CN111574345A - Intelligent strengthening reaction system and process for built-in micro-interface unit for producing PTA (purified terephthalic acid) by PX (para-xylene) - Google Patents
Intelligent strengthening reaction system and process for built-in micro-interface unit for producing PTA (purified terephthalic acid) by PX (para-xylene) Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 334
- 238000000034 method Methods 0.000 title claims abstract description 22
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical compound CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 title claims description 116
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 title claims description 101
- 230000008569 process Effects 0.000 title abstract description 19
- 238000005728 strengthening Methods 0.000 title description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 57
- GOUHYARYYWKXHS-UHFFFAOYSA-N 4-formylbenzoic acid Chemical compound OC(=O)C1=CC=C(C=O)C=C1 GOUHYARYYWKXHS-UHFFFAOYSA-N 0.000 claims description 40
- LPNBBFKOUUSUDB-UHFFFAOYSA-N p-toluic acid Chemical compound CC1=CC=C(C(O)=O)C=C1 LPNBBFKOUUSUDB-UHFFFAOYSA-N 0.000 claims description 38
- 238000004519 manufacturing process Methods 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 20
- 238000007254 oxidation reaction Methods 0.000 claims description 19
- FXLOVSHXALFLKQ-UHFFFAOYSA-N p-tolualdehyde Chemical compound CC1=CC=C(C=O)C=C1 FXLOVSHXALFLKQ-UHFFFAOYSA-N 0.000 claims description 16
- 230000009471 action Effects 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 239000007791 liquid phase Substances 0.000 claims description 13
- 239000003054 catalyst Substances 0.000 claims description 12
- 238000012544 monitoring process Methods 0.000 claims description 11
- 239000000839 emulsion Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000007670 refining Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000011541 reaction mixture Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 13
- 238000005265 energy consumption Methods 0.000 abstract description 9
- 239000007810 chemical reaction solvent Substances 0.000 abstract description 6
- 239000000047 product Substances 0.000 description 11
- 239000007789 gas Substances 0.000 description 10
- 238000012546 transfer Methods 0.000 description 10
- 230000008901 benefit Effects 0.000 description 8
- 239000000376 reactant Substances 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 4
- 238000007086 side reaction Methods 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 description 2
- 229940011182 cobalt acetate Drugs 0.000 description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 229940071125 manganese acetate Drugs 0.000 description 2
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- HJUGFYREWKUQJT-UHFFFAOYSA-N tetrabromomethane Chemical compound BrC(Br)(Br)Br HJUGFYREWKUQJT-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- -1 paraxylene PX Chemical compound 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
- C07C51/23—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of oxygen-containing groups to carboxyl groups
- C07C51/235—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of oxygen-containing groups to carboxyl groups of —CHO groups or primary alcohol groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/373—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by introduction of functional groups containing oxygen only in doubly bound form
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00054—Controlling or regulating the heat exchange system
- B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
- B01J2219/00058—Temperature measurement
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0873—Materials to be treated
- B01J2219/0877—Liquid
Abstract
The invention provides an intelligent reinforced reaction system and process of a built-in micro-interface unit for producing PTA by PX, wherein the system comprises: the system comprises a reactor, a micro-interface unit arranged in the reactor and an intelligent control module; the reactor comprises a shell, an inner barrel and a circulating heat exchange device, wherein the inner barrel and the part of the inner barrel are arranged inside the shell in a concentric mode, the circulating heat exchange device is arranged outside the shell, the bottom end of the inner barrel is connected to the upper portion of the inner bottom surface of the shell in a closed mode, the top end of the inner barrel is open, the shell and an area between the inner barrels are a first reaction area, a second reaction area and a third reaction area are sequentially arranged inside the inner barrel from top to bottom, and the circulating heat exchange device is respectively connected with the inner barrel and the micro-interface unit. The invention effectively solves the problems that the reaction solvent acetic acid is greatly wasted at high temperature and high pressure and the product TA can not be taken out in time in the existing process of producing PTA by PX, thereby greatly reducing the energy consumption, saving the acetic acid solvent and improving the reaction efficiency.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to an intelligent enhanced reaction system and process of a built-in micro-interface unit for producing PTA (pure terephthalic acid) by PX (p-xylene).
Background
The oxidation reaction process for producing TA (terephthalic acid) from PX (p-xylene) is very complicated, mainly comprising 4 steps, namely p-xylene (PX) → p-Tolualdehyde (TALD) → p-toluic acid (p-TA) → p-carboxybenzaldehyde (4-CBA) → Terephthalic Acid (TA), and the 4 oxidation reactions in the reaction process are series reactions, which generally use acetic acid as a solvent and cobalt acetate, manganese acetate and hydrobromic acid (or tetrabromomethane) as catalysts.
