CN212269951U - High-viscosity high-strength nylon-666 copolymerization polymerization continuous polymerization device - Google Patents
High-viscosity high-strength nylon-666 copolymerization polymerization continuous polymerization device Download PDFInfo
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Abstract
A high-viscosity high-strength nylon-666 copolymerization polymerization continuous polymerization device sequentially comprises a caprolactam salt feeding device (1), a high-pressure cracker (2), a prepolymerization reactor (3), a front polymerization reactor (4), a rear polymerization reactor (5), a granulating device (6), a slice water mixing tank (7), an extraction device (8), a centrifugal dehydrator (9), a drying device (10) and a slice conveying and packaging device (11), wherein the extraction device (8) is also connected with an extraction water recovery device (12), and the extraction water recovery device (12) comprises a primary-effect heater, a primary-effect evaporation tower, a secondary-effect heater, a secondary-effect evaporation tower, a tertiary-effect heater, a tertiary-effect evaporation tower, a quaternary-effect steam-water separator, a quaternary-effect heater and a concentrated solution dehydration tank which are sequentially connected; the single-station operation of the extraction rotary discharger and the drying rotary discharger is realized, and the equipment investment is saved.
Description
Technical Field
The utility model relates to a nylon-666 copolymerization polymerization apparatus for producing technical field, concretely relates to high viscosity high strength nylon-666 copolymerization polymerization continuous polymerization device.
Background
The nylon 666 copolymerization chip which is an important member of a synthetic fiber family, the upstream raw material is the nylon-666 chip which is formed by the copolymerization of caprolactam, hexamethylene diamine and adipic acid, the technology is only produced by a nylon 6 polymerization device at home, and is not produced by a standard production device, and the production plant can be low and is not produced in scale.
Disclosure of Invention
In order to solve the technical defects existing in the prior art, the utility model provides a high-viscosity high-strength nylon-666 copolymerization polymerization continuous polymerization device.
The utility model discloses a technical solution be: the utility model provides a high viscosity high strength nylon-666 copolymerization polymerization device in succession includes caprolactam salt feed arrangement, high pressure cracker, prepolymerization reactor, preceding polymerization reactor, postpolymerization reactor, cuts grain device, section water blending tank, extraction device, centrifugal dehydrator, drying device, section transport packing apparatus, extraction device on still be connected with extraction water recovery unit, extraction water recovery unit including consecutive one imitate the heater and imitate the evaporating tower, two imitate the heater and two imitate evaporating tower, three imitate heater and three imitate evaporating tower, four imitate catch water and four imitate heater and concentrate dewatering tank.
The first-effect evaporation tower, the second-effect evaporation tower, the third-effect evaporation tower and the fourth-effect steam-water separator are respectively provided with a first-effect concentrated solution circulating pump, a second-effect concentrated solution circulating pump, a third-effect concentrated solution circulating pump and a fourth-effect concentrated solution circulating pump. And a concentrated solution discharge pump and a four-effect regulating valve are arranged between the four-effect steam-water separator and the concentrated solution dewatering tank. Concentrated solution is completely recovered and is evaporated through MVR four-effect, and the concentrated solution enters a pre-dehydration reactor after high-pressure hydrolysis reaction, so that the water content of the material entering the pre-dehydration reactor can reach less than 25%.
A melt pump is arranged between the front polymerization reactor and the rear polymerization reactor.
And a casting belt pump is arranged between the post polymerization reactor and the granulating device.
The caprolactam salt feeding device comprises a caprolactam salt water solution storage tank, a caprolactam salt heater, a flash tank and a caprolactam fine filter in sequence.
The extraction device comprises a pre-extraction water tank, an extraction water storage tank and an extraction tower in sequence, wherein a rotary discharger and a slice cement slurry pump are arranged at the bottom of the extraction tower.
Drying device include drying tower and nitrogen gas dehydrating unit, the top of drying tower be equipped with the cyclone of interception section particle, nitrogen gas dehydrating unit include nitrogen gas washing tower, nitrogen gas washing water pump, nitrogen gas washing cooler to and nitrogen gas washing water filter.
