WO2018127034A1

WO2018127034A1 - Non-stirred reactor, non-stirred pta aging crystallization device, and process and method thereof

Info

Publication number: WO2018127034A1
Application number: PCT/CN2018/070004
Authority: WO
Inventors: 汪英枝; 姚瑞奎
Original assignee: 中国昆仑工程有限公司
Priority date: 2017-01-05
Filing date: 2018-01-02
Publication date: 2018-07-12
Also published as: CN106669581A

Abstract

The present invention relates to a non-stirred reactor and a reaction process thereof, and also relates to a PTA aging crystallization device using the non-stirred reactor and an aging crystallization method thereof. A first inlet, a second inlet, a first outlet, and a second outlet are provided on a housing of the reactor, in which both the first inlet and the second inlet are lateral inlets, respectively arranged at an upper portion and a lower portion of the reactor housing, and the first outlet and the second outlet are respectively arranged at a central outlet and a top outlet of the reactor. The non-stirred reactor relies on steam bubbles and kinetic energy generated from a pressure drop to realize the stirring and suspension of a slurry, thereby reducing the manufacturing and maintenance costs of the reactor and the PTA aging crystallization device.

Description

Stirred reactor without stirring, PTA ripening crystallization device and process method thereof

Technical field

The invention relates to a non-stirred reactor mainly used for chemical production, a non-stirred PTA curing crystallization device and a process method using the same, and belongs to the technical field of chemical industry.

Background technique

The reactor is a common equipment for chemical production. Usually, a stirrer is needed to stir the materials to achieve the mixing and mass transfer required for the reaction. In the prior art, a reactor is provided in the reactors of oxidation, ripening and crystallization, and the slurry in the reactor is stirred and stirred by the blades to realize mass transfer, heat transfer and suspension of the solid particles in the reactor. The bottom is deposited. For example, an oxidation crystallizer (secondary or tertiary crystallization) in a purified terephthalic acid (PTA) industry and a refining unit crystallizer (four or five crystallization), terephthalic acid (TA) flowing through the above equipment. The slurry concentration is very high. In the case of static state or insufficient stirring strength, the solids in the slurry are easily deposited, causing blockage of equipment or pipelines and affecting the continuous production of the device. Therefore, it is necessary to stir the slurry with a stirrer to make the slurry The material is in a mixed state, and the solid suspension does not deposit. Although the setting of the agitator can meet the production requirements, it has a high cost in terms of cost and energy consumption, especially since the solvent in the PTA slurry is acetic acid, which is highly corrosive, and the device body usually adopts composite titanium material. The thickness of the titanium material is only 2-3mm, and the stirrer needs all titanium material, so the price of the equipment body and the agitator is roughly equivalent, which leads to a substantial increase in equipment cost. In addition, the stirrer needs to be driven by a motor. The energy consumption is very high, the agitator itself is a mechanical transmission device, and sometimes mechanical failure occurs.

In addition to the mechanical agitator described above, airflow agitation is also employed in some reactors. Air or other gas having a certain pressure enters the reactor, and a swirling flow is formed by the swirling air distributor, thereby agitating the liquid in the reactor. The energy used for agitation is derived from the kinetic energy produced by the input gas, which requires a large enough gas flow compared to mechanical agitation. For this reason, airflow agitation has only been used for a small number of special occasions.

For a long time, it has been thought that when PTA ripening and crystallization are involved in slurry containing solid particles, mechanical agitation must be used. The existing domestic and foreign PTA production maturation reactors and crystallization reactors are equipped with mechanical agitation without exception. The slurry is stirred and mixed by means of a mechanical stirrer.

Summary of the invention

In order to overcome the above-mentioned drawbacks of the prior art, the present invention provides a non-stirred reactor and a corresponding non-stirring reaction process, and also provides a non-stirred PTA curing crystallization apparatus using the non-stirred reactor and corresponding no Stirring PTA ripening crystallization method, no mechanical stirrer is provided in the non-stirred reactor, and the external input gas does not need to reach the extent that the slurry can be sufficiently stirred, and all of the non-stirred PTA ripening crystallization device is used for aging and crystallization. The reactor adopts the above-mentioned non-stirred reactor and the above-mentioned non-stirring reaction process, and these apparatuses and methods are suitable for the reaction containing the solid slurry, without the need of providing a mechanical agitator, and without the external input gas having sufficient stirring ability, thereby Significantly save the manufacturing cost and maintenance cost of the reactor and PTA curing crystallization unit, and greatly reduce the power consumption and production cost of related chemical production.

The technical solution adopted by the present invention is: a non-stirred reactor suitable for containing a solid slurry, comprising a reactor casing, wherein the reactor casing is not provided with a mechanical agitator, and the reactor casing is provided with a first inlet, a second inlet, a first outlet, and a second outlet, the first inlet being a lateral inlet, disposed at an upper portion of the reactor housing, and the second inlet being a lateral inlet, the reactor being disposed At the lower portion of the housing, the first outlet is a bottom outlet, disposed at the center of the bottom of the reactor, and the second outlet is a top outlet disposed at the top of the reactor housing.

A non-stirring reaction process suitable for containing a solid slurry, the reaction is carried out by using any of the non-stirred reactors disclosed in the present invention, and the slurry for reaction is fed from the first inlet of the reactor, from the second The inlet is fed to the gas or slurry for the reaction, the post-reaction slurry is output from the first outlet, the post-reaction gas (generally referred to as tail gas) is discharged from the second outlet, and the material (gas or slurry) fed by the second inlet is fed. The pushing of the material or the mutual pushing of the materials fed by the first inlet and the second inlet forms a swirling flow in the reactor, and the operating pressure (pressure, the same below) in the reactor is lower than the feeding pressure of the slurry. Part of the slurry component is converted into a gas phase (vapor) by decompression, and continuously forms vapor bubbles (or evaporating bubbles) throughout the slurry, and the slurry is stirred, or is mixed by a bubble or by a bubble agitation and a slurry swirling action. The solid material in the slurry is in a suspended fully mixed state to prevent solid particles in the slurry from depositing at the bottom of the reactor.

An agitated PTA ripening crystallization apparatus comprising a sequentially connected maturation reactor and a crystallization reactor, the number of the maturation reactors being one or more, the number of the crystallization reactors being one or more, the maturation The reactor adopts any of the non-stirred reactors disclosed in the present invention, and the crystallization reactor adopts any of the non-stirred reactors disclosed in the present invention, and when the number of the ripening reactors is plural, the plurality of reactors The maturation reactor may adopt the same non-stirred reactor, or different non-stirred reactors may be used. When the number of the crystallization reactors is plural, the plurality of crystallization reactors may adopt the same The non-stirred reactor may also adopt different said non-stirred reactors, and the first outlets of any of the pre-reactors (including the maturation reactor and the crystallization reactor) should be connected to the adjacent post-reactor An inlet may also be connected or not connected to the second inlet of the adjacent subsequent reactor.

The invention relates to a method for aging crystallization without stirring, and the aging and crystallization of the slurry after oxidation is carried out by using any non-stirred PTA aging crystallization device disclosed in the present invention, and the maturation reactor adopts any non-stirring reaction process disclosed in the present invention. The crystallization reactor also adopts any non-stirring reaction process disclosed in the present invention. When the number of the maturation reactors is plural, the plurality of maturation reactors may adopt the same non-stirring reaction process, Different said agitation-free reaction processes may be employed. When the number of the crystallization reactors is plural, the plurality of crystallization reactors may employ the same agitation-free reaction process or a different agitation-free reaction process.