At present, in the existing PTA production technology, 4 main steps in the oxidation reaction process are all carried out in the same reactor, although the reaction rate constants of the 4 steps are different by dozens of times, a mixed reaction process is adopted, different conditions are not given for different reactions, reaction solvent acetic acid is greatly wasted under high temperature and high pressure, and meanwhile, a product TA cannot be taken out in time, so that the energy consumption is high, the acetic acid consumption is large, and the reaction efficiency is low.
Disclosure of Invention
In view of this, the invention provides an intelligent enhanced reaction system and process of a built-in micro-interface unit for producing PTA by PX, and aims to solve the problems that a reaction solvent acetic acid is greatly wasted at high temperature and high pressure and a product TA cannot be taken out in time in the existing PX production PTA process.
In one aspect, the present invention provides an intelligent enhanced reaction system of a built-in micro interface unit for PX production PTA, comprising: the system comprises a reactor, a micro-interface unit arranged in the reactor and an intelligent control module; wherein the content of the first and second substances,
the reactor comprises a shell, an inner cylinder concentrically arranged in the shell and a circulating heat exchange device partially arranged outside the shell, the bottom end of the inner cylinder is connected to the inner bottom surface of the shell in a closed mode, the top end of the inner cylinder is open, the area between the shell and the inner cylinder is a first reaction area, a second reaction area and a third reaction area are sequentially arranged in the inner cylinder from top to bottom, and the circulating heat exchange device is respectively connected with the inner cylinder and the micro-interface unit;
the micro interface unit comprises a first micro interface generator and a second micro interface generator, the first micro interface generator is respectively arranged at the bottoms of the first reaction zone, the second reaction zone and the third reaction zone and is used for crushing air serving as a reaction raw material into micro bubbles with the diameter of more than or equal to 1 mu m and less than 1mm, the second micro interface generator is arranged at the upper end of the second reaction zone, is opposite to the first micro interface generator arranged at the bottom of the second reaction zone and is used for sucking unreacted air collected at the top of the reactor into the interior of the second reaction zone and crushing the unreacted air into the micro bubbles under the power action of reaction liquid in the second reaction zone conveyed by the circulating heat exchange device;
the intelligent control module is arranged on the reactor and comprises a PLC (programmable logic controller), a sensor and a cloud processor, the sensor transmits acquired electric signals to the cloud processor, the cloud processor screens and compares the acquired electric signals in a cloud database according to reaction parameters returned by the sensor, and corresponding commands are sent to the PLC after the optimal control parameters are screened.
Further, in the above-mentioned built-in micro-interface unit intelligence of PX production PTA intensifies reaction system, the PLC controller includes:
the first PLC controller is used for controlling the reaction temperature and the reaction pressure of the first reaction zone;
the second PLC controller is used for controlling the reaction temperature and the reaction pressure of the second reaction zone; (ii) a
And the third PLC is used for controlling the generator of the micro-interface unit to work.
Further, in the above-mentioned built-in micro-interface unit intelligence of PX production PTA intensifies reaction system, the sensor includes:
the temperature sensors are respectively arranged in the first reaction zone, the second reaction zone, the third reaction zone and the circulating heat exchange device and are used for monitoring the temperature of the system in real time;
and the pressure sensors are respectively arranged in the reactors and used for monitoring the system pressure in real time.
Further, in the intelligent enhanced reaction system of the built-in micro-interface unit for producing PTA by PX, the first reaction zone is a reaction zone in which p-xylene is converted into p-tolualdehyde, and p-tolualdehyde is converted into p-toluic acid, the second reaction zone is a reaction zone in which p-toluic acid is converted into p-carboxybenzaldehyde, and the third reaction zone is a reaction zone in which p-carboxybenzaldehyde is converted into terephthalic acid.
Further, in the intelligent enhanced reaction system of the built-in micro-interface unit for producing PTA by PX, the height of the inner cylinder is 4/5 of the height of the outer shell.
Further, in the intelligent enhanced reaction system of the built-in micro-interface unit for producing PTA by PX, the volume of the first reaction zone accounts for 45% of the total reaction volume in the reactor, the volume of the second reaction zone accounts for 53.5% of the total reaction volume in the reactor, and the volume of the third reaction zone accounts for 1.5% of the total reaction volume in the reactor.
Further, in the intelligent enhanced reaction system of the built-in micro-interface unit for producing PTA by PX, the first micro-interface generator is pneumatic, and the second micro-interface generator is hydraulic.