The utility model has the advantages that: the utility model provides a high viscosity high strength nylon-666 copolymerization polymerization continuous polymerization device has realized that the caprolactam feeding adopts high pressure feeding single platform operation, has realized that the three-section polymerization comes the operation, has realized that the prepolymerization adopts high temperature high pressure to come the operation, and the high temperature high nitrogen flow that has realized the drying tower comes the operation, has realized section conveying system's single line operation, has realized the single platform operation of extraction rotatory discharger, dry rotatory discharger, has saved the equipment investment.
Drawings
Fig. 1 is a schematic view of the device of the present invention.
The method comprises the following steps of 1-caprolactam salt feeding device, 2-high-pressure cracker, 3-prepolymerization reactor, 4-front polymerization reactor, 5-rear polymerization reactor, 6-granulating device, 7-slice water mixing tank, 8-extraction device, 9-centrifugal dehydrator, 10-drying device, 11-slice conveying and packing device, 12-extraction water recovery device, 13-melt pump and 14-casting belt pump.
Detailed Description
Now, the utility model discloses it is further explained with reference to fig. 1, a high viscosity high strength nylon-666 copolymerization polymerization continuous polymerization device includes caprolactam salt feed arrangement 1, high pressure cracker 2, prepolymerization reactor 3, preceding polymerization reactor 4, postpolymerization reactor 5 in proper order, cuts grain device 6, section water blending tank 7, extraction plant 8, centrifugal dehydrator 9, drying device 10, section transport packing apparatus 11, extraction plant 8 on still be connected with extraction water recovery unit 12, extraction water recovery unit 12 including consecutive one imitate heater and one imitate the evaporating tower, two imitate heater and two imitate the evaporating tower, three imitate heater and three imitate the evaporating tower, four imitate catch water and four imitate heater and concentrate dehydration jar. The first-effect evaporation tower, the second-effect evaporation tower, the third-effect evaporation tower and the fourth-effect steam-water separator are respectively provided with a first-effect concentrated solution circulating pump, a second-effect concentrated solution circulating pump, a third-effect concentrated solution circulating pump and a fourth-effect concentrated solution circulating pump. And a concentrated solution discharge pump and a four-effect regulating valve are arranged between the four-effect steam-water separator and the concentrated solution dewatering tank.
A melt pump 13 is arranged between the front polymerization reactor 4 and the rear polymerization reactor 5.
A casting belt pump 14 is arranged between the post-polymerization reactor 5 and the granulating device 6.
The caprolactam salt feeding device 1 sequentially comprises a caprolactam salt water solution storage tank, a caprolactam salt heater, a flash tank and a caprolactam fine filter. And (3) delivering the purchased 50%66 saline solution into a 66 saline solution storage tank through an unloading pump, filtering the solution through a 66 saline discharge pump, continuously delivering the solution to a 66 saline heater, and repeatedly and circularly concentrating the solution through a 66 saline circulating pump and a flash tank to ensure that the concentration of the 66 saline solution is concentrated to 80 Wt%. Liquid caprolactam from the plant is continuously conveyed into a caprolactam storage tank after being filtered through a caprolactam filter, and the storage capacity of the caprolactam storage tank is designed to be the consumption required when the caprolactam storage tank is continuously operated at a rated capacity of 110% for 48 hours. All pipelines of the caprolactam conveying and storing tanks are heated by hot water at 90-92 ℃. The caprolactam in the storage tank is filtered by a caprolactam circulating pump through a caprolactam fine filter, and then the filtered caprolactam is partially conveyed to a subsequent working section: caprolactam and 66 salt concentrated solution compounding area.
The extraction device 8 comprises a pre-extraction water tank, an extraction water storage tank and an extraction tower in sequence, and a rotary discharger and a slice cement slurry pump are arranged at the bottom of the extraction tower.