The invention has the beneficial effects of overcoming the technical prejudation that the suspended solid slurry has to be mechanically stirred for a long time, and creatively utilizes the vapor bubbles generated throughout the system under reduced pressure and the temperature drop between the front and rear equipments. The generated kinetic energy achieves an effective and reliable slurry mixing without any dead angle, and uses the system heat energy as a source of energy for the mixing, thereby saving the huge power consumption required for mechanical stirring and saving the mechanical setting. The huge equipment manufacturing cost required by the agitator can also be used to form the kinetic energy of the swirling flow by using the feed pressure, and the potential energy of the system can be used as the energy source of the swirling flow, further ensuring and enhancing the mixing effect, especially mixing with the air bubbles. The action is coordinated to effectively avoid the deposition of solid particles at the bottom of the reactor. According to the applicant's test, in the PTA crystallization process involving high concentration slurry, the final stage crystallization reactor (two crystals) is not exposed to external gases. In this case, effective mixing can still be achieved, and according to the prior art or in the long-term concept of people, this A large number of high-concentration slurry of the solid particles, can not use only airflow stirring, even with mechanical stirring, can also require a lot of power adds.

Since the vapor bubbles generated by the pressure reduction are spread over all areas of the slurry, the problem of poor local agitation or mechanical deadness under mechanical agitation is completely avoided; since the bubbles are moved upwards, the collision and breakage occur during the movement. And polymerization, the higher the gas volume, the better the stirring effect. Therefore, compared with the mechanical agitator, it is allowed to adopt a tower reactor with a higher or higher aspect ratio, which can significantly reduce the floor space and lengthen the slurry. The path is also beneficial to the sufficient contact and mass transfer of different reactants. In the case of the same reaction requirements, it is beneficial to reduce the volume of the reactor; since the lateral material inlet is provided, and because the lateral material inlet is at least The upper and lower two are not only beneficial to use the feed momentum to push the slurry in the reactor to form and maintain the swirling state, but also can promote the formation of the slurry in the reactor by the synergistic pushing of the upper and lower inlets. The swirling state, according to the applicant's experiment, in the same situation under other circumstances, the effect of the up and down feeding together to promote the swirl is significantly better than the single The effect of the lower feed is more obvious than the effect of feeding from the top alone. At the same time, in the case of feed including gas and slurry, it can be formed from the lower part, the upper part (slurry), gas and liquid. The reverse flow is beneficial to improve the mass transfer and reaction effect, and is beneficial to the use of bubbles formed by the intake air to enhance the mixing effect, enhance the bubble mixing effect, and compensate for the relatively small defects of the evaporation bubbles at the bottom of the reactor; The discharge port is preferably located at the center of the bottom, which not only realizes the reverse flow of the slurry and the bubble, but also helps to strengthen the swirling state at the bottom of the reactor, prevents the discharge flow from disturbing the swirl flow, and prevents the local swirl flow rate from falling, preventing the flow. The swirling dead angle occurs, and since the bottom head (lower head) of the reactor can usually be in the shape of a spherical shape, an ellipsoidal shape or the like, the diameter is gradually reduced and there is no dead zone, and the slurry flows downward, and the rotation speed is particularly close. The faster the line speed of the inner surface, the stronger the flushing effect on the inner surface of the reactor, and the same direction of swirling flow formed by the swirling direction of the slurry and the grounding biasing force. Under the condition that no energy is consumed, the swirling speed and the scouring action can be further enhanced by the action of the grounding biasing force, thereby ensuring that the bottom air bubble is small and still capable of generating sufficient mixing effect and effectively avoiding The deposition of solid particles at the bottom.

The non-stirring reaction process and the non-stirring reaction apparatus of the present invention are suitable for the processes of oxidation, ripening and crystallization in the production of PTA. Especially for the PTA curing and crystallization process, it has been generally believed that effective gas flow agitation cannot be achieved regardless of the pressure and flow rate of the external input, and it is effective without increasing the flow rate of the reaction gas or even inputting any gas. The airflow is even more unimaginable. The applicant found that in the above reaction, taking into account the combination of air suspension and slurry flow mixing, the solid suspension in the slurry in the reactor can be prevented from being deposited, and the material is in a fully mixed state, even at the bottom of the equipment, the material It is also in a turbulent mixing state, and solid deposit clogging does not occur, thereby achieving agitator-free operation.

According to the same mechanism, the present invention is also applicable to other similar production processes or production units involved in suspension slurries and depressurization and cooling processes in the chemical industry.

For the one-tonnage deep oxidation PTA plant, after the invention is used, only mechanical agitation is eliminated in the maturation, crystallization and RPF feed tanks, which can reduce the investment by about 40% and reduce the power consumption by about 1000 kW. considerable.

DRAWINGS

1 is a flow chart of a non-stirred PTA ripening crystallization process according to the present invention.

detailed description

Referring to FIG. 1, the present invention is directed to the defect that a mechanical stirring device must be disposed in a reactor involving a solid slurry in the prior art, and provides a non-stirred reactor suitable for containing a solid slurry, which comprises a reactor housing. There is no mechanical agitator in the reactor housing, and the reactor housing is provided with a first inlet, a second inlet, a first outlet and a second outlet, and the first inlet is a lateral inlet, which is disposed at the The upper portion of the reactor housing, the second inlet is a lateral inlet, the lower portion of the reactor housing is disposed, the first outlet is a bottom outlet, is disposed at the center of the bottom of the reactor, and the second outlet is a top outlet. It is disposed at the top of the reactor casing, thereby forming an inlet and outlet mode for feeding from the upper and lower sides, and discharging from the bottom and the top, respectively. When the lower feed is gas, the liquid gas in the reactor is formed. In the reverse flow, after the slurry enters the reactor, the pressure drops, part of the composition is converted into the gas phase, and vaporized bubbles are formed. The bubbles from the evaporation and the lower intake move upward, and continuously collide, crush and polymerize during the ascending process. Thus, the slurry in the reactor is stirred, and the tangential feed can push the slurry in the reactor to rotate, forming a swirling flow, further enhancing the mixing effect and avoiding precipitation of the solid material.

The number of the first inlets may be one or plural.

The number of the second inlets may be one or plural.

Preferably, the first inlet may be provided with a swirling flow guiding structure for forming a swirling flow and/or a swirling flow guiding device for forming a swirling flow to facilitate pushing the slurry to form a swirling flow.

Preferably, the second inlet may be provided with a swirl flow guiding structure for forming a swirling flow and/or a swirling flow guiding device for forming a swirling flow to facilitate pushing the slurry to form a swirling flow. When the upper and lower inlets both push the swirling flow, the synergy between the upper and lower sides can significantly improve the swirling effect.

Preferably, the second inlet is also connected with or without a bubbling device, and when the bubbling device is provided, it is beneficial to optimize the bubbling effect of the intake air, and when the bubbling device is not provided, it is beneficial to avoid The bubbling device interferes with and hinders the swirling flow. Therefore, in practice, reasonable settings should be made according to the specific conditions.

Preferably, the swirling flow direction of the swirling flow guiding device and/or the swirling flow guiding structure is the same as the swirling direction formed by the grounding biasing force, thereby combining the two swirling forces to strengthen the swirling flow. effect.

Preferably, the reactor shell is in the shape of a tower, that is, a reaction tower shell is adopted. Correspondingly, the reactor may be referred to as a reaction tower. Since the high diameter of the reaction tower is relatively large, it is advantageous to extend the slurry path and at the same time due to evaporation. The more the bubbles converge upward, the higher the aspect ratio will not affect the mixing effect, and the greater the power required for mechanical agitation.