On the other hand, the invention also provides an intelligent enhanced reaction process of the built-in micro-interface unit for producing PTA by PX, which is characterized by comprising the following steps:
the method comprises the following steps of enabling a mixture of p-xylene, acetic acid and a catalyst to enter a first reaction zone between a shell and an inner barrel of a reactor through the lower end of the reactor, simultaneously introducing air into a micro-interface generator which is arranged at the bottom of the first reaction zone and controlled by a third PLC (programmable logic controller) to break the mixture into micro-bubbles with the diameter of more than or equal to 1 mu m and less than 1mm, forming emulsion with a liquid-phase material, controlling the reaction temperature and the reaction pressure in real time through the first PLC, converting the p-xylene into p-tolualdehyde under the action of the catalyst, and simultaneously converting the p-tolualdehyde into p-toluic acid, wherein the unreacted air leaves a liquid level and rises above the reactor, and monitoring the internal reaction temperature in real time through a temperature sensor arranged in the first reaction zone;
along with the mixed liquid which continuously reacts in the first reaction zone overflows from the first reaction zone into the inner cylinder, the reaction temperature and the reaction pressure are controlled by a second PLC (programmable logic controller), meanwhile, air which is crushed into micro-bubbles is introduced into the zone through a first micro-interface generator arranged at the bottom of a second reaction zone arranged at the upper part of the inner cylinder, and reacts with the p-toluic acid in the mixed liquid under the action of the catalyst to generate p-carboxybenzaldehyde, the internal reaction temperature of the reaction zone is monitored in real time through a temperature sensor arranged in the second reaction zone, wherein unreacted air leaves from the liquid level and rises to the upper part of the reactor, and is sent to the bottom of the zone through a gas guide tube to continuously participate in the generation reaction of the p-carboxybenzaldehyde under the entrainment action of a second micro-interface generator arranged at the upper part of the second reaction zone under the power action of a circulating heat exchange device, after multiple cycles, under the pressure pushing, the tail gas enters a tail gas treatment unit from an outlet at the top of the reactor;
the p-carboxybenzaldehyde generated by the reaction in the second reaction zone passes through a wave-proof grating and enters a third reaction zone below the second reaction zone, the p-carboxybenzaldehyde and micro-bubbles introduced into a first micro-interface generator arranged at the bottom of the third reaction zone are subjected to oxidation reaction under the action of the catalyst to generate terephthalic acid, the terephthalic acid and unreacted reaction mixture are discharged through an outlet below the reactor and enter a subsequent separation and refining section, and the reaction pressure of a system is monitored in real time through a plurality of pressure sensors arranged in the reactor in the reaction process.
Further, in the intelligent enhanced reaction process of the built-in micro-interface unit for producing PTA by PX, the volume of the first reaction zone accounts for 45% of the total reaction volume in the reactor, the volume of the second reaction zone accounts for 53.5% of the total reaction volume in the reactor, and the volume of the third reaction zone accounts for 1.5% of the total reaction volume in the reactor.
Further, in the intelligent enhanced reaction process of the built-in micro-interface unit for producing PTA by PX, the first micro-interface generator is pneumatic, and the second micro-interface generator is hydraulic.
Compared with the prior art, the intelligent strengthening reaction system and the intelligent strengthening reaction process for the built-in micro-interface unit for PX production PTA have the advantages that the rate difference of four-step reaction for PX production PTA is considered, a sectional reaction concept is adopted, the interior of the reactor is provided with three different reaction areas, and different reaction steps are performed in each reaction area, so that different conditions are provided for different reaction stages in the same reactor, especially the contradiction that an acetic acid solvent cannot bear high-temperature oxidation conditions is solved, water is used as a solvent for p-TA oxidation reaction, the problems that a large amount of reaction solvent acetic acid is wasted at high temperature and high pressure and a product TA cannot be taken out in time in the existing PX production PTA process are effectively solved, and further energy consumption is greatly reduced, the acetic acid solvent is saved, and the reaction efficiency is improved.
Particularly, the intelligent strengthening reaction system and the process of the built-in micro-interface unit for producing PTA by PX provided by the invention have the advantages that the micro-interface generator is arranged in each reaction zone in the reactor, air is crushed in each reactor to be micro-bubbles with the diameter of more than or equal to 1 mu m and less than 1mm, and the micro-bubbles and liquid-phase materials form emulsion, so that the mass transfer area between the air and the liquid-phase materials is effectively increased, the thickness of a liquid film is reduced, the mass transfer resistance is reduced, the energy consumption is effectively reduced, and the reaction efficiency is improved.
Furthermore, the intelligent enhanced reaction system and process of the built-in micro-interface unit for PX production PTA provided by the invention have the advantages that the temperature in the reaction process is effectively controlled in the reaction process by arranging the circulating heat exchange device, the mixing uniformity of all reaction materials in the reactor is ensured, all reactants can fully participate in the reaction, the utilization rate of the reactants is greatly improved, side reactions caused by local temperature unevenness are prevented, and the quality of products is improved to a certain extent.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
fig. 1 is a schematic structural diagram of an intelligent enhanced reaction system of a built-in micro-interface unit for PX production PTA according to an embodiment of the present invention.
