CN113680286A - Propylene carbonylation reaction system and method with recyclable catalyst - Google Patents
Propylene carbonylation reaction system and method with recyclable catalyst Download PDFInfo
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- CN113680286A CN113680286A CN202111011158.5A CN202111011158A CN113680286A CN 113680286 A CN113680286 A CN 113680286A CN 202111011158 A CN202111011158 A CN 202111011158A CN 113680286 A CN113680286 A CN 113680286A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 69
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 title claims abstract description 55
- 238000005810 carbonylation reaction Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 97
- 239000007789 gas Substances 0.000 claims abstract description 66
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 31
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000007789 sealing Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 10
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 4
- 239000001257 hydrogen Substances 0.000 claims abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims description 98
- 239000007788 liquid Substances 0.000 claims description 46
- 239000000945 filler Substances 0.000 claims description 12
- 238000012856 packing Methods 0.000 claims description 11
- 238000005192 partition Methods 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- 230000006315 carbonylation Effects 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 2
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 abstract description 22
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 abstract description 11
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 42
- 230000000052 comparative effect Effects 0.000 description 11
- 239000002245 particle Substances 0.000 description 11
- 239000007791 liquid phase Substances 0.000 description 8
- 238000012546 transfer Methods 0.000 description 5
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- QJEBFGJWFJQTAO-UHFFFAOYSA-N butanal;prop-1-ene Chemical compound CC=C.CCCC=O QJEBFGJWFJQTAO-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000012264 purified product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/005—Separating solid material from the gas/liquid stream
- B01J8/006—Separating solid material from the gas/liquid stream by filtration
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- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/005—Separating solid material from the gas/liquid stream
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/005—Separating solid material from the gas/liquid stream
- B01J8/007—Separating solid material from the gas/liquid stream by sedimentation
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- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
- B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
- B01J8/224—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid the particles being subject to a circulatory movement
- B01J8/228—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid the particles being subject to a circulatory movement externally, i.e. the particles leaving the vessel and subsequently re-entering it
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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Abstract
The invention provides a propylene carbonylation reaction system and a method with a recyclable catalyst, which comprises the following steps: a sealing plate is arranged in the reactor, a reaction section is arranged above the sealing plate, and a heating section is arranged below the sealing plate; a first micro-interface unit and a second micro-interface unit are sequentially arranged in the reaction section from top to bottom, and a propylene pipeline for introducing a propylene raw material and a synthesis gas pipeline for introducing carbon monoxide and hydrogen are arranged on the side wall of the reaction section; the top of the reaction section is an overflow area, and the bottom of the overflow area is inclined inwards to form an inclined plane; the lateral wall of the overflow area is provided with a material outlet, and the material outlet is connected with the heating section through an external pipeline so as to convey the product of the reaction section to the heating section. The reaction system can realize the recycling of the catalyst, improves the utilization rate of the catalyst, reduces the cost, has low overall energy consumption, high safety, low required reaction temperature and pressure and high butyraldehyde yield, and is worthy of wide popularization and application.
Description
Technical Field
The invention relates to the field of preparation of propylene hydroxylation, in particular to a propylene carbonylation reaction system and method with a recyclable catalyst.
Background
Butanol and octanol are important raw materials for synthesizing fine chemical products, and the preparation of butyraldehyde is the most important one-ring in the preparation process of butanol and octanol. In the prior art, the generation of butyraldehyde mainly takes synthesis gas and propylene as raw materials, a rhodium carbonyl/triphenylphosphine complex as a catalyst, mixed butyraldehyde is generated by reaction, and a butyraldehyde mixture is obtained by further rectification after the catalyst is separated; however, in the prior art, the carbonylation of propylene to butyraldehyde has the following problems:
1. when the synthesis gas and the propylene are subjected to the oxo reaction under the action of the catalyst, the synthesis gas and the propylene cannot be fully mixed, so that the reaction efficiency is low and the energy consumption is high in the reaction process, and the yield of the butyraldehyde is low and the production cost is high due to overhigh reaction temperature;
2. the catalyst used in the existing propylene carbonylation reaction is high in price and difficult to recycle, so that the cost is high.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a propylene carbonylation reaction system with a recyclable catalyst, which comprises a first micro interface unit and a second micro interface unit, wherein the first micro interface unit and the second micro interface unit are arranged to disperse and crush synthesis gas into micro bubbles at a micron level, so that the gas-liquid mass transfer area of propylene and the synthesis gas is increased, the retention time of the gas in a liquid phase is increased, the reaction efficiency is improved, the operation temperature and pressure in a reactor are reduced, and the safety and stability of the whole reaction system are improved; on the other hand, the overflow area is matched with the baffle plate, and the product is filtered, so that the catalyst flows back to the reaction section through the baffle plate and the inclined plane at the bottom of the overflow area, the loss of the catalyst is effectively prevented, the utilization rate of the catalyst is improved, and the cost is reduced.
