阅读说明：本技术 一种碳纤维生产过程中脱单脱泡提浓的方法及其设备 (Method and equipment for demonomerization, deaeration and concentration in carbon fiber production process ) 是由 赵彦国 张立坚 张伟 刘运波 沈传石 杨昆 陈志敏 孙毅 刘根房 张超 王春晓 于 2021-10-21 设计创作，主要内容包括：本发明提供一种碳纤维生产过程中脱单脱泡提浓的方法及其设备,设有浓缩塔,所述浓缩塔包括筒体、上封头、下封头,所述上封头上设有进料管,所述进料管上连接下料管,所述下料管上设有固定法兰,所述固定法兰上设有喷淋口,所述下料管上设有物料均分管,所述筒体内还设有均散盘,所述均散盘下方设有栅格支撑,所述栅格支撑下方设有填料,所述填料下方设有驼峰支撑,所述驼峰支撑下部设有蒸汽筒,所述蒸汽筒上连接再沸器,所述筒体上方连接真空系统,所述下封头底部设有出料口。其解决了现有碳纤维生产中不能有效控制聚合液的浓度、聚合液中的单体、气泡脱不净、产能受限、设备内产生凝胶的技术问题。本发明可广泛应用于碳纤维生产中。(The invention provides a method and equipment for demonomerization, defoamation and concentration in the production process of carbon fibers, which are provided with a concentration tower, wherein the concentration tower comprises a cylinder body, an upper end enclosure and a lower end enclosure, the upper end enclosure is provided with a feeding pipe, the feeding pipe is connected with a blanking pipe, the blanking pipe is provided with a fixing flange, the fixing flange is provided with a spray port, the blanking pipe is provided with a material equalizing pipe, the cylinder body is also internally provided with an equalizing disc, a grid support is arranged below the equalizing disc, a filler is arranged below the grid support, a hump support is arranged below the filler, a steam cylinder is arranged below the hump support, the steam cylinder is connected with a reboiler, the cylinder body is connected with a vacuum system, and the bottom of the lower end enclosure is provided with a discharge port. The method solves the technical problems that the concentration of a polymerization liquid, monomers and bubbles in the polymerization liquid cannot be effectively controlled, the capacity is limited and gel is generated in equipment in the existing carbon fiber production. The invention can be widely applied to the production of carbon fiber.)

1. A demonomerization, deaeration and concentration device in the carbon fiber production process is characterized in that a concentration tower is arranged, the concentration tower comprises a barrel body, an upper end enclosure and a lower end enclosure, the upper end enclosure is positioned above the barrel body, the lower end enclosure is positioned below the barrel body, the upper end enclosure is provided with a feeding pipe, the feeding pipe is connected with a discharging pipe, the discharging pipe is provided with a fixed flange, the discharging pipe is fixed on the upper end enclosure through the fixed flange, the fixed flange is provided with a spray opening, the discharging pipe is provided with a material uniform distribution pipe, a uniform dispersion disc is further arranged in the barrel body, a grid support is arranged below the uniform dispersion disc, filler is arranged below the grid support, a reboiler peak support is arranged below the filler, a gap is reserved between the hump supports, a steam barrel is arranged below the hump support, and the steam barrel is connected with the steam barrel, the vacuum system is connected to barrel top, the low head bottom is equipped with the discharge gate.

2. The apparatus for demonomerization, debubbling and concentration in carbon fiber production process according to claim 1, wherein the cylinder is further provided with an upper manhole and a lower manhole, the lower manhole is arranged on the cylinder at the position of the filler, and the lower manhole is provided with a blocking plate.

3. The apparatus for demonomerization, deaeration and concentration during carbon fiber production according to claim 1, wherein an upper view mirror is arranged on the upper head, a lower view mirror is arranged on the barrel below the hump support, an inspection port is arranged above the feeding pipe, a thermometer socket, a sampling port and a standby port are arranged on the lower head, and a thermal resistance thermometer is arranged on the thermometer socket.