In the figure: 10 is a shell, 11 is an inner cylinder, 13 is a first reaction zone, 14 is a second reaction zone, 15 is a third reaction zone, 16 is a pipeline, 17 is a wave-proof grid, 18 is a defoaming net, 19 is a gas-guide tube, 20 is a first micro-interface generator, 21 is a second micro-interface generator, 121 is a heat exchanger, and 122 is a pressure pump 122.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
Referring to fig. 1, an intelligent enhanced reaction system of a built-in micro-interface unit for PX production PTA according to an embodiment of the present invention includes: the system comprises a reactor, a micro-interface unit arranged in the reactor and an intelligent control module; wherein the content of the first and second substances,
the reactor comprises: the heat exchanger comprises a shell 10, an inner cylinder 11 arranged in the shell 10 and a circulating heat exchange device; the bottom end of the inner cylinder 11 is connected to the inner bottom surface of the shell 10, and the top end is open; the area between the outer shell 10 and the inner cylinder 11 is a first reaction zone 13, the first reaction zone 13 is a reaction zone for converting p-xylene into p-tolualdehyde and p-tolualdehyde into p-toluic acid (i.e. the first two-step oxidation reaction for PX producing PTA), the inner cylinder 11 is sequentially provided with a second reaction zone 14 and a third reaction zone 15 from top to bottom, the second reaction zone 14 is a reaction zone for converting p-toluic acid into p-carboxybenzaldehyde (i.e. the third-step oxidation reaction for PX producing PTA), and the third reaction zone 15 is a reaction zone for converting p-carboxybenzaldehyde into terephthalic acid (i.e. the fourth-step oxidation reaction for PX producing PTA); the circulating heat exchange device is respectively connected with the inner cylinder 11 and the micro-interface unit, is formed by connecting a heat exchanger 121 and a pressure pump 122 through a pipeline 16, is used for effectively controlling the temperature in the reaction process, simultaneously ensures the mixing uniformity among all reaction materials in the reactor, ensures that all reactants can fully participate in the reaction, further greatly improves the utilization rate of the reactants, simultaneously prevents the occurrence of side reactions caused by uneven local temperature, and improves the quality of products to a certain extent. In addition, the top end of the housing 10 is further opened with a tail gas channel, and the bottom is provided with a mixed material for taking out the reaction product terephthalic acid in the third reaction zone 15. It can be understood that, in the invention, the rate difference of the four-step reaction for producing PTA by PX is considered, a sectional type reaction concept is adopted, the reactor is internally provided with a first reaction area, a second reaction area and a third reaction area which are different, different reaction steps are carried out in each reaction area, the purpose of giving different conditions to different reaction stages in the same reactor is effectively realized, especially the contradiction that an acetic acid solvent cannot bear high-temperature oxidation conditions is solved, water is used as a solvent of p-TA oxidation reaction, the problems that a large amount of acetic acid which is a reaction solvent in the existing PX production PTA process is wasted at high temperature and high pressure and a product TA cannot be taken out in time are effectively solved, the energy consumption is greatly reduced, the acetic acid solvent is saved, and the reaction efficiency is improved.
In this embodiment, a shell 10, an inner tube 11 concentrically disposed inside the shell 10, and a circulating heat exchange device partially disposed outside the shell 10, the inner tube 11 is connected to the inner bottom surface of the shell 10 in a closed manner at the bottom end, has an open top end, and extends upwards to 4/5 of the height of the shell 10 along the axial direction of the reactor, the annular region between the shell 10 and the inner tube 11 is a first reaction zone 13 for performing the first two-step oxidation reaction for PX to produce PTA, the volume of the first reaction zone is 45% of the total reaction volume in the reactor, the interior of the inner tube 11 is sequentially from top to bottom a second reaction zone 14 for performing the third-step oxidation reaction for PX to produce PTA and a third reaction zone 15 for performing the fourth-step oxidation reaction for PX to produce PTA, the volume of the second reaction zone is 53.5% of the total reaction volume in the reactor, the volume of the third reaction zone accounts for 1.5 percent of the total reaction volume in the reactor, and a wave-proof grating 17 is arranged between the third reaction zone and the third reaction zone; the circulating heat exchange device is respectively connected with the inner cylinder 11 and the micro-interface unit and is formed by connecting a heat exchanger 121 and a pressure pump 122 through a pipeline 16, so that the temperature in the reaction process is effectively controlled in the reaction process, power is provided for a second micro-interface generator connected with the circulating heat exchange device, the mixing uniformity of all reaction materials in the reactor is ensured, the reactants can fully participate in the reaction, the utilization rate of the reactants is greatly improved, meanwhile, the occurrence of side reaction caused by uneven local temperature is prevented, and the quality of products is improved to a certain extent. In addition, the upper part of the shell 10 is also provided with a defoaming net 16, the top end part is also provided with a tail gas channel, and the bottom part is provided with a mixed material for taking out a reaction product terephthalic acid in the third reaction zone 15. It can be understood that, in the embodiment, in consideration of the rate difference of the four-step reaction for producing PTA by PX, a sectional reaction concept is adopted, the reactor is internally provided with three different reaction regions, and different reaction steps of each reaction region realize that different conditions are applied to different reaction stages in the same reactor, and particularly, the reaction volume of each reaction region is determined according to the reaction difficulty or the reaction time of different reaction stages, so that each reaction in the process of producing PTA by PX can be sufficiently performed, further, the reaction efficiency of each reaction region is greatly improved while the contradiction that an acetic acid solvent cannot bear high-temperature oxidation conditions is solved, and finally, the yield of products is effectively improved.