The second purpose of the present invention is to provide a reaction method, which improves the utilization rate and catalytic efficiency of the catalyst, reduces the reaction temperature and pressure, and improves the conversion rate of the raw material by using the above reaction system.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a propylene carbonylation reaction system with a recyclable catalyst, which comprises: the reactor is internally provided with a sealing plate, a reaction section is arranged above the sealing plate, and a heating section is arranged below the sealing plate; a first micro-interface unit and a second micro-interface unit are sequentially arranged in the reaction section from top to bottom, and a propylene pipeline for introducing a propylene raw material and a synthesis gas pipeline for introducing carbon monoxide and hydrogen are arranged on the side wall of the reaction section; wherein the synthesis gas pipeline is communicated into the second micro-interface unit;
the top of the reaction section is an overflow area, and the bottom of the overflow area is inclined inwards to form an inclined plane; a material outlet is formed in the side wall of the overflow area and connected with the heating section through an external pipeline so as to convey a product of the reaction section into the heating section; and a baffle is arranged in the overflow area and close to the material outlet, and the baffle is matched with the inclined plane to filter the catalyst carried in the material.
In the prior art, synthesis gas and propylene cannot be fully mixed when undergoing a oxo reaction under the action of a catalyst, so that the reaction efficiency is low and the energy consumption is high in the reaction process, and the yield of butyraldehyde is low and the production cost is high due to overhigh reaction temperature; in addition, the catalyst used in the existing propylene carbonylation reaction is high in price and difficult to recycle, so that the cost is high
In order to solve the technical problems, the invention provides a propylene carbonylation reaction system with a recyclable catalyst, which separates the products in the reaction section through a baffle plate and the side wall of an overflow area, wherein undissolved catalyst particles are separated to the bottom along the side wall due to higher density and flow back to the reaction area along the inclined plane at the bottom of the overflow area to continuously participate in the reaction, thereby greatly reducing the loss of the catalyst, improving the utilization rate and the catalytic efficiency of the catalyst and saving the cost; in addition, the reaction system is also provided with a first micro-interface unit and a second micro-interface unit, and the synthesis gas is dispersed and crushed by the micro-interface and then mixed with the catalyst and propylene to form a gas-liquid emulsion, so that the mass transfer area between the gas phase and the liquid phase is increased, the reaction efficiency is increased, and the temperature and the pressure required by the reaction are reduced.
Preferably, a plurality of layers of grid plates are arranged between the first micro interface unit and the second micro interface unit and above the first micro interface unit. The grid plate is arranged to slow down liquid flow, so that the fully mixed flow is changed into plug flow, the liquid flow on the upper part is prevented from being back-mixed, the separation of gas and liquid is facilitated, meanwhile, undissolved catalyst particles are precipitated, and the service efficiency of the catalyst is improved.
Preferably, the propylene pipeline is divided into two branches, wherein one branch is connected with the first micro interface unit, and the other branch is connected with the lower part of the reaction section. The propylene entering from the lower part is used for providing a liquid phase environment for the dispersion and the crushing of the micro interface unit, and the propylene entering the first micro interface unit from the upper part is used for continuously reacting with the unreacted synthesis gas, so that the conversion rate of raw materials is improved.