High-pressure cracker
Concentrated solution dehydration tanks (caprolactam and oligomers) from an MVR extraction water recovery section are conveyed by a special multi-head diaphragm pump, preheated and then enter a high-pressure cracker, the oligomers in the high-pressure cracker are cracked to ensure that the oligomers can be used for the production of subsequent high-end products, and cracked mixtures are continuously conveyed to a special mixing device in front of a prepolymerizer by a cracking solution discharge regulating valve.
Prepolymerization reactor
The caprolactam and 66 salt concentrated solution compound liquid from a caprolactam intermediate storage tank is conveyed by a prepolymerization feeding pump, preheated by a preheater and conveyed into a mixer, wherein the caprolactam and 66 salt concentrated solution compound liquid and a hexamethylenediamine auxiliary agent are uniformly and quantitatively mixed in a special mixer in proportion, then mixed with a recovered mixture from a cracker in another special mixing device, enter a prepolymerization reactor, and then the feeding amount of the caprolactam and 66 salt concentrated solution compound liquid into the prepolymerization reactor is automatically controlled by the liquid level of the prepolymerization reactor.
The process design of the prepolymerization reactor is a pressurized reactor and stably operates in the range of designed yield of 70-110%, and in order to stabilize the pressure of the prepolymerization reactor, a prepolymerization packing tower and a pressure regulating valve are arranged at the top of the prepolymerization reactor; the residence time of the materials in the prepolymerization reactor ensures the ring-opening reaction and the polyaddition reaction; a sufficient equilibrium is reached already under the corresponding process conditions.
The prepolymer was conveyed to the prepolymer melt dryer via a melt discharge pump. In the prepolymer melt dryer, the majority of the water in the reaction mixture is separated into the gas phase and is fed together with the prepolymer melt to the prepolymerization reactor, where the pressure may reach 16-40 bar.
Pre-polymerization reactor
The prepolymer containing a large amount of water in the prepolymerization reactor is conveyed to a prepolymerization melt dryer through a melt discharge pump, and most of water is separated through a front polymerization packed tower at the top of the polymerization reactor before entering the front polymerization reactor, so that the polymerization reaction is continuously and rapidly pushed forward. The pressure in the pre-polymerization reactor was controlled to 6-10 bar.
Postpolymerization reactor
The melt from the front polymerization reactor is conveyed by a front polymerization discharge gear pump, passes through a front polymerization dryer and enters a rear polymerization reactor, excessive water is separated from the melt in the front polymerization dryer and is mixed with protective nitrogen in a rear polymerization packed tower at the top of the rear polymerization reactor due to pressure change, the mixture is cooled and then enters a rear polymerization condenser together to be cooled, and then enters a rear polymerization water-sealed tank, and the low-molecular raw material carried by water is condensed in the rear polymerization packed tower and flows back to enter the rear polymerization reactor. The post-polymerization reactor operates under normal pressure and is protected by nitrogen, and the post-polymerization reactor can be divided into four stages, and each stage is provided with corresponding special internal components to ensure that the polymerization melt is completely kept uniformly and stably distributed on the process. The process design of the residence time ensures that the corresponding polyaddition and polycondensation reactions are sufficiently balanced in the different output ranges (70-110%).
Grain cutting device
The production line is cut grain and is used a set of Germany BKG underwater pelleter UGW-AH4000, the melt is conveyed to a melt reversing valve through a rear poly gear pump, and the polymer melt enters a grain cutting chamber filled with water through a template hole forming melt strip under the thrust action. The cutter immediately cuts the melt strand that passes through the die plate into pellets. Since the temperature difference between the melt and water is large, the melt which is cut into pellets solidifies immediately and forms spherical sphericity peculiar to underwater pellets, depending on the viscosity of the product. From the pelletizing chamber, the mixture of pellets and water is separated from the pellets once it enters the pellet dryer. Due to the high speed rotation of the rotor, plus the angle of the rotor blades, the particles are transported spirally upward. Because the dryer screen was installed, the pellets stayed in the dryer rotor until reaching the top and exited the pellet outlet of the dryer. The blower forms a convection air stream through the pelletizing outlet; the rotating speed of the blower motor can be adjusted through the frequency converter, and the air convection is adjusted to achieve the optimal drying effect. Convective air flow and centrifugal dryers can minimize the moisture content of the particles at the dryer exit. The water content of the particles at the outlet of the dryer is related to the polymer type and the hygroscopicity of the material, and can reach 0.02 to 0.3 percent. To clean the equipment, the dryer is fitted with two gates to provide easy access to the internal components. To prevent the door from being opened while the dryer is operating, the dryer is equipped with a safety interlock key.