The micro-interface unit includes: the first micro-interface generator 20 is arranged at the bottom of the first reaction zone 13, the second reaction zone 14 and the third reaction zone 15, and is used for crushing air serving as a reaction raw material into micro-bubbles with the diameter of more than or equal to 1 micrometer and less than 1mm in each reactor zone inside the reactor so as to provide the reaction raw material for reactions in different stages; the second micro-interface generator 21 is disposed at the upper end of the second reaction zone 14, is opposite to the first micro-interface generator 20 disposed at the bottom of the second reaction zone 14, and is used for sucking the unreacted air collected at the top of the reactor into the interior of the reactor under the power of the reaction liquid in the second reaction zone 14 conveyed by the circulating heat exchange device to be broken into the micro-bubbles. The specific construction of the micro-interfacial surface generator is shown in the prior patent of the present inventor, such as the patent of publication No. 106215730A, and the core of the micro-interfacial surface generator is bubble collapse, which is not described in detail. The reaction mechanism and the control method of the micro-interface generator 4 are disclosed in the prior patent CN107563051B by the present inventor, and are not described in detail herein. It can be understood that in the invention, through arranging the micro-interface generator in each reaction zone in the reactor, the air is crushed in each reaction zone to be crushed into micro-bubbles with the diameter of more than or equal to 1 μm and less than 1mm, and the micro-bubbles and the liquid-phase material form emulsion, so that the mass transfer area between the air and the liquid-phase material is effectively increased, the thickness of the liquid film is reduced, the mass transfer resistance is reduced, the energy consumption is effectively reduced, and the reaction efficiency is improved.
In this embodiment, the first micro-interface generator 20 and the second micro-interface generator 21, the first micro-interface generator 20 is a pneumatic micro-interface generator, which is respectively disposed at the bottom of the first reaction zone 13, the second reaction zone 14 and the third reaction zone 15, and is used to break air as a reaction raw material into micro-bubbles with a diameter of 1 μm or more and less than 1mm in each reactor zone inside the reactor, so as to provide the reaction raw material for different stages of reactions; the second micro-interface generator 21 is a hydraulic micro-interface generator, is arranged at the upper end of the second reaction zone 14, is opposite to the first micro-interface generator 20 arranged at the bottom of the second reaction zone 14, and is used for sucking unreacted air collected at the top of the reactor into the interior of the second reaction zone 14 under the power action of the reaction liquid in the second reaction zone and conveyed by the circulating heat exchange device to be broken into the micro-bubbles. It can be understood that, in the embodiment, the micro interface generator is arranged in each reaction zone in the reactor, and the air is crushed in each reaction zone to be crushed into micro bubbles with the diameter of more than or equal to 1 μm and less than 1mm, so as to form emulsion with the liquid-phase material, thereby effectively increasing the mass transfer area between the air and the liquid-phase material, reducing the thickness of the liquid film, reducing the mass transfer resistance, further effectively reducing the energy consumption and improving the reaction efficiency.
The intelligent control module is arranged on the reactor and mainly comprises a PLC (programmable logic controller), a sensor and a cloud processor; the sensor is used for acquiring the reaction pressure and the reaction temperature in each reaction zone in the reaction system in real time and transmitting the acquired electric signals of the pressure and the temperature to the cloud processor; and the cloud processor screens and compares the reaction parameters transmitted back by the sensors in a cloud database, and sends a corresponding command to the PLC after screening out the optimal pressure and temperature control parameters so as to control the temperature and pressure of the reaction in each reaction zone. It can be understood that the cloud processor can be, but is not limited to, a computer, the computer comprises cloud receiving, cloud computing, cloud storage and cloud control, the cloud processor is electrically or wirelessly connected with the PLC controller and the sensor, the sensor returns data through the cloud receiving, the received data is stored through the uniform storage, the cloud database is analyzed, screened and compared through the cloud computing, optimal control parameters are optimized, the PLC controller is controlled through the cloud control, and therefore process parameters are adjusted rapidly and accurately; meanwhile, PLC is an abbreviation of programmable logic controller, which is a digital electronic device with a microprocessor, and is a digital logic controller for automation control, and can load control instructions into a memory at any time for storage and execution. The programmable controller is modularly assembled by an internal CPU, an instruction and data memory, an input/output unit, a power supply module, a digital analog unit and the like, and the PLC is widely applied to the current industrial control field, and the principle of controlling electric appliances is not repeated herein.