Preferably, the first micro-interface unit and the second micro-interface unit are one or a combination of a plurality of pneumatic micro-interface generators, hydraulic micro-interface generators and hybrid micro-interface generators. Furthermore, the first micro-interface unit is a hydraulic micro-interface generator, and the second micro-interface unit is a hybrid micro-interface generator.
The reaction section is internally provided with a first micro interface unit and a second micro interface unit, and the first micro interface unit is positioned above the second micro interface unit. During reaction, the first micro-interface unit disperses and crushes the synthesis gas into micro bubbles, and then the micro bubbles are mixed with propylene and a catalyst to carry out carbonylation reaction, unreacted gas rises into the second micro-interface unit to carry out second dispersion and crushing to form a secondary micro-interface system, and the secondary micro-interface system continuously reacts with the propylene, so that the conversion rate of the synthesis gas is effectively improved. The first micro-interface unit is preferably a hydraulic micro-interface generator, so that unreacted gas can be trapped by utilizing the entrainment effect, and the conversion rate of raw materials is improved.
In the invention, a plurality of grid plates are arranged between the first micro interface unit and the second micro interface unit, so that gas and liquid are separated through the barrier effect of the grid plates, the gas enters the second micro interface unit and continues to participate in the reaction after the micro interface is crushed, and meanwhile, the backflow and backmixing of reaction products are prevented, thereby being beneficial to improving the conversion rate and the purity of the products; and a plurality of grid plates are also arranged above the second micro-interface unit, so that the flow velocity is reduced, undissolved catalyst particles are separated from a product, the catalyst sedimentation is promoted, and the utilization rate of the catalyst is improved.
The overflow area is arranged above the reaction section, and the baffle is arranged in the overflow area, so that undissolved catalyst particles in the product are separated, the catalyst is promoted to settle to the bottom, and flows back to the reaction area along the inclined plane at the bottom of the overflow area to continuously participate in the reaction, the loss of the catalyst is greatly reduced, the utilization rate and the catalytic efficiency of the catalyst are improved, and the cost is saved. Therefore, the invention improves the reaction efficiency, improves the utilization rate of the catalyst and reduces the reaction cost by combining and applying the micro-interface unit, the grid plate, the overflow area, the baffle plate and the like.
It will be appreciated by those skilled in the art that the micro-interface generator used in the present invention is described in the prior patents of the present inventor, such as the patents of application numbers CN201610641119.6, CN201610641251.7, CN201710766435.0, CN106187660, CN105903425A, CN109437390A, CN205833127U and CN 207581700U. The detailed structure and operation principle of the micro bubble generator (i.e. micro interface generator) is described in detail in the prior patent CN201610641119.6, which describes that "the micro bubble generator comprises a body and a secondary crushing member, wherein the body is provided with a cavity, the body is provided with an inlet communicated with the cavity, the opposite first end and second end of the cavity are both open, and the cross-sectional area of the cavity decreases from the middle of the cavity to the first end and second end of the cavity; the secondary crushing member is disposed at least one of the first end and the second end of the cavity, a portion of the secondary crushing member is disposed within the cavity, and an annular passage is formed between the secondary crushing member and the through holes open at both ends of the cavity. The micron bubble generator also comprises an air inlet pipe and a liquid inlet pipe. "the specific working principle of the structure disclosed in the application document is as follows: liquid enters the micro-bubble generator tangentially through the liquid inlet pipe, and gas is rotated at a super high speed and cut to break gas bubbles into micro-bubbles at a micron level, so that the mass transfer area between a liquid phase and a gas phase is increased, and the micro-bubble generator in the patent belongs to a pneumatic micro-interface generator.