4. The apparatus for demonomerization, defoamation and concentration in carbon fiber production process according to claim 1, wherein three spray openings are provided on each mounting flange, the spray openings are connected with a spray system, the spray system is provided with an electromagnetic valve, and the spray system adopts a DCS to control the on-off of the electromagnetic valve.

5. The apparatus for demonomerization, defoamation and concentration in the carbon fiber production process according to claim 1, wherein the material homogenizing pipe is an annular material homogenizing pipe, and the filler is a random packing.

6. A method for demonomerization, deaeration and concentration in the carbon fiber production process according to any one of claims 1 to 5 is characterized by comprising the following specific steps:

(1) the polymer liquid enters the blanking pipe from the feeding pipe and flows onto the dispersion plate through the annular material distribution pipe on the blanking pipe, so that the polymer liquid is uniformly distributed, and a polymer liquid film is formed in the falling flowing process of the polymer liquid;

(2) the spraying system is intermittently started, the polymerization liquid in the concentration tower is sprayed diagonally through the spraying port, the concentration of the polymerization liquid is adjusted, and the part on the upper part in the cylinder body is prevented from being glued;

(3) the uniformly distributed polymerization liquid after passing through the dispersion plate falls on the random packing to form a thinner polymerization liquid film on the random packing, so that the polymerization liquid is fully contacted with the gas phase, and a large amount of monomers, bubbles and solvents are removed from the polymerization liquid;

(4) the reboiler conveys high-temperature gaseous solvent to the concentration tower through the steam drum, the temperature in the concentration tower is raised, the solvent and the monomer in the polymerization liquid are gasified, and the evaporated gas is pumped away by a vacuum system;

(5) the polymerization liquid after passing through the random packing passes through the gap between the hump supports, falls to the bottom of the concentration tower, and removes the residual monomers, bubbles and partial solvent in the polymerization liquid in the falling process;

(6) the polymerization liquid flows out from the discharge hole to finish the demonomerization, defoaming and concentration of the polymerization liquid.

7. The method for demonomerization, deaeration and concentration in the carbon fiber production process according to claim 6, characterized in that the spraying system uses a DCS control solenoid valve to realize intermittent start-up of the spraying system.

8. The method for demonomerization, defoamation and concentration in carbon fiber production process of claim 6, wherein the concentration of the polymerization solution is adjusted by adjusting the solvent supply amount of the reboiler.

9. The method for demonomerization, deaeration and concentration in carbon fiber production process according to claim 6, characterized in that the concentration of the polymerization solution is adjusted by adjusting the solvent supply amount of the spraying system.

Technical Field

The invention relates to a carbon fiber production method and equipment thereof, in particular to a method for demonomerization, deaeration and concentration in the carbon fiber production process and equipment thereof.

Background

In the production process of carbon fibers, the subsequent treatment of the polymerization solution is particularly critical, and particularly the control of demonomerization, defoaming and concentration directly influences the yield and quality of the precursor. The former equipment can not effectively solve the problems of concentration control of the polymerization liquid, whether the monomer is completely removed, whether bubbles are removed, internal glue formation and the like, seriously influences the uniformity of the polymerization liquid, and causes the product qualification rate of subsequent production to be low or even unqualified, so that the concentration tower plays a vital role in the whole production of the polymerization liquid.

In the carbon fiber industry, a single cylinder form is usually adopted to be directly connected with a vacuum pumping system, or a simple filling mode is adopted, the equipment form is not emphasized, the concentration of a polymerization liquid cannot be controlled, bubbles in the polymerization liquid cannot be removed completely, and the problem of glue formation on internal parts cannot be solved; due to the existence of equipment and process problems, the yield is low, the index of the polymerization solution is unstable, the production cost is greatly increased, and the modern production requirement cannot be met.