Preferably, the height-to-diameter ratio of the column-shaped reactor shell is preferably 6-10:1 or 7-9:1, such as 6:1, 7:1, 9:1 and 10:1, further preferably 8:1.

The cyclone flow directing device and the bubbling device may generally be disposed within the reactor housing, and the swirl flow diversion structure may be one or more tangential inlets.

The present invention also provides a non-stirring reaction process suitable for containing a solid slurry, which is carried out by using any of the non-stirred reactors disclosed in the present invention, and is fed from the first inlet of the reactor for reaction. The slurry is fed from the second inlet to the gas or slurry for the reaction, the post-reaction slurry is output from the first outlet, and the post-reaction gas (generally referred to as tail gas) is discharged from the second outlet, and is fed by the second inlet. The material (gas or slurry) is pushed or the slurry fed by the first inlet and the second inlet is combined to form a slurry swirl in the reactor, and the operating pressure (pressure, the same below) in the reactor is lower than The feed pressure of the slurry, part of the slurry component is converted into a gas phase (evaporation) due to decompression, continuously forming vapor bubbles throughout the slurry, stirring the slurry, by bubble agitation or by bubble agitation and slurry swirling action The solid material in the slurry is in a suspended fully mixed state to prevent solid particles in the slurry from depositing at the bottom of the reactor. Thereby, it is possible to ensure that the slurry is in a good mixed state and suspended state without providing a mechanical stirring device.

The second inlet gas is also connected to the slurry. According to the process requirements, the gas to be inserted should generally be the gas required for the reaction, without adding the gas not required for the reaction itself for mixing purposes, so as to reduce the material load in the system. . For example, for the crystallization two reactor in the PTA process, the first inlet and the second inlet are only connected to the reaction slurry, and no gas is connected, and the desired suspension and mixing effects can still be achieved, from which it can be inferred that At least for other reactions with similar or lower material viscosity and similar or higher reaction gas production volume and inlet and outlet pressure difference, the required suspension and mixing effects can be achieved without the need to access external gases, satisfying the reaction and process. Requirements. Certain experimental tests and verifications can be performed according to the methods described below.

The pressure difference between the operating pressure in the reactor and the feed pressure of the slurry is not less than the critical pressure difference of the suspension, and the critical pressure difference of the suspension is when the gas velocity of the rising gas (bubble) is equal to the critical suspended gas velocity. a pressure difference between an operating pressure in the reactor and a feed pressure of the slurry, the critical gas velocity being a minimum gas velocity in which the solid gas in the slurry is suspended and in a fully mixed state, in a specific practice The minimum gas velocity and the corresponding suspension critical pressure difference corresponding thereto can be obtained by experimental and/or theoretical calculations.

The present invention also provides an agitated PTA ripening crystallization apparatus comprising a curing reactor and a crystallization reactor which are sequentially connected, the number of the aging reactors being one or more, and the number of the crystallization reactors is one or a plurality of said maturation reactors adopting any of the non-stirred reactors disclosed in the present invention, and the crystallization reactor also employs any of the non-stirred reactors disclosed in the present invention, when the number of the maturation reactors is large At a time, the plurality of maturation reactors use the same non-stirred reactor or different ones of the non-stirred reactors. When the number of the crystallization reactors is plural, the plurality of crystallization reactors Using the same non-stirred reactor or a different said non-stirred reactor, the first outlet of any pre-reactor is connected to a first inlet of an adjacent subsequent reactor, said pre-reactor The first outlet may be connected to the second inlet of the adjacent subsequent reactor or may not be connected to the second inlet of the adjacent subsequent reactor. Generally, when the feed of the adjacent subsequent reactor of the current sequential reactor is only the discharge of the first outlet of the pre-reactor, the discharge of the first outlet of the pre-reactor is divided into two paths, which are respectively connected through the pipeline. Into the first inlet and the second inlet of the adjacent subsequent reactor, the feed of the adjacent subsequent reactor of the current sequential reactor comprises the discharge of the first outlet of the pre-reactor and the second outlet of the pre-reactor When discharging (exhaust gas), the first outlet of the pre-reactor is connected to the first inlet of the adjacent subsequent reactor through a pipeline, and the second outlet of the pre-reactor is connected to the second inlet of the adjacent subsequent reactor through the pipeline Thereby, adjacent sequential reactors are fed into the slurry from the first inlet located at the upper portion and from the second inlet located at the lower portion.

Preferably, the number of the ripening reactors is two, including a ripening I reactor and a ripening II reactor located in the subsequent step of the ripening I reactor, and the number of the crystallizing reactors is also two, including one crystal. a reactor and a two-crystallization reactor located in the subsequent stage of the crystallization reactor, the first inlet of the aging I reactor is used to access an oxidizing slurry output from the PTA oxidizing unit, and an input for transporting the oxidizing slurry is connected a conduit, a second inlet for accessing an oxygen-containing gas (eg, air) required for the reaction, and a first inlet of the ripening II reactor for accessing the matured I slurry output from the ripening I reactor, through the pipeline a first outlet for connecting the ripening I reactor, a second inlet for accessing the matured tail gas discharged from the ripening I reactor, and a second outlet of the ripening I reactor connected by a pipe, the one crystal reaction The first inlet of the device is used to access the mature II slurry outputted by the ripening II reactor, the first outlet of the ripening II reactor is connected through a pipeline, and the second inlet is used to access the ripening II reactor for discharging Ripening II tail gas through the tube a second outlet of the ripening II reactor, the first inlet of the two-crystallization reactor is used to access a portion of a crystal slurry output from the one of the crystallization reactors, and the one crystal is connected through a pipeline a first outlet of the reactor, a second inlet for accessing a remaining portion of a crystal slurry outputted by the one crystallization reactor, and a first outlet of the crystallization reactor connected by a conduit, the crystallization reaction The second outlet of the device is connected with a crystallization tail gas output pipe for feeding a crystal tail gas into the PTA oxidation unit, whereby the maturation I reactor, the maturation II reactor and the crystallization-reactor are all from the upper part. Imported into the slurry, from the lower second inlet, while the crystallization two reactor is the first inlet and the second inlet are only into the slurry, not in the air, the bubbles in the reactor are all derived from the pressure drop Evaporation of bubbles, thereby indicating that even for the high concentration slurry of the crystallization two reactor, using the method of the invention, under suitable operating parameters, only the swirl formed by the evaporation bubble and the feed However, the mix can be effective and suspension.

According to actual needs, an oxidation slurry pressurization and a heater may be disposed on the input pipe connected to the first inlet of the ripening I reactor for increasing the temperature and pressure of the oxidizing slurry, and the oxidizing slurry heater is preferably A heat exchanger that uses high pressure steam as a heat medium.

Preferably, the ripening I reactor is provided with a curing I level sensor for collecting its liquid level signal and a curing I pressure sensor for collecting a pressure signal thereof, the first outlet of the curing I reactor and the curing a curing I discharge control valve controlled by an output signal of the curing I level sensor, a second outlet of the curing I reactor and the curing II is disposed on a connecting pipe between the first inlets of the II reactor A curing I vent control valve controlled by the output signal of the aging I pressure sensor may be disposed on the connecting pipe between the second inlets of the reactor, thereby controlling the slurry discharging of the aging I reactor according to the liquid level control According to the pressure control, the exhaust gas of the ripening I reactor is maintained, and the liquid level in the reactor is maintained within a reasonable range by the slurry discharge, and the pressure in the reactor is maintained within a reasonable range by exhaust gas discharge, which is beneficial to The stability of the reaction conditions/process parameters of the ripening I reactor is good, and a good reaction effect is obtained.