In addition, the first patent 201610641251.7 describes that the primary bubble breaker has a circulation liquid inlet, a circulation gas inlet and a gas-liquid mixture outlet, and the secondary bubble breaker communicates the feed inlet with the gas-liquid mixture outlet, which indicates that the bubble breakers all need to be mixed with gas and liquid, and in addition, as can be seen from the following drawings, the primary bubble breaker mainly uses the circulation liquid as power, so that the primary bubble breaker belongs to a hydraulic micro-interface generator, and the secondary bubble breaker simultaneously introduces the gas-liquid mixture into an elliptical rotating ball for rotation, thereby realizing bubble breaking in the rotating process, so that the secondary bubble breaker actually belongs to a gas-liquid linkage micro-interface generator. In fact, the micro-interface generator is a specific form of the micro-interface generator, whether it is a hydraulic micro-interface generator or a gas-liquid linkage micro-interface generator, however, the micro-interface generator adopted in the present invention is not limited to the above forms, and the specific structure of the bubble breaker described in the prior patent is only one of the forms that the micro-interface generator of the present invention can adopt. Furthermore, the prior patent 201710766435.0 states that the principle of the bubble breaker is that high-speed jet flows are used to achieve mutual collision of gases, and also states that the bubble breaker can be used in a micro-interface strengthening reactor to verify the correlation between the bubble breaker and the micro-interface generator; moreover, in the prior patent CN106187660, there is a related description on the specific structure of the bubble breaker, see paragraphs [0031] to [0041] in the specification, and the accompanying drawings, which illustrate the specific working principle of the bubble breaker S-2 in detail, the top of the bubble breaker is a liquid phase inlet, and the side of the bubble breaker is a gas phase inlet, and the liquid phase coming from the top provides the entrainment power, so as to achieve the effect of breaking into ultra-fine bubbles, and in the accompanying drawings, the bubble breaker is also seen to be of a tapered structure, and the diameter of the upper part is larger than that of the lower part, and also for better providing the entrainment power for the liquid phase.
Since the micro-interface generator was just developed in the early stage of the prior patent application, the micro-interface generator was named as a micro-bubble generator (CN201610641119.6), a bubble breaker (201710766435.0) and the like in the early stage, and is named as a micro-interface generator in the later stage along with the continuous technical improvement, and the micro-interface generator in the present invention is equivalent to the micro-bubble generator, the bubble breaker and the like in the prior art, and has different names. In summary, the micro-interface generator of the present invention belongs to the prior art.
Preferably, the device also comprises a liquid-solid separation tower, wherein a partition plate is arranged in the liquid-solid separation tower, a first separation section is arranged below the partition plate, and a second separation section is arranged below the partition plate; a first sprayer is arranged in the first separation section and connected with the bottom of the heating section; a first pressure reducing valve is arranged between the heating section and the first sprayer, and a product in the heating section is reduced in pressure by the first pressure reducing valve and then sprayed into the first separation section by the first sprayer. The first pressure reducing valve is arranged for reducing the pressure of the product heated in the heating section, the liquid in the product is gasified, and the carried catalyst particles fall to the bottom of the first separation section, so that the separation of the catalyst is realized.
Preferably, a liquid distributor is arranged in the heating section, a heating plate is arranged below the liquid distributor, and the liquid distributor is connected with the material outlet. This is arranged to provide the product with a temperature prior to entering the first separation stage to facilitate gasification after entering the first separation stage.
Preferably, a first filler is arranged above the first sprayer; a heating pipe is arranged below the first sprayer, and a grid plate is arranged between the heating pipe and the first sprayer; the bottom of the first separation section is connected with the bottom of the reaction section. The heating pipe is arranged for accelerating the gasification of liquid in the product and promoting the separation of the product and the catalyst; the grid plates and the first packing are provided to prevent the catalyst from being carried in the gasified product, and further to facilitate the separation of the catalyst and the purification of the product.
Preferably, a separator outlet is arranged above the first separation section, and the separator outlet is positioned above the second sprayer; a third sprayer is arranged in the second separation section, and a second filler is arranged above the third sprayer; the separator outlet is connected with the third sprayer; and a second pressure reducing valve is arranged between the separator outlet and the third sprayer, and the separator is decompressed and gasified by the second pressure reducing valve and then enters the second separation section through the third sprayer. A second pressure reduction valve is provided to further vaporize the product and thereby further purify the product.
Preferably, the device also comprises a deep separation tower, wherein two layers of third packing are arranged in the deep separation tower, and a separator inlet is arranged on the side wall of the deep separation tower; said separator inlet is located between two of said layers of third packing; the separator inlet is connected with the top of the second separation section, a gas-liquid separator is arranged between the separator inlet and the second separation section, and products in the second separation section enter the deep separation tower through the separator inlet after being separated by the gas-liquid separator.