Disclosure of Invention

The invention provides a method and equipment for removing monomer, defoaming and concentrating in the production process of carbon fiber, which can conveniently control the concentration of a polymerization liquid, effectively remove monomer and bubbles in the polymerization liquid, limit the capacity and effectively avoid the gel generated by the equipment, aiming at the technical problems that the concentration of the polymerization liquid, the monomer and bubbles in the polymerization liquid cannot be effectively controlled in the existing carbon fiber production, and the gel is generated in the equipment.

Therefore, the invention adopts the technical scheme that the equipment for demonomerization, deaeration and concentration in the carbon fiber production process is provided with a concentration tower, the concentration tower comprises a cylinder body, an upper seal head and a lower seal head, the upper seal head is positioned above the cylinder body, the lower seal head is positioned below the cylinder body, the upper seal head is provided with a feed pipe, the feed pipe is connected with a discharge pipe, the discharge pipe is provided with a fixed flange and is fixed on the upper seal head through the fixed flange, the fixed flange is provided with a spray opening, the discharge pipe is provided with a material uniform distribution pipe, a uniform dispersion disc is further arranged in the cylinder body, a grid support is arranged below the uniform dispersion disc, filler is arranged below the grid support, hump supports are arranged below the filler, gaps are arranged among the hump supports, the lower part of the hump support is provided with a steam cylinder, and the steam cylinder is connected with a reboiler, the vacuum system is connected to barrel top, the low head bottom is equipped with the discharge gate.

Preferably, still be equipped with upper portion manhole, lower part manhole on the barrel, the lower part manhole is established on the barrel of filler department, be equipped with the closure plate on the manhole of lower part.

Preferably, the upper end enclosure is provided with an upper viewing mirror, the barrel below the hump support is provided with a lower viewing mirror, the upper portion of the feeding pipe is provided with an inspection hole, the lower end enclosure is provided with a thermometer socket, a sampling hole and a standby hole, and the thermometer socket is provided with a thermal resistance thermometer.

Preferably, three spraying ports are formed in each fixing flange, the spraying ports are connected with a spraying system, electromagnetic valves are arranged on the spraying system, and the spraying system is controlled to be opened and closed by a DCS.

Preferably, the material uniform distribution pipe is an annular material uniform distribution pipe, and the filler is random packing.

A method for demonomerization, deaeration and concentration in the production process of carbon fiber comprises the following steps:

(1) the polymer liquid enters the blanking pipe from the feeding pipe and flows onto the dispersion plate through the annular material distribution pipe on the blanking pipe, so that the polymer liquid is uniformly distributed, and a polymer liquid film is formed in the falling flowing process of the polymer liquid;

(2) the spraying system is intermittently started, the polymerization liquid in the concentration tower is sprayed diagonally through the spraying port, the concentration of the polymerization liquid is adjusted, and the part on the upper part in the cylinder body is prevented from being glued;

(3) the uniformly distributed polymerization liquid after passing through the dispersion plate falls on the random packing to form a thinner polymerization liquid film on the random packing, so that the polymerization liquid is fully contacted with the gas phase, and a large amount of monomers, bubbles and solvents are removed from the polymerization liquid;

(4) the reboiler conveys high-temperature gaseous solvent to the concentration tower through the steam drum, the temperature in the concentration tower is raised, the solvent and the monomer in the polymerization liquid are gasified, and the evaporated gas is pumped away by a vacuum system;

(5) the polymerization liquid after passing through the random packing passes through the gap between the hump supports, falls to the bottom of the concentration tower, and removes the residual monomers, bubbles and partial solvent in the polymerization liquid in the falling process;

(6) the polymerization liquid flows out from the discharge hole to finish the demonomerization, defoaming and concentration of the polymerization liquid.

Preferably, the spraying system adopts a DCS control electromagnetic valve to realize the intermittent starting of the spraying system.

Preferably, the concentration of the polymerization liquid is adjusted by adjusting the amount of the solvent supplied to the reboiler.