Preferably, the ripening II reactor is provided with a ripening II liquid level sensor for collecting its liquid level signal and a ripening II pressure sensor for collecting the pressure signal thereof, the first outlet of the curing II reactor and the first a curing II discharge control valve controlled by an output signal of the ripening II level sensor, a second outlet of the curing II reactor and the first crystal is disposed on a connecting pipe between the first inlets of the crystallization reactor A curing II exhaust gas control valve controlled by the output signal of the curing II pressure sensor is disposed on the connecting pipe between the second inlets of the reactor, so that the slurry discharging of the ripening II reactor can be controlled according to the liquid level. According to the pressure control, the tail gas discharge of the maturation reactor II is maintained, and the liquid level in the reactor is maintained within a reasonable range by the slurry discharge, and the pressure in the reactor is maintained within a reasonable range by exhaust gas discharge, which is beneficial to the ripening. II reactor reaction conditions / process parameters are stable, and a good reaction effect is obtained.

Preferably, the one crystallizing reactor is provided with a crystal liquid level sensor for collecting the liquid level signal thereof and a crystal pressure sensor for collecting the pressure signal thereof, the first outlet of the one crystallizing reactor and the second The first inlet of the crystallization reactor and the second inlet of the two-crystallization reactor are connected in such a manner that a first outlet of the crystallization reactor is connected to a crystallization outlet tube, a first inlet of the two-crystallization reactor and The second inlet is respectively connected to the one crystal discharge pipe through the two-crystal first feed pipe and the two-crystal second feed pipe, thereby dividing the discharge of one crystal slurry into two paths, respectively passing through the two-crystallization reactor The first inlet and the second inlet enter the two-crystallization reactor, thereby achieving simultaneous and proportional feeding of the first inlet and the second inlet of the two-crystallization reactor, wherein the slurry passing through the second inlet of the two-crystallization reactor is used for passage The corresponding swirling flow guiding structure and/or the swirling flow guiding device pushes the slurry in the two-crystallization reactor to form a swirling flow, and the proportion of the slurry entering the second inlet should be moderately controlled as long as the required swirling flow can be formed. To It is possible to increase the proportion of the feed of the first inlet, the crystallization outlet pipe is provided with a crystallization discharge control valve controlled by the output signal of the crystallization level sensor, and the crystallization discharge control valve is located at the Before the connection between the crystallization outlet pipe and the second crystallization first feed pipe and the second crystallization second feed pipe, all the crystal slurry is flowed through the control valve to ensure that the control valve is a crystal slurry For the effective control of the material discharge, the one crystal tail gas output pipe is provided with a crystal tail gas heat recovery device for by-product steam, and the one crystal tail gas heat recovery device is a heat exchanger with a crystal tail gas as a heat medium. The crystallization exhaust gas output pipe is provided with a crystallization exhaust control valve controlled by an output signal of the crystallization pressure sensor, and the crystallization exhaust gas control valve is installed at a position behind the crystallization exhaust gas heat recovery device. The crystallization tail gas output pipe is connected to a crystallization return pipe, and the inlet end of the crystallization return pipe is connected to the condensate outlet of the crystallization tail gas heat recovery device or Connected to the one crystal tail gas output pipe between the one crystal tail gas heat recovery device and the one crystal exhaust gas control valve, the outlet end of the one crystal return pipe is connected to the one crystallizing reactor, According to the liquid level, the slurry discharge of a crystallization reactor can be controlled, the tail gas discharge of a crystallization reactor can be controlled according to the pressure, and the liquid level in the reactor can be maintained within a reasonable range by the slurry discharge, and the exhaust gas is discharged through the exhaust gas. Maintaining the pressure in the reactor within a reasonable range is beneficial to the stability of the reaction conditions/process parameters of a crystallization reactor, and a good reaction effect is obtained.

Preferably, the two-crystallization reactor is provided with a two-crystallization liquid level sensor for collecting its liquid level signal and a two-crystallization pressure sensor for collecting a pressure signal thereof, and the first outlet of the two-crystallization reactor is connected with two crystals. a discharge pipe, wherein the two-crystal discharge pipe is provided with a two-crystal discharge control valve controlled by an output signal of the two-crystallization liquid level sensor, and a second outlet of the two-crystallization reactor is connected with a two-crystal tail gas output a pipe, the two-crystal exhaust gas output pipe is provided with a two-crystal exhaust gas control valve controlled by an output signal of the two-crystallization pressure sensor. Therefore, the slurry discharge of the two-crystallization reactor can be controlled according to the liquid level, the tail gas discharge of the two-crystallization reactor can be controlled according to the pressure, and the liquid level in the reactor can be maintained within a reasonable range by the slurry discharge, and the exhaust gas is passed through the exhaust gas. The discharge maintains the pressure in the reactor within a reasonable range, which is favorable for the stability of the reaction conditions/process parameters of the two-crystallization reactor, and a good reaction effect is obtained.

Preferably, the dicrystalline tail gas output pipeline is connected to the dehydration tower to dehydrate the dicrystalline tail gas and realize reuse, and the feed tank of the filtering device is arranged behind the two crystallizing reactor, and the filtering device is preferably The pressure filter is further preferably an RPF (Rotary Pressure Filter).

The feed tank may adopt any suitable prior art, preferably any of the non-stirred reactors disclosed in the present invention, and is provided with a first inlet, a second inlet, a first outlet and a second outlet, the feed tank The first inlet is a lateral inlet, disposed at an upper portion of the supply tank housing, the second inlet is a lateral inlet, a lower portion of the supply tank housing is disposed, and the first outlet is a bottom outlet, and is disposed at the bottom a central portion of the bottom of the feed tank, a second outlet being a top outlet, disposed at the top of the feed tank, the first inlet of the feed tank for accessing a portion of the second crystal slurry output from the two-crystallization reactor Feeding the first feed pipe of the feed tank, the second inlet of the feed tank is for accessing the remaining two crystal slurry outputted by the two-crystallization reactor, and the feed tank is connected a second feeding tube, the first feeding tube of the feeding trough and the second feeding tube of the feeding trough are connected with the two crystal discharging tube to form two branches of the two crystal discharging tube, The feed tank is provided with a feed tank level sensor for collecting its liquid level signal, the feed tank The first outlet is connected with a supply tank discharge pipe for accessing the RPF or other filtering device, and the supply trough discharge pipe is provided with a supply trough controlled by the output signal of the supply tank liquid level sensor a material control valve, a second outlet of the feed tank is connected to a feed trough exhaust gas output pipe, and a supply tank exhaust gas heat recovery device for by-product steam is provided on the feed trough exhaust gas output pipe, the feed trough The exhaust gas heat recovery device is a heat exchanger in which the tail gas of the feed tank is used as a heat medium, and the end of the tail gas output pipe of the feed tank can be emptied, thereby controlling the discharge of the slurry of the feed tank according to the liquid level. The slurry discharge maintains the liquid level in the feed tank within a reasonable range, and the inside of the feed tank is kept empty at the end of the tail gas output pipe of the feed tank, which is favorable for a crystallization reactor reaction condition/process The parameters are stable and a good reaction effect is obtained.

The invention also provides a non-stirred PTA curing crystallization method, which adopts any non-stirred PTA curing crystallization device disclosed in the invention to perform aging and crystallization of the oxidized slurry, and the maturation reactor adopts any of the disclosed inventions. The invention relates to a non-stirring reaction process, and the crystallization reactor also adopts any non-stirring reaction process disclosed in the present invention. When the number of the maturation reactors is plural, the plurality of maturation reactors adopt the non-stirring process. The reaction process may be the same or different. When the number of the crystallization reactors is plural, the agitation reaction processes employed in the plurality of crystallization reactors may be the same or different.

