain a considerable demonomerization-defoaming mass transfer surface area, and flows downwards through a cone 3 below the silk screen-shaped filler 4 to form a thin-thread polymerization liquid with the diameter of 0.5-5 mm; a top sight glass 9, a middle sight glass 11 and a bottom sight glass 12 are arranged on the reaction kettle 5, and the glue formation phenomenon in the reaction kettle 5 is observed through the sight glass of the reaction kettle 5 so as to ensure the demonomerization and defoaming quality of the polymerization liquid;
(3) DMSO is slowly delivered to a DMSO feeding dispersion pipe 18 in a reboiler 16 through a DMSO feeding pipe 17, and the flow rate is 12% of the flow rate of the polymer; a reboiler viewing mirror 14 is arranged on the reboiler 16, the reboiler viewing mirror 14 is arranged above the DMSO feeding dispersion pipe 18 and below the demister 20, the liquid level is observed through the reboiler viewing mirror 14, the DMSO feeding dispersion pipe 18 is ensured to be filled with DMSO, then steam is introduced through a steam inlet 19 on the reboiler 16 for heating, DMSO in the DMSO feeding dispersion pipe 18 is flashed into gas under the vacuum condition, and DMSO steam enters a DMSO steam pipe 21 through the demister 20 and then enters the DMSO steam dispersion disc 1 in the reaction kettle 5; a condensate outlet pipe 15 is arranged on the reboiler 16, the condensate outlet pipe 15 is arranged at the lower part of the DMSO feeding dispersion pipe 18, the condensate outlet pipe 15 is connected with the DMSO feeding dispersion pipe 18, and steam condensate is discharged from the steam condensate outlet pipe 15; the flash evaporation state of DMSO is observed at any time through a reboiler sight glass 14, and the DMSO passes through a demister 20 after being flashed, so that the nonuniformity of DMSO steam is prevented; through DMSO steam regulation, the monomer content and the concentration of the polymerization solution after the polymerization solution is demonomerized and defoamed can be quantitatively controlled, and the generation of gel is effectively prevented;
(4) DMSO steam enters a reaction kettle 5 through a DMSO steam dispersion plate 1 and goes upward under the action of vacuum, the DMSO steam upwards infiltrates a cone 3, a wire mesh-shaped filler 4 and a feeding distribution plate 10, the DMSO steam and a polymerization solution 2 are in reverse dispersion contact on the above components and in a space between the wire mesh-shaped filler 4 and the DMSO steam dispersion plate 1, and the demonomerization and debubbling process is completed;
(5) the bottom end of the reaction kettle 5 is provided with a discharge pipe 13, and the AN content of the monomer in the polymerization liquid is measured to be 13ppm by sampling and detecting from the discharge pipe 13.
The state of the polymerization solution after demonomerization and defoaming is observed through a bottom sight glass, the uniformity is good, no bubbles can be seen by naked eyes, the device can realize high-load continuous production, and the production efficiency is greatly improved.
The differences in the specific parameters of examples 1 to 4 are shown in Table 1.
| Item | Example 1 | Example 2 | Example 3 | Example 4 |
| Internal pressure of reaction kettle (kpa) | 0.1 | 0.8 | 5 | 50 |
| Flow rate of polymerization solution (kg/hr) | 5500 | 3800 | 2300 | 400 |
| Monomer concentration (%) | 10 | 10 | 10 | 10 |
| DMSO flow/polymerization flow (%) | 25 | 25 | 23 | 12 |
| AN monomer content (ppm) in the polymerization liquid after the reaction | 8 | 9 | 10 | 13 |
However, the above description is only exemplary of the present invention, and the scope of the present invention should not be limited thereby, and the replacement of the equivalent components or the equivalent changes and modifications made according to the protection scope of the present invention should be covered by the claims of the present invention.