Preferably, the concentration of the polymerization solution is adjusted by adjusting the amount of solvent supplied to the spray system.

The beneficial effects of the invention are that,

(1) by arranging the spray opening, the polymerization liquid is sprayed diagonally by the spray system, so that the polymerization liquid can be effectively diluted, the concentration of the polymerization liquid can be adjusted, and the polymerization liquid can be placed in a barrel for the glue formation of parts, thereby realizing continuous production and improving the yield;

(2) through the falling process of the polymerization liquid and the uniform distribution on the random packing, the polymerization liquid is easy to form a film, the contact area of the polymerization liquid and the gas phase is increased, and the monomer, the bubbles and the solvent in the polymerization liquid can be removed easily;

(3) the reboiler heats the polymerization liquid in the film state, so that the contact area of the polymerization liquid and a gas phase can be further increased, the polymerization liquid and the gas phase are more uniform, monomers and partial solvent in the polymerization liquid are vaporized, the gaseous monomers and the gaseous solvent are pumped out of the concentration tower under the action of the vacuum system, and bubbles in the polymerization liquid in the film state are also removed;

(4) the device is provided with an upper manhole and a lower manhole for maintenance, a blocking plate is arranged at the lower manhole to prevent the aggregation of the polymerization liquid at the lower manhole, and the lower manhole can meet the maintenance requirement of random packing; the upper sight glass and the lower sight glass are used for observing the flowing condition of the polymerization liquid in the concentration tower and the state of internal structural parts;

(5) the problem of the glue formation of the structural member in the concentration tower is solved by configuring a spraying system, and the polymerization liquid is heated and the concentration can be adjusted by arranging a reboiler to input a gaseous solvent; the concentration of the polymerization liquid is further adjusted by setting a vacuum system to pump out vaporized gaseous substances and bubbles in the polymerization liquid; the structure is simple, the continuous production can be realized, the yield is increased, and the production cost is reduced.

Drawings

Fig. 1 is a schematic view of the overall structure of the embodiment of the present invention.

The symbols in the drawings illustrate that:

1. an upper end enclosure; 2. a fixed flange; 3. the annular materials are uniformly distributed; 4. a feed pipe; 5. an inspection opening; 6. a lower end enclosure; 7. a discharging pipe; 8. a spray port; 9. an upper sight glass; 10. a vacuum system connection port; 11. a barrel; 12. random packing; 13. supporting a hump; 14. a steam drum; 15. a reboiler connection port; 16. a thermometer socket; 17. a sampling port; 18. a discharge port; 19. a spare port; 20. a lower view mirror; 21. a lower manhole; 22. a blocking plate; 23. supporting the grids; 24. a uniform dispersion plate; 25. an upper manhole.

Detailed Description

The present invention will be further described with reference to the following examples.