Preferably, the non-stirred PTA ripening crystallization apparatus provided with any of the two ripening reactors and two crystallizing reactors disclosed in the present invention is used.

In the case of any of the non-stirred PTA ripening crystallization apparatus provided with two maturation reactors and two crystallization reactors disclosed in the present invention:

Optionally, before the oxidizing slurry enters the aging I reactor, the oxidizing slurry is heated by the oxidizing slurry pressurization and the heater to make the pressure higher than the operating pressure of the aging I reactor, and the aging is performed The pressure difference between the operating pressures of the I reactor is not less than the minimum pressure difference in which the solid material in the slurry is in a suspended fully mixed state (the minimum pressure difference can be obtained experimentally and/or calculated), and is sent to the ripening I reaction. The oxygen-containing gas of the device is a pressurized gas, for example, compressed air, or compressed air mixed into any reactor exhaust gas or mixed with a certain pressure of air and exhaust gas of any reactor, and the pressure of the pressurized gas should be It is enabled to enter the ripening I reactor and is capable of propelling the slurry in the ripening I reactor to form the desired swirl, the minimum of which can be obtained experimentally and/or calculated.

Preferably, the ripening I reactor has an operation of 3.2-4.5 MPaG and an operating temperature of 230-240 °C. The operating pressure and temperature of the ripening I reactor may be controlled within the above range by an automatic control method, or may be controlled to any value within the above range or any interval, for example, the operating pressure may be 3.2 MPaG, 4.0 MPaG or 4.5 MPaG, The operating temperature can be 230 ° C, 235 ° C or 240 ° C.

Preferably, the slurry output of the ripening I reactor is controlled by the liquid level in the ripening I reactor, and when the liquid level reaches and/or exceeds the set upper limit of the liquid level control, the output of the curing I discharge control valve is turned on. Curing the I slurry, when the liquid level reaches and/or falls below the set lower liquid level control lower limit, the ripening I discharge control valve is closed, the ripening I slurry is not output, and the pressure in the ripening I reactor is controlled. Exhaust gas discharge from the I reactor, when the pressure reaches and/or exceeds the set upper pressure control limit, the maturation I exhaust control valve is opened to discharge the mature I tail gas when the pressure reaches and/or falls below a set value. When the lower limit of the pressure is controlled, the ripening I exhaust control valve is closed, and the mature I exhaust gas is not discharged.

Preferably, the ripening II reactor has an operating pressure of 2.0-3.0 MPaG and an operating temperature of 210-230 °C. The operating pressure and temperature of the ripening II reactor may be controlled within the above range by an automatic control method, or may be controlled to any value or any interval within the above range. For example, the operating pressure may be 2.0 MPaG, 2.5 MPaG or 3.0 MPaG. The operating temperature can be 210 ° C, 220 ° C or 230 ° C.

Preferably, the slurry output of the ripening II reactor is controlled by the liquid level in the ripening II reactor, and when the liquid level reaches and/or exceeds the set upper limit of the liquid level control, the output of the curing II discharge control valve is turned on. Curing the II slurry, when the liquid level reaches and/or falls below the set lower liquid level control lower limit, the ripening II discharge control valve is closed, and the ripening II slurry is not output, and the pressure in the ripening II reactor is controlled. The exhaust gas of the ripening II reactor, when the pressure reaches and/or exceeds the set upper limit of the pressure control, the ripening II exhaust control valve is opened to discharge the matured tail gas, when the pressure reaches and/or falls below the set When the lower limit of the pressure is controlled, the ripening II exhaust control valve is closed, and the mature II exhaust gas is not discharged.

Preferably, the crystallization reactor has an operating pressure of 1.5-2.0 MPaG and an operating temperature of 179-195 °C. The operating pressure and temperature of a crystallization reactor may be controlled within the above range by an automatic control method, or may be controlled to any value or any interval within the above range, for example, the operating pressure may be 1.5 MPaG, 1.75 MPaG or 2.0 MPaG, The operating temperature can be 179 ° C, 187 ° C or 195 ° C.

Preferably, the slurry output of the crystallization-reactor is controlled by the liquid level in the crystallization-reactor, and when the liquid level reaches and/or exceeds the set upper limit of the liquid level control, the crystallization-discharge control valve output is turned on. Crystallizing a slurry, when the liquid level reaches and/or falls below a set lower limit of liquid level control, the crystallization-discharge control valve is closed, no crystal-slurry is output, and pressure control in the crystallization-reactor is performed. Crystallization of the exhaust gas of a reactor, when the pressure reaches and/or exceeds a set upper limit of pressure control, the crystallization-exhaust control valve is opened to discharge a crystallization gas, when the pressure reaches and/or falls below a set value When the lower limit of the pressure is controlled, the crystallization-exhaust control valve is closed, and no crystallization of exhaust gas is discharged.

Preferably, the operating pressure of the two-crystallization reactor is 0.2-0.4 MPaG, and the operating temperature is 135-145 °C. The operating pressure and temperature of the two-crystallization reactor may be controlled within the above range by an automatic control method, or may be controlled to any value or any interval within the above range. For example, the operating pressure may be 0.2 MPaG, 0.3 MPaG or 0.4 MPaG. The operating temperature can be 135 ° C, 140 ° C or 145 ° C.

Preferably, the slurry output of the crystallization two reactor is controlled by the liquid level in the crystallization two reactor, and when the liquid level reaches and/or exceeds the set upper limit of the liquid level control, the output of the crystallization two discharge control valve is turned on. Crystallizing the two slurry, when the liquid level reaches and/or falls below the set lower liquid level control lower limit, the crystal two discharge control valve is closed, the crystal two slurry is not output, and the pressure in the crystal two reactor is controlled. Exhaust gas discharge from the crystallization two reactor, when the pressure reaches and/or exceeds a set upper limit of pressure control, the crystallization two-exhaust control valve is opened to discharge the crystallization two tail gas when the pressure reaches and/or is lower than the set When the lower limit of the pressure is controlled, the crystallization two-exhaust control valve is closed, and the crystallization of two tail gases is not discharged.

Preferably, the slurry of the crystallization two reactor is fed to a feed tank of a filtration device, and the operating pressure of the feed tank is normal pressure.

The following is an example of a PTA ripening crystallization apparatus and method:

The number of the deep oxidation reactors is two, including a ripening I reactor and a ripening II reactor located in the subsequent step of the ripening I reactor, the number of the crystallization reactors being two, including a crystallization reactor ( a crystallization reactor) and a two-crystallization reactor (two-crystallization reactor) located in the subsequent step of the crystallization reactor, the first inlet of the aging I reactor is used to access the oxidizing slurry output from the oxidation reaction unit ( Oxidation slurry), the second inlet is used to access an oxygen-containing gas (for example, compressed air) required for the reaction, the operation of the ripening I reactor is 3.2-4.5 MPaG, the operating temperature is 230-240 ° C, in the oxidizing slurry Before entering the ripening I reactor, the slurry is heated by oxidizing slurry pressurization and heating to a pressure higher than the operating pressure of the ripening I reactor and between the operating pressure of the ripening I reactor The pressure difference is not less than the minimum pressure difference in which the solid material in the slurry is in a suspended fully mixed state (the minimum pressure difference can be obtained experimentally and/or calculated), and the oxygen-containing gas fed to the ripening I reactor is a pressurized gas. , the pressure should be such that it can enter the ripening I The reactor is capable of propelling the slurry in the ripening I reactor to form the desired swirl (the minimum of which can be obtained experimentally and/or calculated), the first inlet of the ripening II reactor is used for access The slurry output from the ripening I reactor is connected to the first outlet of the ripening I reactor through a pipeline, and the second inlet is used to access the ripening I tail gas output from the ripening I reactor, and the ripening is connected through a pipeline. a second outlet of the I reactor, the operating pressure of the ripening II reactor is 2.0-3.0 MPaG, the operating temperature is 210-230 ° C, and the ripening I reactor is provided with a curing I level for collecting the liquid level signal thereof. a sensor and a curing I pressure sensor for collecting a pressure signal thereof, wherein the curing I level is provided on a connecting pipe between the first outlet of the curing I reactor and the first inlet of the curing II reactor The ripening I discharge control valve controlled by the output signal of the sensor, when the liquid level in the ripening I reactor is higher than the upper limit of the liquid level control, the curing I discharge control valve is opened to deliver to the ripening II reactor Ripening I slurry, the ripening I reaction A curing I vent control valve controlled by the output signal of the aging I pressure sensor is provided on the connecting pipe between the second outlet of the aging reactor and the second inlet of the aging II reactor, when the aging I reactor is When the pressure inside is higher than the upper limit of the pressure control, the ripening I exhaust control valve opens to deliver the ripening I tail gas to the ripening II reactor, and the first inlet of the one crystallizing reactor is used to access the ripening II The slurry output from the reactor is connected to the first outlet of the ripening II reactor through a pipeline, and the second inlet is used to access the matured tail gas output from the ripening II reactor, and the ripening II reactor is connected through a pipeline. a second outlet, the ripening II reactor is provided with a ripening II level sensor for collecting its liquid level signal and a curing II pressure sensor for collecting a pressure signal thereof, the first outlet of the curing II reactor and the a curing II discharge control valve controlled by the output signal of the ripening II level sensor is disposed on the connecting pipe between the first inlet of a crystallization reactor, when the liquid level in the curing II reactor is higher than Liquid level control And the ripening II discharge control valve opens to transfer the ripening II slurry to the one crystallizing reactor, and the connecting pipe between the second outlet of the ripening II reactor and the second inlet of the one crystallizing reactor An aging II exhaust control valve controlled by an output signal of the aging II pressure sensor is provided, and when the pressure in the aging II reactor is higher than an upper limit of the pressure control, the aging control valve is opened The first crystallization reactor transports the mature II tail gas, the first inlet of the two crystallization reactor is used to access a part of the slurry outputted by the crystallization reactor, and the first outlet of the crystallization reactor is connected through a pipeline a second inlet for accessing the remaining slurry of the output of the one crystallization reactor (except for all the slurry that is connected to the first inlet), and connecting the first outlet of the one crystallization reactor through a pipe, a second outlet of a crystallization reactor is connected to a crystallization tail gas output line for accessing the PTA oxidation unit, the crystallization reactor operating at a pressure of 1.5-2.0 MPaG, an operating temperature of 179-195 ° C, the crystallization Reactor for use a crystallization level sensor for collecting a liquid level signal thereof and a crystallization pressure sensor for collecting a pressure signal thereof, a first outlet of the crystallization reactor and a first inlet and the second crystallization of the two crystallization reactor The second inlet of the reactor is connected in such a manner that a first outlet of the one crystallization reactor is connected to a crystallization outlet pipe, and the first inlet and the second inlet of the two crystallization reactor respectively pass through the second crystallization first feed tube And a second crystal second feed tube is connected to the one crystal discharge tube, thereby dividing the slurry output of the one crystallizing reactor into two paths, all the way into the first inlet of the two crystallizing reactor, and Passing all the way into the second inlet of the two-crystallization reactor, the crystallization discharge pipe is provided with a crystallization discharge control valve controlled by the output signal of the crystallization liquid level sensor, and the crystallization discharge control a valve is located in front of the junction of the one crystallized discharge pipe and the second crystal first feed pipe and the second crystal second feed pipe, when the liquid level in the one crystallizing reactor is higher than the liquid level control The upper limit, the one crystal discharge The control valve is opened to synchronously convey a crystal slurry to the first inlet and the second inlet of the two-crystallization reactor, and the one crystal tail gas output pipeline is provided with a crystal tail gas heat recovery device for by-product steam, the one The crystal tail gas heat recovery device is a heat exchanger using a crystal tail gas as a heat medium, and the one crystal tail gas output line is provided with a crystal exhaust gas control valve controlled by an output signal of the crystal pressure sensor, the one a crystallization exhaust gas control valve is installed on the one crystal tail gas output pipe behind the one crystal tail gas heat recovery device, and the one crystal tail gas output pipe is further connected with a crystal return pipe, and the inlet end of the one crystal return pipe is connected An outlet end of the crystallization return pipe is connected to the crystallization reactor on the one crystallization tail gas output pipe between the one crystal tail gas heat recovery device and the one crystallization exhaust gas control valve. When the pressure in the one crystal is higher than the upper limit of the pressure control, the one crystal exhaust gas control valve is opened to deliver a crystal tail gas to the one crystal tail gas heat recovery unit, and a crystal tail gas is passed through After the heat exchange, the non-condensable gas is sent to the oxygen unit, and the condensate is refluxed into the crystallization reactor through the one crystallization return tube, and the feed tank for feeding the filtering device is arranged behind the two-crystallization reactor. The feeding trough is provided with a first inlet, a second inlet, a first outlet and a second outlet, and the first inlet of the feeding trough is a lateral inlet, which is arranged at an upper part of the feeding trough casing, The second inlet is a lateral inlet, a lower portion of the supply tank housing is disposed, the first outlet is a bottom outlet, is disposed at a center of the bottom of the supply tank, and the second outlet is a top outlet, and is disposed at the feeding a top of the tank, a first outlet of the two-crystallization reactor is connected with a two-crystal discharge pipe, and the two-crystal discharge pipe is respectively connected to the first feed pipe of the feed tank and the second feed pipe of the feed tank. The two crystal tail gas output pipeline is connected to the dehydration tower, the operating pressure of the two crystallizing reactor is 0.2-0.4 MPaG, the operating temperature is 135-145 ° C, the operating pressure of the feed tank is atmospheric pressure, and the two crystals The reactor is provided with a two-crystal level sensor for collecting its liquid level signal a two-crystal pressure sensor for collecting a pressure signal thereof, wherein the two-crystal discharge tube is provided with a two-crystal discharge control valve controlled by an output signal of the two-crystal level sensor, when the two-crystal reactor is When the liquid level is higher than the upper limit of the liquid level control, the two crystal discharge control valve opens to synchronously transport the two crystal slurry to the first inlet and the second inlet of the feed tank, and the two crystal tail gas output pipeline Providing a two-crystal exhaust gas control valve controlled by an output signal of the two crystal pressure sensor, when the pressure in the two crystals is higher than an upper limit of the pressure control, the two-crystal exhaust gas control valve is opened to open the two crystals The dehydration tower is sent to a dehydration treatment.

The upper and lower portions of the reactor housing of the present invention are mainly used to indicate the relative positional relationship between the first inlet and the second inlet, and the specific positions of the inlets in the axial direction of the reactor housing are set according to actual needs. Since the setting positions of the first inlet and the second inlet are closely related to the liquid level height, generally, the first inlet may be disposed at an upper portion of the slurry region, particularly a near liquid surface region, which is a middle upper portion of the reactor casing, and a second The inlet can be placed in the lower portion of the slurry zone as the lower portion of the reactor housing, particularly the near lower header region.

The term "slurry" as used in the present invention refers to a liquid or liquid-like material relating to a reaction, and includes a liquid containing solid particles (abbreviated as solids), and a liquid containing no solid particles.