In this embodiment, the intelligent control module includes a PLC controller, a sensor, and a cloud processor; the sensor is used for acquiring the reaction pressure and the reaction temperature in each reaction zone in the reaction system in real time and transmitting the acquired electric signals of the pressure and the temperature to the cloud processor; and the cloud processor screens and compares the reaction parameters transmitted back by the sensors in a cloud database, and sends a corresponding command to the PLC after screening out the optimal pressure and temperature control parameters so as to control the temperature and pressure of the reaction in each reaction zone. Wherein, the PLC controller includes: the first PLC controller is used for controlling the reaction temperature and the reaction pressure of the first reaction zone; the second PLC controller is used for controlling the reaction temperature and the reaction pressure of the second reaction zone; and the third PLC is used for controlling the generator of the micro-interface unit to work. The sensor includes: the temperature sensors are respectively arranged in the first reaction zone, the second reaction zone, the third reaction zone and the circulating heat exchange device and are used for monitoring the temperature of the system in real time; and the pressure sensors are respectively arranged in the reactors and used for monitoring the system pressure in real time.
Please refer to fig. 1, the working process of the intelligent enhanced reaction system of the built-in micro-interface unit for PX PTA production in this embodiment is:
firstly, a mixture of raw materials of p-xylene, acetic acid and catalysts (cobalt acetate, manganese acetate and hydrobromic acid) enters a first reaction zone 13 between a shell 10 and an inner cylinder 11 of a reactor through the lower end of the reactor (the volume of the zone accounts for 45% of the total reaction volume in the reactor, the setting is that the time for the first two-step reaction for producing PTA by PX is about 45% of the total time of all four-step reaction), meanwhile, air enters a first micro-interface generator 20 controlled by a third PLC controller at the bottom of the first reaction zone 13 in the reactor, is crushed into micro-bubbles with the diameter of more than or equal to 1 mu m and less than 1mm, and is mixed with liquid-phase materials in the zone to form emulsion, the reaction temperature and the reaction pressure are controlled in real time by the first PLC controller, and the internal reaction temperature is monitored in real time by a temperature sensor arranged in the first reaction zone, effectively increasing the contact area between the air and the liquid-phase reaction materials, and further promoting the reaction in the area. Two reactions before PX produces PTA occur in the area, namely, p-xylene is converted into p-tolualdehyde, p-tolualdehyde is converted into p-toluic acid, and overflows to the inner barrel, and unreacted gas leaves the liquid level (wave line), passes through the defoaming net 18 and rises to the upper part of the reactor. In this region, the fluid is in a steady plug flow, completing primarily the first reaction PX → TALD and the second reaction TALD → p-TA.
Then, air broken into the micro-bubbles is introduced into the region through a first micro-interface generator arranged at the bottom of a second reaction zone at the upper part of the inner cylinder and controlled by a third PLC controller, the air is mixed with liquid-phase materials in the region to form emulsion and reacts with p-toluic acid in the mixed solution under the action of the catalyst to generate p-carboxybenzaldehyde, wherein unreacted gas leaves the liquid level (wave line), passes through a defoaming net 18 and rises to the upper part of the reactor, unreacted air leaves the liquid level and rises to the upper part of the reactor, and the unreacted air is sent to the bottom of the second reaction zone 14 at the upper part of the inner cylinder 11 through a gas guide pipe 19 under the entrainment action of a second micro-interface generator 21 arranged at the upper part of the second reaction zone 14 under the power of a circulating heat exchange device and under the entrainment action of a second micro-interface generator controlled by the third PLC controller, continuously participating in the reaction, monitoring the internal reaction temperature in real time through a temperature sensor arranged in the second reaction zone, and after multiple cycles, taking the temperature as tail gas to enter a tail gas treatment unit from an outlet at the top of the reactor under the pressure pushing condition, so that the utilization rate of oxygen in the air can be improved. In this region, two micro-interfacial generators (the first micro-interfacial generator 20 and the second micro-interfacial generator 21) opposed up and down are used to generate a vigorous and complete mixed flow to perform the third step of reaction p-TA → 4-CBA (this step has the slowest reaction speed, so the effect of complete mixed flow is to be made to enhance the mass transfer and accelerate the reaction at the same time, this region occupies 53.5% of the total reaction volume in the reactor for the same reason). Meanwhile, the temperature of the materials in the region is controlled by a circulating heat exchange device outside the reactor, the bubbles generated by the second micro-interface generator 21 in the second reaction zone 14 move downwards, the bubbles generated by the first micro-interface generator 20 move upwards, and the bubbles are violently collided, so that the turbulence of the fluid is strengthened, smaller bubbles can be generated, the gas-liquid two-phase contact area is further increased, and the mass transfer and reaction are accelerated.