Separated from the process water in a centrifugal dryer. The pellets continuously pass through and exit the dryer while process water flows out, is filtered, regulated to process temperature and pumped back to the pellet chamber. Water treatment systems are generally a compact unit mounted on a floor, the main parts of which comprise: the water tank, the polygonal rotary water filter, the process water pump, the water flow meter, the centrifugal dryer, the fan, the heat exchanger and the internal piping, after the slices are separated from the water, the overlong unqualified slices in the slices are separated by the screen, and the qualified slices enter the collection tank through the screen.
After the particles are separated from the process water, the process water enters the water tank and is filtered by a rotary filter in the water tank. The water pump pumps the process water out of the tank through the plate heat exchanger where it is cooled as required. During production, the temperature of the process water is measured downstream of the heat exchanger. An electronic servo valve is installed at the inlet and outlet of the cooling water of the heat exchanger to control the flow rate of the cooling water, thereby regulating the temperature of the process water. Before starting the vehicle, the temperature of the process water is measured in a water tank, a heater is arranged in the water tank, the process water is heated as required before production, and then the process water is converted and measured in the production process of the water temperature at the downstream heat exchanger. The water level of the water tank is detected by a sensor to ensure an optimum water level. When the process water flows out of the water treatment system, the magnetic induction type sensor measures the process water flow.
The continuous water filter is suitable for production of easily produced large amount of powder and functions as follows: the process water from the centrifugal dryer enters a water filtration device which consists of a rotary drum and a screen plate. The water level within the drum is monitored.
When the water level rises, the rotary drum starts to rotate, so that the clean filter screen plate is positioned at the process water flow. At the same time, the water sprayed from the nozzle flushes the dirty filter screen plate, the powder/pollutant falls into a groove and then flushes to the belt filter, and the filter belt automatically conveys the powder/impurity out of the system.
Extraction device
The monomers and oligomers in the PA6/66 slice are extracted and removed by hot water countercurrent in an extraction tower.
PA6/66 slices from the long-strip separator enter a pre-extraction water tank, overflow water of the pre-extraction water tank enters an extraction water storage tank of a recovery system through an overflow pipeline, the pre-extraction water tank is conveyed to a slice separator through a pre-extraction rotary discharging device and a slice cement slurry pump and enters an extraction tower, and extraction water and extraction tower overflow water separated by the slice separator return to a pre-extraction degassing tank through the overflow pipeline and enter the pre-extraction water tank. The extraction water with certain amount and high concentration from the top of the extraction enters from the bottom of the pre-extraction water tank to carry out convection extraction with the slices, a water circulation is arranged in the middle of the pre-extraction water tank, the extraction water at the upper part enters a pre-extraction circulating water pump after coming out, dust is filtered out by a pre-extraction water filter, and the extraction water enters the pre-extraction water tank after being heated by a pre-extraction circulating water heater.
The extracted slices are automatically controlled by the bottom of the extraction tower according to the liquid level and are conveyed to a dehydrator to enter a subsequent drying section through an extraction rotary discharger and a slice cement slurry pump, and conveying water is sent back for recycling.