Preferably, a second sprayer is arranged above the first filler; a fourth sprayer is arranged above the second filler; the bottom of the deep separation tower is respectively connected with the second sprayer and the fourth sprayer; liquid at the bottom of the deep separation tower is respectively sprayed into the first separation section and the second separation section through the second sprayer and the fourth sprayer, so that gas in the first separation section and the second separation section can be cleaned, and catalyst particles are prevented from being carried by the gas.
Preferably, a second heat exchanger is arranged between the second separation section and the gas-liquid separator, and gas flowing out of the second separation section is condensed by the second heat exchanger and then enters the gas-liquid separator for separation and purification.
Preferably, the side wall of the reaction section is provided with a first circulation pipeline, an inlet of the first circulation pipeline is connected with the side wall of the reaction section, and an outlet of the first circulation pipeline is connected with the first micro-interface unit. Therefore, the hydraulic power can be provided for the first micro-interface unit, and the micro-interface dispersion efficiency is improved.
Preferably, a second circulating pipeline is arranged on the side wall of the reaction section; an inlet of the second circulating pipeline is connected with the side wall of the first grid plate layer, and an outlet of the second circulating pipeline is connected with the second micro interface unit and the first sprayer respectively; and a first heat exchanger is arranged on the second circulating pipeline. Therefore, hydraulic power can be provided for the second micro-interface unit, and micro-interface dispersion efficiency is improved.
Preferably, the deep separation column is provided with a first product outlet and a second product outlet; the first product outlet is positioned between two layers of the third packing, and the second product outlet is positioned at the bottom of the deep separation column.
Preferably, the bottom of the second separation section is connected with the lower part of the deep separation tower. And the material settled at the bottom of the second separation section enters the bottom of the deep separation tower and returns to the first separation section and the second separation section through the deep separation tower to be continuously separated.
Preferably, the top of the reaction section is connected with a third heat exchanger, after the gas at the top of the reaction section is subjected to heat exchange and cooling by the third heat exchanger, one part of the gas flows back to the reaction section, and the other part of the gas is extracted for recycling.
Preferably, the gas-liquid separator is provided with a non-condensable gas outlet; and a gas outlet is formed in the top of the deep separation tower. The gas discharged from the non-condensable gas outlet and the gas discharged from the gas outlet are mainly propylene and propane, and the extracted gas is compressed by a compressor and then recycled.
The invention also provides a method for adopting the propylene carbonylation reaction system with the recyclable catalyst, which comprises the following steps:
dispersing and crushing the synthesis gas through a micro interface, and then carrying out hydroxyl synthesis reaction with propylene in the presence of a catalyst.
Preferably, the hydroxyl synthesis reaction temperature is 60-180 ℃, and the pressure is 0.5-5.0 MPa; preferably, the hydroxyl synthesis reaction temperature is 80-87 ℃, and the pressure is 1.1-1.6 MPa; in practice, the temperature can be chosen to be 60 deg.C, 70 deg.C, 80 deg.C, 90 deg.C, 100 deg.C, and the pressure can be chosen to be 0.8MPa, 0.9MPa, 1.0MPa, 1.1MPa, 1.2MPa, 1.3MPa, 1.4 MPa.
In the present invention, the type of the catalyst is not particularly limited, and it may be any catalyst suitable for catalyzing the carbonylation of propylene.
Specifically, the reaction method comprises the step of dispersing and crushing the synthesis gas by arranging the micro interface unit in the reactor, so that the synthesis gas is crushed into micro bubbles with the diameter of more than or equal to 1 mu m and less than 1mm before the carbonylation reaction, the mass transfer area of a phase boundary is increased, the reaction pressure is reduced, and the reaction efficiency is improved.