Finally, the product in the second reaction zone 14 passes through the wave grating 17 into the third reaction zone 15 (this zone has a volume of 1.5% of the total reaction volume in the reactor for the same reason), which is turned into a plug flow by the wave grating 17, and the fourth reaction step 4-CBA → TA is carried out, i.e., the conversion of p-carboxybenzaldehyde into terephthalic acid. Air enters the reaction zone through a first micro-interface generator 20 at the bottom of the reaction zone to perform the oxidation reaction. Discharging a reaction product (terephthalic acid TA) together with unreacted paraxylene PX, a solvent, a catalyst, byproducts and the like through an outlet pipeline below the reactor, entering a subsequent separation and refining section, and monitoring the reaction pressure of a system in real time through a plurality of pressure sensors arranged in the reactor in the reaction process.
Obviously, the intelligent strengthening reaction system and the intelligent strengthening reaction process for the built-in micro-interface unit for producing the PTA by the PX have the advantages that the rate difference of four-step reactions for producing the PTA by the PX is considered, the segmented reaction concept is adopted, the interior of the reactor is provided with three different reaction areas, and the reaction steps of the reaction areas are different, so that different conditions are provided for different reaction stages in the same reactor, especially the contradiction that an acetic acid solvent cannot bear high-temperature oxidation conditions is solved, water is used as a solvent for p-TA oxidation reaction, the problems that a large amount of acetic acid which is a reaction solvent in the existing PX production PTA process is wasted at high temperature and high pressure, and meanwhile, the product TA cannot be taken out in time are effectively solved, the energy consumption is greatly reduced, the acetic acid solvent is saved, and the reaction efficiency is improved.
Particularly, the intelligent strengthening reaction system and the process of the built-in micro-interface unit for producing PTA by PX provided by the invention have the advantages that the micro-interface generator is arranged in each reaction zone in the reactor, air is crushed in each reactor to be micro-bubbles with the diameter of more than or equal to 1 mu m and less than 1mm, and the micro-bubbles and liquid-phase materials form emulsion, so that the mass transfer area between the air and the liquid-phase materials is effectively increased, the thickness of a liquid film is reduced, the mass transfer resistance is reduced, the energy consumption is effectively reduced, and the reaction efficiency is improved.
Furthermore, the intelligent enhanced reaction system and process of the built-in micro-interface unit for PX production PTA provided by the invention have the advantages that the temperature in the reaction process is effectively controlled in the reaction process by arranging the circulating heat exchange device, the mixing uniformity of all reaction materials in the reactor is ensured, all reactants can fully participate in the reaction, the utilization rate of the reactants is greatly improved, side reactions caused by local temperature unevenness are prevented, and the quality of products is improved to a certain extent.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. An intelligent enhanced reaction system of a built-in micro-interface unit for producing PTA by PX is characterized by comprising: the system comprises a reactor, a micro-interface unit arranged in the reactor and an intelligent control module; wherein the content of the first and second substances,
the reactor comprises a shell, an inner cylinder concentrically arranged in the shell and a circulating heat exchange device partially arranged outside the shell, the bottom end of the inner cylinder is connected to the inner bottom surface of the shell in a closed manner, the top end of the inner cylinder extends to the top end of the reactor, the area between the shell and the inner cylinder is a first reaction area, a second reaction area and a third reaction area are sequentially arranged in the inner cylinder from top to bottom, and the circulating heat exchange device is respectively connected with the inner cylinder and the micro-interface unit;
the micro interface unit comprises a first micro interface generator and a second micro interface generator, the first micro interface generator is respectively arranged at the bottoms of the first reaction zone, the second reaction zone and the third reaction zone and is used for crushing air serving as a reaction raw material into micro bubbles with the diameter of more than or equal to 1 mu m and less than 1mm, the second micro interface generator is arranged at the upper end of the second reaction zone, is opposite to the first micro interface generator arranged at the bottom of the second reaction zone and is used for sucking unreacted air collected at the top of the reactor into the interior of the second reaction zone and crushing the unreacted air into the micro bubbles under the power action of reaction liquid in the second reaction zone conveyed by the circulating heat exchange device;
the intelligent control module is arranged on the reactor and comprises a PLC (programmable logic controller), a sensor and a cloud processor, the sensor transmits acquired electric signals to the cloud processor, the cloud processor screens and compares the acquired electric signals in a cloud database according to reaction parameters returned by the sensor, and corresponding commands are sent to the PLC after the optimal control parameters are screened.