The extraction tower is provided with a water supplementing system and a circulating water path, wherein the water supplementing system supplements condensed water from the MVR recovery system to the extraction water immersion tank according to the process requirement; one circulation is that the water is pressurized by a bottom extraction water delivery pump at the outlet of the extraction water immersion tank, the bottom extraction water filter filters the water, the extraction water enters the lower part of the extraction tower after being heated by a heater at the bottom of the extraction water to participate in extraction and slice delivery, and a heated circulating water system ensures the stability of concentration gradient and temperature gradient in the tower.
Drying device
The extracted slice is automatically controlled by the bottom of the extraction tower according to the liquid level, conveyed to a dehydrator to enter a drying tower through an extraction rotary discharger and a slice cement slurry pump, and slowly moves downwards from the top of the drying tower to be dried by the hot nitrogen flowing upwards in a counter-current manner. And cooling the dried slices at the lower part of the drying tower, and then sending the slices to a packaging machine for packaging.
In the drying system, a cyclone dust removal device is arranged at the top outlet of nitrogen of the drying tower to intercept the slice particles, the nitrogen on the upper part of the drying tower is sent to a nitrogen washing tower for dehumidification and then enters a nitrogen purifier for deoxidization, and then is pressurized by a second-stage drying circulating fan and enters a second-stage nitrogen heater, the second-stage nitrogen heater heats the nitrogen and then enters the lower part of the drying tower, and the moisture in the slices of the drying tower is removed through the continuous circulation of the nitrogen.
The nitrogen dehumidification system comprises a nitrogen washing tower, a nitrogen washing water pump, a nitrogen washing cooler and a nitrogen washing water filter.
The dried slices are conveyed to a slice cooling bin by a drying rotary discharging device at the bottom of the drying tower to be sliced, and are pneumatically conveyed to a slice packaging bin through the slices after being cooled by a cooling section nitrogen circulating fan.
Slice conveying and packing device
Pneumatic conveying of slices is achieved through nitrogen circulation, cooling slices from a cooler below a drying tower are conveyed to a slice bin through a slice conveying system through a rotary valve, and finally the slices are converted into an intermediate bin to be packed through a packing system.
The conveying capacity of the slices can be adjusted according to the yield, the designed conveying capacity is 4500Kg/h,
the slices enter a packaging system and can be packaged into a small packet of 25Kg and a large packet of 750Kg or 800Kg according to market demands.
MVR extraction water recovery unit
The MVR evaporation process can greatly reduce the consumption of steam and energy consumption, the steam consumption of each ton of PA6/66 slices is reduced by 0.5 ton compared with the conventional triple-effect evaporation, and the total energy consumption of a recovery system is saved by 1.5 times compared with the conventional triple-effect evaporation.
The secondary steam of the two-effect separator is compressed by a compressor and then is supplied to the first-effect evaporator and the third-effect evaporator; the secondary steam generated by the first-effect separator is supplied to the second-effect evaporator, so that the energy is saved by cyclic utilization.
The first-effect separator and the second-effect separator are internally provided with special internal components, when steam passes through the internal components, the steam is washed cleanly, and the monomer content is only about 300PPM, so that the effects of recycling and environmental protection are achieved.
After the extraction water from the extraction water storage tank is filtered by an extraction water feeding circulating pump and an extraction water filter and then is preheated by a recovered water heater to enter a first-effect heater and a first-effect evaporation tower to establish a normal liquid level, starting the first-effect circulating pump for circulation and feeding the extraction water to a second-effect heater, a third-effect heater and a second/third-effect evaporation tower through a first-effect to second-effect regulating valve to establish a normal liquid level; sequentially starting a two-effect circulating pump and a three-effect concentrated solution circulating pump for circulation; after the four-effect steam-water separator and the four-effect heater are fed with materials through the three-effect to three-effect regulating valve to establish a normal liquid level, the four-effect concentrated liquid circulating pump is started; slowly providing fresh steam for the four-effect heater to heat so that the four effects start to evaporate; starting a steam compressor to keep the evaporation liquid level of each effect to a set value; the liquid level of each effect is switched from manual control to automatic control.