The butyraldehyde product obtained by the reaction method has good quality and high yield. And the preparation method has the advantages of low reaction temperature, greatly reduced pressure and remarkably reduced cost.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the propylene carbonylation reaction system with the recyclable catalyst, the first micro-interface unit and the second micro-interface unit are arranged to disperse and crush the synthesis gas into micro-bubbles at the micron level, so that the gas-liquid mass transfer area of propylene and the synthesis gas is increased, the retention time of the gas in a liquid phase is increased, the reaction efficiency is improved, the operation temperature and pressure in the reactor are reduced, and the safety and stability of the whole reaction system are improved;
(2) the overflow area is matched with the baffle plate, so that the product is filtered, and the catalyst flows back to the reaction section through the baffle plate and the inclined plane at the bottom of the overflow area, thereby effectively preventing the loss of the catalyst, improving the utilization rate of the catalyst and reducing the cost;
(3) through set up the grid tray above first little interface unit and between first little interface unit and the second little interface unit, can slow down liquid flow, be favorable to undissolved catalyst particle to subside to improve the availability factor of catalyst.
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 a propylene carbonylation reaction system according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a reactor provided in an embodiment of the present invention;
fig. 3 is a schematic structural diagram of a liquid-solid separation column according to an embodiment of the present invention.
Description of the drawings:
10-a reactor; 101-a heating plate;
102-a liquid distributor; 103-sealing plate;
104-a second micro-interface unit; 105-a second circulation line;
106 — a first heat exchanger; 107-a first micro-interface unit;
108-first circulation line; 109-a baffle;
110-grid plate; 111-material outlet;
112-overflow area; 20-a liquid-solid separation column;
201-heating pipe; 202-a first sprayer;
203-a first filler; 204-a second sprayer;
205-a separator; 206-a second pressure relief valve;
207-a third sprayer; 208-a separator outlet;
209-a second filler; 210-a fourth sprayer;
30-deep separation column; 301-a separator inlet;
302-a first product outlet; 303-a second product outlet;
304-a third packing layer; 40-a first pressure relief valve;
50-a second heat exchanger; 60-a gas-liquid separator;
70-a third heat exchanger; 80-propylene line;
90-syngas line.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In order to more clearly illustrate the technical solution of the present invention, the following description is made in the form of specific embodiments.
Example 1
Referring to fig. 1 to 3, the present example provides a catalyst-recyclable propylene carbonylation reaction system, including: a reactor 10, a liquid-solid separation column 20, and a depth separation column 30. Wherein, a sealing plate 103 is arranged in the reactor 10, a reaction section is arranged above the sealing plate 103, and a heating section is arranged below the sealing plate; a first micro-interface unit 107 and a second micro-interface unit 104 are sequentially arranged in the reaction section from top to bottom, and a propylene pipeline 80 for introducing a propylene raw material and a synthesis gas pipeline 90 for introducing carbon monoxide and hydrogen are arranged on the side wall of the reaction section; wherein the syngas line 90 leads into the second micro interface unit 104; the propylene line 80 is divided into two branches, one of which is connected to the first micro-interface unit 107 and the other of which is connected to the lower part of the reaction section.
As shown in fig. 2, the top of the reaction section is an overflow area 112, and the bottom of the overflow area 112 is inclined inwards to form an inclined plane; the side wall of the overflow area 112 is provided with a material outlet 111, and the material outlet 111 is connected with the heating section through an external pipeline so as to convey a product of the reaction section into the heating section; a baffle plate 109 is arranged in the overflow area 112 near the material outlet 111, and the baffle plate 109 is matched with the inclined plane to filter the catalyst carried in the material.
Wherein, be provided with liquid distributor 102 in the heating section, be provided with heating plate 101 below liquid distributor 102, liquid distributor 102 links to each other with material export 111.
With continued reference to fig. 2, a plurality of grid plates 110 are disposed between the first micro interface unit 107 and the second micro interface unit 104 and above the first micro interface unit 107. During the reaction, the grid plate 110 can slow down the liquid flow, promote the sedimentation of the undissolved catalyst particles, and improve the use efficiency of the catalyst.