The solid slurry in the present invention refers to a slurry containing suspended solid particles, wherein the solid particles are dispersed phases, and the solid particles usually precipitate under a standing state, and the solid particles can be uniformly or substantially uniformly in a mixed state. Dispersed in the slurry, since the solid particles in the slurry should be in suspension during the reaction, the slurry may also be referred to as a suspension slurry.

The solid particulate matter referred to in the present invention includes particulate solid matter and physical properties (mainly dispersion, suspension and precipitation characteristics) in the slurry, and other dispersed phase materials similar to the granular pure solid material.

The term "no agitation" as used in the present invention means that there is no mechanical agitator stirring.

The preferred and optional technical means disclosed in the present invention can be combined in any combination to form a plurality of different technical solutions, unless otherwise specified, and a preferred or optional technical means is further defined by another technical means.

Claims

A non-stirred reactor suitable for containing a solid slurry, comprising a reactor housing, characterized in that there is no mechanical agitator in the reactor housing, and the reactor housing is provided with a first inlet and a second An inlet, a first outlet and a second outlet, the first inlet being a lateral inlet, disposed at an upper portion of the reactor housing, the second inlet being a lateral inlet, and a lower portion of the reactor housing, An outlet is a bottom outlet, disposed in the center of the bottom of the reactor, and a second outlet is a top outlet disposed at the top of the reactor housing.
A stirred-free reactor according to claim 1, wherein said first inlet is provided with a swirling flow guiding structure for forming a swirling flow and/or a swirling flow guiding means for forming a swirling flow, said a second inlet is provided with a swirling flow guiding structure for forming a swirling flow and/or a swirling flow guiding device for forming a swirling flow, the second inlet is also connected with or without a bubbling device, the rotation The swirling direction of the flow guiding device and/or the swirling flow guiding structure is preferably the same as the swirling direction formed by the geostrophic biasing force, and the reactor casing preferably has a tower shape, and the tower-shaped reactor shell The height to diameter ratio of the body is preferably from 6 to 10:1.
A non-stirring reaction process suitable for containing a solid slurry, characterized in that the reaction is carried out by using any of the non-stirred reactors according to claim 1 or 2, and is fed from the first inlet of the reactor for reaction The slurry is fed from the second inlet to the gas or slurry for the reaction, the post-reaction slurry is discharged from the first outlet, the reacted gas is discharged from the second outlet, and the material fed by the second inlet is driven or relied on. The co-pushing of the materials fed by the first inlet and the second inlet forms a swirling flow in the reactor, the operating pressure in the reactor is lower than the feeding pressure of the slurry, and part of the slurry component is converted into the gas phase due to the reduced pressure. Continuously forming vapor bubbles throughout the slurry, stirring the slurry, and causing the solid materials in the slurry to be in a fully suspended state by bubble mixing or by bubble agitation and slurry swirling to avoid solid particles in the slurry. The bottom of the device is deposited.
The non-stirring reaction process according to claim 3, wherein the pressure difference between the operating pressure in the reactor and the feed pressure of the slurry is not less than the suspension critical pressure difference, and the suspension critical pressure difference is The gas velocity of the ascending gas is equal to the pressure difference between the operating pressure in the reactor and the feed pressure of the slurry at a critical suspending gas velocity, the critical suspending gas velocity being an ascending gas suspending solid particulates in the slurry and at The minimum gas velocity in the fully mixed state.
An agitated PTA ripening crystallization device characterized by comprising a sequentially connected maturation reactor and a crystallization reactor, the number of the maturation reactors being one or more, and the number of the crystallization reactors being one or more, The maturation reactor adopts any one of the non-stirred reactors according to claim 1 or 2, and the crystallization reactor also adopts any one of the non-stirred reactors according to claim 1 or 2, and any pre-reaction reaction The first outlet of the unit is connected to the first inlet of the adjacent subsequent reactor.
The non-stirred PTA ripening crystallization apparatus according to claim 5, wherein the number of the ripening reactors is two, including a ripening I reactor and a ripening II reactor located in the subsequent step of the ripening I reactor. The number of crystallization reactors is two, including a crystallization reactor and a two-crystallization reactor located in the subsequent step of the crystallization reactor, and the first inlet of the aging I reactor is used to access the output of the PTA oxidation unit. An oxidizing slurry to which is connected an input pipe for transporting the oxidizing slurry, a second inlet for accessing an oxygen-containing gas required for the reaction, and a first inlet of the aging II reactor for accessing the aging I reactor The outputted mature I slurry is connected to the first outlet of the ripening I reactor through a pipeline, and the second inlet is used to access the ripening I tail gas discharged from the ripening I reactor, and the matured I reactor is connected through a pipeline a second outlet, the first inlet of the crystallization reactor is used to access the ripening II slurry outputted by the ripening II reactor, the first outlet of the ripening II reactor is connected by a pipeline, and the second inlet is used for Access to the ripening I The ripening II tail gas discharged from the I reactor is connected to the second outlet of the ripening II reactor through a pipeline, and the first inlet of the two-crystallization reactor is used to access a crystal slurry outputted by the one crystallizing reactor a portion of the first outlet of the crystallization reactor connected by a pipe, the second inlet for accessing the remaining portion of a crystal slurry outputted by the crystallization reactor, and the crystallization reactor being connected by a pipe The first outlet of the crystallization reactor is connected to a crystallization tail gas output line for feeding a crystal tail gas to the PTA oxidation unit.
The agitating PTA aging crystallization apparatus according to claim 5 or 6, wherein an oxidizing slurry heater is disposed on the input pipe of the first inlet of the aging I reactor, and the oxidizing slurry heater is preferably a heat exchanger using high pressure steam as a heat medium, the ripening I reactor is provided with a curing I level sensor for collecting a liquid level signal thereof, and a curing I pressure sensor for collecting a pressure signal thereof, the curing I reactor a curing I discharge control valve controlled by an output signal of the curing I level sensor is disposed on a connecting pipe between the first outlet and the first inlet of the ripening II reactor, and the curing I reactor is A curing I vent control valve controlled by an output signal of the aging I pressure sensor is disposed on a connecting pipe between the second outlet and the second inlet of the aging II reactor, and the aging II reactor is provided for a ripening II level sensor for collecting its liquid level signal and a curing II pressure sensor for collecting a pressure signal thereof, a connecting pipe between the first outlet of the ripening II reactor and the first inlet of the one crystallizing reactor Providing a ripening II discharge control valve controlled by an output signal of the ripening II level sensor, a connection pipe between the second outlet of the ripening II reactor and the second inlet of the one crystallizing reactor a maturation II exhaust control valve controlled by an output signal of the ripening II pressure sensor, the crystallizing reactor being provided with a crystal liquid level sensor for collecting the liquid level signal thereof and a crystal for collecting the pressure signal thereof a pressure sensor, wherein a first outlet of the one crystallizing reactor is connected to a first inlet of the two-crystallization reactor and a second inlet of the two-crystallization reactor is a first outlet of the one crystallizing reactor a crystallization discharge pipe, the first inlet and the second inlet of the two crystallization reactor are respectively connected to the one crystallization discharge pipe through a two-crystal first feed pipe and a two-crystal second feed pipe, thereby The discharge of the crystallization slurry is divided into two paths, and the first inlet and the second inlet of the two crystallization reactor respectively enter the two crystallization reactor, and the crystallization outlet tube is provided with the crystallization liquid level sensor Output letter a controlled crystallization discharge control valve, the crystallization discharge control valve being located