As shown in figure 1, the equipment for demonomerization, defoamation and concentration in the carbon fiber production process is provided with a concentration tower, wherein the concentration tower comprises a cylinder body 11, an upper seal head 1 and a lower seal head 6, a uniform dispersion disc 24 is also arranged in the cylinder body 11, the uniform dispersion disc 24 is fixed on the cylinder body 11 through a grid support 23 below the uniform dispersion disc 24, random packing 12 is arranged below the grid support 23, and the surface roughness of the random packing 12 is less than or equal to 0.4 mu m. A hump support 13 is arranged below the random packing 12, a gap is arranged between the hump supports 13, a steam drum 14 is arranged at the lower part of the hump support 13, the steam drum 14 is processed into a semi-tubular form by a thick round tube, which is beneficial to the integral diffusion of steam, and the distance between the steam drum 14 and the lower part of the hump support 13 is 1 meter. The steam drum 14 is connected with a reboiler through a reboiler connecting port 15, the upper part of the drum body 11 is connected with a vacuum system connecting port 10, the vacuum system connecting port 10 is connected with a vacuum system, and the bottom of the lower end enclosure 6 is provided with a discharge port 18. The upper end enclosure 1 is located above the barrel body 11, the lower end enclosure 6 is located below the barrel body 11, the upper end enclosure 1 is provided with a feeding pipe 4, the feeding pipe 4 is connected with a discharging pipe 7, the discharging pipe 7 can be divided into 6 groups, 18 groups, 42 groups and the like, the initial design can be adjusted according to the capacity, and the number of the scattering disks 24 corresponds to that of the discharging pipes 7. Be equipped with annular material equipartition pipe 3 on unloading pipe 7, annular material equipartition pipe 3 is to material pipeline direction opening, be equipped with the pipeline on the unloading pipe 7, mounting flange 2, the loop flange, loop flange joint is on the pipeline that annular material equipartition pipe 3 draws, mainly for easy to assemble when daily maintenance of examining, unloading pipe 7 passes through mounting flange 2 to be fixed on upper cover 1, mounting flange 2 is inside to be equipped with and sprays the liquid runner way groove, be equipped with on mounting flange 2 and spray mouth 8, be equipped with three on every mounting flange 2 and spray mouth 8, spray mouth 8 and spraying system connection, the last solenoid valve that is equipped with of spraying system, spraying system adopts the switch of DCS control solenoid valve, realize spraying system's intermittent type start. The fixed flange 2 can be detached, and the spraying port 8 connected below the fixed flange 2 can be conveniently overhauled. The discharging pipe 7 adopts a sleeve structure, the inner part and the outer part of the discharging pipe are all polished to a mirror surface, the shape of the material scattering disk 24 is composed of a semicircle and a trapezoid, the semicircle is connected with the lower bottom of the trapezoid, the semicircle is horizontally arranged at 100mm under the discharging pipe 7, the upper bottom of the trapezoid points to the central axis of the cylinder body 11, and each material scattering disk 24 is provided with 3 small baffles to prevent the polymer liquid on the material scattering disk 24 from flowing unevenly.

The cylinder 11 is also provided with an upper manhole 25 and a lower manhole 21, the lower manhole 21 is arranged on the cylinder 11 at the filling position, and the lower manhole 21 is provided with a blocking plate 22. An upper sight glass 9 is arranged on the upper sealing head 1, a lower sight glass 20 is arranged on the barrel 11 below the hump support 13, an inspection opening 5 is arranged above the feeding pipe 4, a thermometer socket 16, a sampling opening 17 and a standby opening 19 are arranged on the lower sealing head 6, and a thermal resistance thermometer is arranged on the thermometer socket 16.

The inner surface of the concentration tower and the surfaces of parts are polished to mirror surfaces, so that the adhesion of the polymer liquid on the surfaces of the parts can be reduced, and the inner surface of the equipment can be kept from being glued in a production period under the spraying action of a spraying system.

The solvent in the spraying system has stable pressure, each electromagnetic valve switch is controlled through the DCS, the spray nozzles are controlled to spray, when in production, the opening time and the time interval of the DCS electromagnetic valves can be set according to the operation condition in the tower, 6 groups of spraying are arranged near the center, 12 groups are arranged on the second layer, 24 groups are arranged on the third layer, and the spraying system can be additionally designed according to the production capacity requirement.