Claims (9)
1. The carbon fiber production equipment with the one-step demonomerization and defoaming function is characterized by comprising a reaction kettle, a reboiler and a vacuumizing device, wherein the vacuumizing device is connected with the reaction kettle; a polymerization liquid feeding pipe is arranged at the top end of the reaction kettle, a feeding distribution pipe is arranged in the reaction kettle and is connected with the polymerization liquid feeding pipe, a feeding distribution disc is arranged below the feeding distribution pipe, filler is arranged below the feeding distribution disc, a flow distribution device is arranged below the filler, a DMSO steam dispersion disc is arranged in the reaction kettle and is positioned above liquid in the reaction kettle and below the flow distribution device; the device is characterized in that a DMSO feeding pipe is arranged below the reboiler, a DMSO feeding dispersion pipe is arranged in the reboiler, the DMSO feeding pipe is connected with the DMSO feeding dispersion pipe, a steam inlet is further formed in the reboiler, a demister is arranged in the reboiler, the demister is arranged above the DMSO feeding dispersion pipe, the steam inlet is formed in the upper portion of the DMSO feeding dispersion pipe, a DMSO steam pipe is arranged between the reboiler and the reaction kettle, and the DMSO steam pipe is connected with the DMSO steam dispersion disc.
2. The one-step demonomerization and debubbling carbon fiber production equipment as claimed in claim 1, wherein the feed distribution pipes are uniformly distributed in the reaction kettle, the filler is a wire mesh filler, the flow dividing device is a cone with a downward cone tip, and the cone is uniformly distributed below the wire mesh filler.
3. The one-step demonomerization and debubbling carbon fiber production equipment as claimed in claim 1, wherein the reaction kettle adopts a tapered structure with a wide top and a narrow bottom, and a discharge pipe is arranged at the bottom end of the reaction kettle.
4. The one-step demonomerization and debubbling carbon fiber production equipment as claimed in claim 1, wherein the reaction kettle is provided with a sight glass, and the sight glass comprises a top sight glass, a middle sight glass and a bottom sight glass; a reboiler viewing mirror is arranged on the reboiler, and the reboiler viewing mirror is arranged above the DMSO feeding dispersion pipe and below the demister.
5. The one-step demonomerization and debubbling carbon fiber production equipment as claimed in claim 1, wherein a condensate outlet pipe is arranged on the reboiler, the condensate outlet pipe is arranged at the lower part of the DMSO feeding dispersion pipe, and the condensate outlet pipe is connected with the DMSO feeding dispersion pipe.
6. A production method of carbon fiber with one-step demonomerization and deaeration comprises the following specific steps:
(1) starting a vacuumizing device to reduce the pressure in the reaction kettle, and stopping the vacuumizing device when the pressure in the reaction kettle is reduced to 0.1-50 KPa;
(2) the polymerization liquid enters a feeding distribution pipe in the reaction kettle through a polymerization liquid feeding pipe, enters a feeding distribution disc through the feeding distribution pipe, enters the silk screen filler through the feeding distribution disc, and descends through the silk screen filler through the cone;
(3) DMSO enters a DMSO feeding dispersion pipe in a reboiler through a DMSO feeding pipe, after the DMSO feeding dispersion pipe is filled with DMSO, steam is introduced through a steam inlet on the reboiler to heat the DMSO feeding dispersion pipe, DMSO in the DMSO feeding dispersion pipe is flashed into gas under a vacuum condition, the DMSO steam enters a DMSO steam pipe through a demister, and then further enters a DMSO steam dispersion disc in a reaction kettle;
(4) and (3) allowing DMSO steam to enter the reaction kettle through the DMSO steam dispersion plate and move upwards under the action of vacuum, and allowing the DMSO steam to reversely disperse and contact the polymerization solution in the step (2) to complete the demonomerization and debubbling process.
7. The method for producing demonomerized carbon fiber by one-step process according to claim 6, wherein in the step (4), DMSO vapor infiltrates the cone, the silk-screen filler and the feeding distribution plate upwards under the action of vacuum, and the DMSO vapor is in counter-dispersion contact with the polymerization solution.
8. The method for producing demonomerized and debubbled carbon fiber in one step as claimed in claim 6, wherein a discharge pipe at the bottom end of the reaction kettle is sampled and detected to measure the AN content of the monomer in the polymerization liquid.
9. The method for producing demonomerized carbon fiber by one-step process as claimed in claim 6, wherein the feeding amount of the polymerization solution is 400-5500kg/hr, and the feeding amount of the DMSO feeding pipe is 10-30% of the feeding amount of the polymerization solution feeding pipe.
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