Specifically, the first micro-interface unit 107 and the second micro-interface unit 104 may be one or a combination of a pneumatic micro-interface generator, a hydraulic micro-interface generator and a hybrid micro-interface generator. In this embodiment, the first micro interface unit 107 is a hydraulic micro interface generator, and the second micro interface unit 104 is a hybrid micro interface generator.
With continued reference to fig. 2, the side wall of the reaction section is provided with a first circulation pipeline 108 and a second circulation pipeline 105, the inlet of the first circulation pipeline 108 is connected with the side wall of the reaction section, and the outlet is connected with the first micro interface unit 107; the inlet of the second circulating pipeline 105 is connected with the side wall of the first grid plate 110 layer, and the outlet is respectively connected with the second micro interface unit 104 and the first sprayer 202; the second circulation line 105 is provided with a first heat exchanger 106.
The top of the reaction section is connected with a third heat exchanger 70, after the gas at the top of the reaction section is subjected to heat exchange and cooling through the third heat exchanger 70, one part of the gas flows back to the reaction section, and the other part of the gas is extracted for recycling.
As shown in fig. 3, a partition 205 is provided in the liquid-solid separation column 20, a first separation section is provided below the partition 205, and a second separation section is provided below the partition 205; a first sprayer 202 is arranged in the first separation section, and the first sprayer 202 is connected with the bottom of the heating section; a first pressure reducing valve 40 is arranged between the heating section and the first sprayer 202, and the product in the heating section is reduced in pressure by the first pressure reducing valve 40 and then sprayed into the first separation section by the first sprayer 202. The first pressure reducing valve 40 is provided to reduce the pressure of the heated product in the heating section, the liquid in the product is gasified, and the carried catalyst particles fall to the bottom of the first separation section, thereby realizing the separation of the catalyst.
With continued reference to fig. 3, a first filler 203 is disposed above the first sprayer 202; a heating pipe 201 is arranged below the first sprayer 202, and a grid plate 110 is arranged between the heating pipe 201 and the first sprayer 202; the bottom of the first separation section is connected with the bottom of the reaction section. The heating pipe 201 is provided to accelerate the vaporization of the liquid in the product and promote the separation of the product from the catalyst; the grid plates 110 and the first packing 203 are provided to prevent the gasified product from carrying the catalyst, and to further facilitate the separation of the catalyst and the purification of the product.
Specifically, a separator outlet 208 is arranged above the first separation section, and the separator outlet 208 is positioned above the second sprayer 204; a third sprayer 207 is arranged in the second separation section, and a second filler 209 is arranged above the third sprayer 207; the separated matter outlet 208 is connected with a third sprayer 207; a second pressure reducing valve 206 is arranged between the separator outlet 208 and the third sprayer 207, and the separator is decompressed and gasified by the second pressure reducing valve 206 and then enters the second separation section through the third sprayer 207.
As shown in fig. 1, two layers of third packing are arranged in the deep separation tower 30, and a separator inlet 301 is arranged on the side wall of the deep separation tower 30; separator inlet 301 is located between two layers of third packing layer 304; the separator inlet 301 is connected with the top of the second separation section, a gas-liquid separator 60 is arranged between the separator inlet 301 and the second separation section, a second heat exchanger 50 is arranged between the second separation section and the gas-liquid separator 60, and gas flowing out of the second separation section enters the gas-liquid separator 60 for separation and purification after being condensed by the second heat exchanger 50. The purified product enters the deep separation column 30 through the separator inlet 301.
Specifically, the bottom of the second separation section is connected to the lower part of the deep separation column 30. A second sprayer 204 is arranged above the first filler 203; a fourth sprayer 210 is arranged above the second filler 209; the bottom of the deep separation tower 30 is respectively connected with a second sprayer 204 and a fourth sprayer 210; during reaction, the liquid at the bottom of the deep separation tower 30 is respectively sprayed and dropped into the first separation section and the second separation section through the second sprayer 204 and the fourth sprayer 210, and the gas in the first separation section and the second separation section is cleaned to prevent the gas from carrying catalyst particles.
In the present embodiment, the deep separation column 30 is provided with a first product outlet 302 and a second product outlet 303; the first product outlet 302 is located between two layers of the third packing, and the second product outlet 303 is located at the bottom of the deep separation column 30. When the product purity at the bottom of the deep separation column 30 is sufficient, it is directly withdrawn from the second product outlet 303.