A method for demonomerization, deaeration and concentration in the production process of carbon fiber comprises the following steps:

(1) the polymer liquid enters a discharging pipe 7 from a feeding pipe 4 and flows onto a dispersion disc 24 through an annular material homogenizing pipe 3 on the discharging pipe 7, so that the polymer liquid is uniformly distributed, and a polymer liquid film is formed in the process of falling and flowing;

(2) the spraying system is intermittently started, the polymerization liquid in the concentration tower is sprayed diagonally through the spraying port 8, the concentration of the polymerization liquid is adjusted, and structural parts at the upper part in the cylinder 11 are prevented from being caked;

(3) the uniformly distributed polymerization liquid after passing through the dispersion plate 24 falls on the random packing 12 to form a thinner polymerization liquid film on the random packing 12, so that the polymerization liquid is fully contacted with the gas phase, and a large amount of monomers, bubbles and solvents are removed from the polymerization liquid;

(4) the reboiler conveys high-temperature gaseous solvent to the concentration tower through the steam drum 14, the temperature in the concentration tower is raised, the solvent and the monomer in the polymerization liquid are gasified, and the evaporated gas is pumped away by a vacuum system;

(5) the polymerization liquid passing through the random packing 12 passes through the gap between the hump supports 13 and flows to the bottom of the concentration tower, and in the flowing process, the polymerization liquid flows in a linear shape, the lower part of the polymerization liquid is, the thinner the linear column of the polymerization liquid is, and the enough distance is left at the bottom of the hump support 13, namely, the residual monomer, bubbles and partial solvent in the polymerization liquid are removed;

(6) the polymerization liquid flows out from the discharge port 18, the demonomerization, the deaeration and the concentration of the polymerization liquid are completed, and the needed polymerization liquid can be produced by adjusting the operations of the solvent feeding amount in the reboiler, the vacuum degree in the concentration tower, the spraying amount of the spraying system and the like.

The spraying system can be divided into 6 groups, 18 groups or 42 groups and the like, the number of the spraying systems corresponds to that of the blanking pipes 7, and the spraying openings 8 are formed in the root parts of the positions, right below the fixed flanges 2, of the blanking pipes 7 and connected with nozzles. The mist solvent sprayed from the nozzle is sprayed to the upper part of the concentration tower and is used for diluting the polymerization liquid. Connect every mounting flange 2 and spray the outside pipeline of liquid and constitute by hose and electromagnetism ball valve, every solenoid valve all is connected to DCS, and entire system adopts DCS intermittent type formula control, makes the solvent that sprays in the concentration tower less, and can play the preferred effect, reduces the interior load of concentration tower and thermal consumption.

By arranging the spraying port 8, the polymerization liquid is sprayed diagonally through a spraying system, so that the polymerization liquid can be effectively diluted, the concentration of the polymerization liquid can be adjusted, and the polymerization liquid can be placed in the barrel 11 for the glue formation of parts, thereby realizing continuous production and improving the yield; through the falling process of the polymerization liquid and the uniform distribution on the random packing 12, the polymerization liquid is easy to form a film, the contact area of the polymerization liquid and the gas phase is increased, and the monomer, the bubbles and the solvent in the polymerization liquid can be removed easily; the reboiler heats the polymerization liquid in the film state, so that the contact area of the polymerization liquid and a gas phase can be further increased, the polymerization liquid and the gas phase are more uniform, monomers and partial solvent in the polymerization liquid are vaporized, the gaseous monomers and the gaseous solvent are pumped out of the concentration tower under the action of the vacuum system, and bubbles in the polymerization liquid in the film state are also removed; the device is provided with an upper manhole 25 and a lower manhole 21 for maintenance, a blocking plate 22 is arranged at the lower manhole 21 to prevent the aggregation of the polymerization liquid at the lower manhole 21, and the lower manhole 21 can meet the maintenance requirement of the random packing 12; the upper sight glass 9 and the lower sight glass 20 are used for observing the flowing condition of the polymerization liquid in the concentration tower and the state of internal structural parts; the problem of the glue formation of the structural member in the concentration tower is solved by configuring a spraying system, and the polymerization liquid is heated and the concentration can be adjusted by arranging a reboiler to input a gaseous solvent; the concentration of the polymerization liquid is further adjusted by setting a vacuum system to pump out vaporized gaseous substances and bubbles in the polymerization liquid; the structure is simple, the continuous production can be realized, the yield is increased, and the production cost is reduced.

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.