before the junction of the one crystallization discharge pipe and the two crystallization first feed pipe and the second crystallization second feed pipe A crystal tail gas output pipe is provided with a crystal tail gas heat recovery device for by-product steam, and the one crystal tail gas heat recovery device is a heat exchanger with a crystal tail gas as a heat medium, and the one crystal tail gas output pipe is provided a crystallization exhaust control valve controlled by an output signal of the crystallization pressure sensor, the crystallization exhaust control valve being mounted on the crystallization exhaust gas output pipe behind the crystallization exhaust gas heat recovery device The crystallization tail gas output pipe is further connected with a crystallization return pipe, and the inlet end of the crystallization return pipe is connected to the condensate outlet of the crystallization tail gas heat recovery device or connected to the crystallization tail gas heat recovery device and the a crystallization exhaust gas output pipe between the crystallization exhaust gas control valve, the outlet end of the crystallization return pipe is connected to the one crystallization reactor, and the two crystallization reactor is provided for a two-crystal liquid level sensor of the liquid level signal and a two-crystal pressure sensor for collecting the pressure signal thereof, wherein the first outlet of the two-crystallizing reactor is connected with a two-crystal discharge pipe, and the two-crystal discharge pipe is provided a two-crystal discharge control valve controlled by an output signal of the two-crystal level sensor, a second outlet of the two-crystal reactor is connected with a two-crystal tail gas output pipe, and the two-crystal tail gas output pipe is provided with The output signal of the two crystal pressure sensor controls a two-crystal exhaust gas control valve.
The agitating PTA aging crystallization apparatus according to claim 7, wherein the two-crystal tail gas output pipe is connected to a dehydration column, and a supply tank of a filtering device is disposed behind the two-crystallization reactor, the filtering device Preferably, a pressure filter, further preferably RPF, is used in any of the non-stirred reactors according to claim 1 or 2, the first inlet of the feed tank is for accessing the two-crystallization reactor a part of the second crystal slurry is output, and the first feed pipe of the feed tank is connected, and the second inlet of the feed tank is used for accessing the remaining two crystal slurry of the output of the two-crystallization reactor, and the connection is a second feeding pipe of the feeding trough, a first feeding pipe of the feeding trough and a second feeding pipe of the feeding trough are connected with the two crystal discharging pipe to form the two crystal discharging pipe Two branch roads, the feed tank is provided with a feed tank liquid level sensor for collecting liquid level signals, and the first outlet of the feed tank is connected with a feed tank discharge pipe for accessing the RPF. The output pipe of the feed tank is provided with an output signal controlled by the liquid level sensor of the supply tank a feed chute discharge control valve, a second outlet of the feed trough is connected to a feed trough exhaust gas output pipe, and a feed trough heat recovery device for a by-product steam is provided on the feed trough exhaust gas output pipe, The feed tank exhaust gas heat recovery device is a heat exchanger in which the feed tank exhaust gas is a heat medium, and the end of the feed tank exhaust gas output pipe can be evacuated.
A method for aging crystallization without stirring PTA, characterized in that the aging and crystallization of a slurry after oxidation is carried out by using the non-stirred PTA aging crystallization apparatus according to claim 5, wherein the aging reactor adopts any of the claims 3 or 4. A non-stirring reaction process, which also employs any of the agitation-free reaction processes of claim 3 or 4.
The method of pulverizing PTA without pulverization according to claim 9, wherein the non-stirred PTA aging crystallization apparatus adopts any of the non-stirred PTA aging crystallization apparatuses according to claim 6, 7 or 8, in the oxidizing slurry. Before entering the ripening I reactor, the slurry is heated by the oxidation slurry pressurization and the heater to make the pressure higher than the operating pressure of the ripening I reactor, and the operating pressure of the ripening I reactor The pressure difference between the two is not less than the minimum pressure difference in which the solid material in the slurry is in a suspended fully mixed state, and the oxygen-containing gas fed to the ripening I reactor is a pressure gas, and the pressure thereof is such that it can enter the ripening I reactor and can Pushing the slurry in the ripening I reactor to form the required swirling flow, the operation of the ripening I reactor is 3.2-4.5 MPaG, the operating temperature is 230-240 ° C, and the ripening I is controlled by the liquid level in the ripening I reactor. The slurry output of the reactor, when the liquid level reaches and/or exceeds the set upper limit of the liquid level control, the ripening I discharge control valve is opened, and the ripening I slurry is output, when the liquid level reaches and/or is low At the lower limit of the set liquid level control, The ripening I discharge control valve does not output the ripening I slurry, and controls the exhaust emission of the ripening I reactor by the pressure in the ripening I reactor, and when the pressure reaches and/or exceeds the set upper limit of the pressure control, the opening is started. The maturation I exhaust control valve discharges the mature I exhaust gas, and when the pressure reaches and/or falls below a set lower limit of the pressure control, the maturation I exhaust control valve is closed, and the mature I exhaust gas is not discharged, the maturation II The operating pressure of the reactor is 2.0-3.0 MPaG, the operating temperature is 210-230 ° C, and the slurry output of the ripening II reactor is controlled by the liquid level in the ripening II reactor, when the liquid level reaches and/or exceeds the set When the upper limit of the liquid level is controlled, the ripening II discharge control valve is opened to output the ripening II slurry, and when the liquid level reaches and/or falls below the set lower limit of the liquid level control, the ripening II discharge control valve is closed. The mature II slurry is not output, and the exhaust gas of the ripening II reactor is controlled by the pressure in the ripening II reactor. When the pressure reaches and/or exceeds the set upper pressure control limit, the ripening II exhaust control valve is opened. Mature II exhaust gas when the pressure reaches When the pressure control lower limit is reached and/or lower than the set pressure control threshold, the ripening II exhaust gas control valve is closed, and the ripening II tail gas is not discharged. The operating pressure of the one crystallizing reactor is 1.5-2.0 MPaG, and the operating temperature is 179- Controlling the slurry output of the crystallization-reactor by crystallization at a liquid level in the reactor, and opening the crystallization-discharge control valve output when the liquid level reaches and/or exceeds a set upper limit of liquid level control Crystallizing a slurry, when the liquid level reaches and/or falls below a set lower limit of liquid level control, the crystallization-discharge control valve is closed, no crystal-slurry is output, and pressure control in the crystallization-reactor is performed. Crystallization of the exhaust gas of a reactor, when the pressure reaches and/or exceeds a set upper limit of pressure control, the crystallization-exhaust control valve is opened to discharge a crystallization gas, when the pressure reaches and/or falls below a set value When the lower limit of the pressure is controlled, the crystallization-exhaust control valve is closed, and the crystallization-off gas is not discharged. The operating pressure of the two-crystallization reactor is 0.2-0.4 MPaG, the operating temperature is 135-145 ° C, and the crystallization is performed in the two reactors. Liquid level control crystallization The slurry output of the device, when the liquid level reaches and/or exceeds the set upper limit of the liquid level control, the crystallization two discharge control valve is opened to output the crystal two slurry, when the liquid level reaches and/or is lower than the setting When the lower limit of the liquid level is controlled, the crystallization two discharge control valve is closed, the crystal two slurry is not output, and the exhaust gas of the crystallization two reactor is controlled by the pressure in the crystallization two reactor, when the pressure reaches and/or exceeds When the upper limit of the pressure control is set, the crystallization two-exhaust control valve is opened to discharge the crystallization two-tail gas, and when the pressure reaches and/or falls below the set lower pressure control limit, the crystallization two-exhaust control valve is closed, Discharging the crystallization of two off-gases, the slurry of the crystallization two reactor being fed to a feed tank of a filtration apparatus, preferably using any of the non-stirred reactors according to claim 1 or 2, the feed The operating pressure of the tank is normal pressure.