2. The intelligent enhanced reaction system of built-in micro-interface unit for PX production PTA of claim 1, wherein the PLC controller comprises:
the first PLC controller is used for controlling the reaction temperature and the reaction pressure of the first reaction zone;
the second PLC controller is used for controlling the reaction temperature and the reaction pressure of the second reaction zone;
and the third PLC is used for controlling the generator of the micro-interface unit to work.
3. The intelligent reaction system of the built-in micro-interface unit for PTA production by PX of claim 1, wherein said sensor comprises:
the temperature sensors are respectively arranged in the first reaction zone, the second reaction zone, the third reaction zone and the circulating heat exchange device and are used for monitoring the temperature of the system in real time;
and the pressure sensors are respectively arranged in the reactors and used for monitoring the system pressure in real time.
4. The intelligent enhanced reaction system with built-in micro-interface unit for PX production PTA as claimed in claim 1, wherein said first reaction zone is a reaction zone for converting p-xylene into p-tolualdehyde, p-tolualdehyde into p-toluic acid, said second reaction zone is a reaction zone for converting p-toluic acid into p-carboxybenzaldehyde, and said third reaction zone is a reaction zone for converting p-carboxybenzaldehyde into terephthalic acid.
5. The intelligent enhanced reaction system of built-in micro interface unit for PX production PTA of claim 4, wherein the height of said inner barrel is 4/5 of the height of said outer shell.
6. The intelligent enhanced reaction system with built-in micro interface unit for PTA production as claimed in claim 5, wherein the volume of the first reaction zone is 45% of the total reaction volume in the reactor, the volume of the second reaction zone is 53.5% of the total reaction volume in the reactor, and the volume of the third reaction zone is 1.5% of the total reaction volume in the reactor.
7. The intelligent enhanced reaction system of built-in micro-interface unit for PX production PTA of claim 1, wherein the first micro-interface generator is pneumatic and the second micro-interface generator is hydraulic.
8. An intelligent enhanced reaction process of a built-in micro-interface unit for producing PTA by PX is characterized by comprising the following steps:
the method comprises the following steps of enabling a mixture of p-xylene, acetic acid and a catalyst to enter a first reaction zone between a shell and an inner barrel of a reactor through the lower end of the reactor, simultaneously introducing air into a micro-interface generator which is arranged at the bottom of the first reaction zone and controlled by a third PLC (programmable logic controller) to break the mixture into micro-bubbles with the diameter of more than or equal to 1 mu m and less than 1mm, forming emulsion with a liquid-phase material, controlling the reaction temperature and the reaction pressure in real time through the first PLC, converting the p-xylene into p-tolualdehyde under the action of the catalyst, and simultaneously converting the p-tolualdehyde into p-toluic acid, wherein the unreacted air leaves a liquid level and rises above the reactor, and monitoring the internal reaction temperature in real time through a temperature sensor arranged in the first reaction zone;
the reaction mixed liquid overflows from the first reaction zone to the inner cylinder along with the continuous reaction of the reaction in the first reaction zone, the reaction temperature and the reaction pressure are controlled by a second PLC controller, meanwhile, the third PLC controller controls a first micro-interface generator arranged at the bottom of a second reaction zone at the upper part of the inner cylinder to introduce air crushed into micro-bubbles into the zone, and reacts with the p-toluic acid in the mixed solution under the action of the catalyst to generate p-carboxybenzaldehyde, and the temperature sensor arranged in the second reaction zone is used for monitoring the internal reaction temperature in real time, wherein unreacted air leaves the liquid level and rises to the upper part of the reactor, and passes through the entrainment of a second micro-interface generator arranged at the upper part of the second reaction zone under the power action of a circulating heat exchange device, is sent to the bottom of the area through a gas-guide tube to continuously participate in the generation reaction of the p-carboxybenzaldehyde;
the p-carboxybenzaldehyde generated by the reaction in the second reaction zone passes through a wave-proof grating and enters a third reaction zone below the second reaction zone, the p-carboxybenzaldehyde and micro-bubbles introduced into a first micro-interface generator arranged at the bottom of the third reaction zone are subjected to oxidation reaction under the action of the catalyst to generate terephthalic acid, the terephthalic acid and unreacted reaction mixture are discharged through an outlet below the reactor and enter a subsequent separation and refining section, and the reaction pressure of a system is monitored in real time through a plurality of pressure sensors arranged in the reactor in the reaction process.
9. The intelligent enhanced reaction process of built-in micro-interface unit for PX production PTA as claimed in claim 8, wherein the volume of said first reaction zone is 45% of the total reaction volume in said reactor, the volume of said second reaction zone is 53.5% of the total reaction volume in said reactor, and the volume of said third reaction zone is 1.5% of the total reaction volume in said reactor.
10. The intelligent enhanced reaction process of built-in micro-interface unit for PX production PTA of claim 8, wherein said first micro-interface generator is pneumatic and said second micro-interface generator is hydraulic.
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