And after the four-effect concentration reaches the target control concentration, starting a concentrated solution discharge pump and a four-effect regulating valve to continuously feed the concentrated solution to a concentrated solution dehydration tank.
In the description of the present invention, it should be noted that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for convenience of description and simplification of the description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art. In addition, in the description of the present invention, "a plurality" means two or more unless otherwise specified.
The skilled person should understand that: although the present invention has been described in accordance with the above embodiments, the inventive concept is not limited to this embodiment, and any modification of the inventive concept will be included in the scope of the patent claims.
It is above only the utility model discloses a preferred embodiment, the utility model discloses a scope of protection does not only confine above-mentioned embodiment, the all belongs to the utility model discloses a technical scheme under the thinking all belongs to the utility model discloses a scope of protection. It should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The utility model provides a high viscosity high strength nylon-666 copolymerization polymerization continuous polymerization device, its characterized in that includes caprolactam salt feed arrangement (1), high pressure cracker (2), prepolymerization reactor (3), preceding polymerization reactor (4), postpolymerization reactor (5), cuts grain device (6), section water blending tank (7), extraction plant (8), centrifugal dehydrator (9), drying device (10), section transport packing apparatus (11), extraction plant (8) on still be connected with extraction water recovery unit (12), extraction water recovery unit (12) including consecutive one imitate heater and one imitate the evaporating tower, two imitate heater and two imitate the evaporating tower, three imitate heater and three imitate the evaporating tower, four imitate catch water and four imitate heater and concentrate dehydration jar.
2. The continuous polymerization device for the copolymerization and polymerization of high viscosity and high strength nylon-666 as claimed in claim 1, wherein the single-effect evaporation tower, the double-effect evaporation tower, the triple-effect evaporation tower and the four-effect steam-water separator are respectively provided with a single-effect concentrated solution circulating pump, a double-effect concentrated solution circulating pump, a triple-effect concentrated solution circulating pump and a four-effect concentrated solution circulating pump.
3. The continuous polymerization device for the copolymerization and the polymerization of the nylon-666 with high viscosity and high strength as claimed in claim 1, wherein a concentrate discharge pump and a four-effect regulating valve are arranged between the four-effect steam-water separator and the concentrate dehydration tank.
4. The continuous polymerization device for the copolymerization of high viscosity and high strength nylon-666 as claimed in claim 1, wherein a melt pump (13) is provided between the pre-polymerization reactor (4) and the post-polymerization reactor (5).
5. The continuous polymerization device for the copolymerization of high viscosity and high strength nylon-666 as claimed in claim 1, wherein a belt casting pump (14) is provided between the post-polymerization reactor (5) and the pelletizing device (6).
6. The continuous polymerization device for high viscosity and high strength nylon-666 copolymerization polymerization as claimed in claim 1, wherein the caprolactam salt feeding device (1) comprises a caprolactam salt solution storage tank, a caprolactam salt heater, a flash tank and a caprolactam fine filter in sequence.
7. The continuous polymerization device for high viscosity and high strength nylon-666 copolymerization polymerization as claimed in claim 1, wherein the extraction device (8) comprises a pre-extraction water tank, an extraction water storage tank and an extraction tower in sequence, and the bottom of the extraction tower is provided with a rotary discharger and a slice cement slurry pump.
8. The continuous polymerization device of high viscosity and high strength nylon-666 copolymerization polymerization as claimed in claim 1, wherein the drying device (10) comprises a drying tower and a nitrogen gas dehumidifying device, the top of the drying tower is provided with a cyclone dust collector for intercepting the particles of the slices, and the nitrogen gas dehumidifying device comprises a nitrogen gas washing tower, a nitrogen gas washing water pump, a nitrogen gas washing cooler and a nitrogen gas washing water filter.
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| CN111763314A (en) * | 2020-08-17 | 2020-10-13 | 温州邦鹿化工有限公司 | High-viscosity high-strength nylon-666 copolymerization polymerization continuous polymerization device |
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