In this embodiment, the gas-liquid separator 60 is provided with a noncondensable gas outlet; the top of the deep separation column 30 is provided with a gas outlet. The gas discharged from the non-condensable gas outlet and the gas discharged from the gas outlet are mainly propylene and propane, and the extracted gas is compressed by a compressor and then recycled.
Comparative example 1
The present example differs from example 1 only in that the first micro-interface unit is not used in the present example.
Comparative example 2
The present example differs from example 1 only in that the first and second micro-interface units are not used in the present example.
Comparative example 3
The difference between this example and example 1 is that in this example no grid is provided above the first micro-interface unit.
Examples of the experiments
The reaction systems of example 1 and comparative examples 1 to 3 were used to conduct the carbonylation of propylene under the following reaction conditions: the weight ratio of the used propylene, synthesis gas and catalyst is 1: 0.57: 0.29, respectively under the pressure of 1.1Mpa and the temperature of 80 ℃; the pressure is 1.3Mpa, and the temperature is 83 ℃; the reaction was carried out under a pressure of 1.6MPa and at a temperature of 87 ℃. The reaction results are given in the following table:
TABLE 1 (pressure 1.1MPa, temperature 80 ℃ C.)
| Conversion of propylene | Butyraldehyde yield | |
| Example 1 | 98.9％ | 98.0％ |
| Comparative example 1 | 94.8％ | 96.5％ |
| Comparative example 2 | 89.5％ | 94.3％ |
| Comparative example 3 | 95.2％ | 96.7％ |
TABLE 2 (pressure 1.3MPa, temperature 83 deg.C)
TABLE 3 (pressure 1.6MPa, temperature 87 ℃ C.)
| Conversion of propylene | Butyraldehyde yield | |
| Example 1 | 99.4％ | 98.3％ |
| Comparative example 1 | 95.3％ | 97.1％ |
| Comparative example 2 | 91.0％ | 95.3％ |
| Comparative example 3 | 95.8％ | 97.3％ |
As can be seen from tables 1 to 3, the reaction efficiency of example 1 is significantly better than that of comparative examples 1 to 3. The invention adopts the arrangement mode of combining the first micro interface unit and the second micro interface unit, utilizes the first micro interface unit to capture unreacted synthesis gas, disperses the synthesis gas into micro bubbles and then continuously reacts with propylene, thereby improving the conversion rate of raw materials; the product liquid flow is changed from the fully mixed flow to the plug flow by arranging the grid plate, then the layering is formed by the space between the baffle and the side wall of the overflow area, and the catalyst particles flow back to the reaction area from the bottom, so that the utilization rate of the catalyst is improved, the loss of the catalyst is reduced, and the reaction efficiency is improved.
In a word, compared with the reaction system for preparing butyraldehyde by propylene carbonylation in the prior art, the reaction system disclosed by the invention can realize the recycling of the catalyst, the utilization rate of the catalyst is improved, the cost is reduced, the overall energy consumption of the system is low, the safety is high, the required reaction temperature and pressure are low, the butyraldehyde yield is high, and the method is worthy of wide popularization and application.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A catalyst-recyclable propylene carbonylation reaction system, comprising: the reactor is internally provided with a sealing plate, a reaction section is arranged above the sealing plate, and a heating section is arranged below the sealing plate; a first micro-interface unit and a second micro-interface unit are sequentially arranged in the reaction section from top to bottom, and a propylene pipeline for introducing a propylene raw material and a synthesis gas pipeline for introducing carbon monoxide and hydrogen are arranged on the side wall of the reaction section; wherein the synthesis gas pipeline is communicated into the second micro-interface unit;
the top of the reaction section is an overflow area, and the bottom of the overflow area is inclined inwards to form an inclined plane; a material outlet is formed in the side wall of the overflow area and connected with the heating section through an external pipeline so as to convey a product of the reaction section into the heating section; and a baffle is arranged in the overflow area and close to the material outlet, and the baffle is matched with the inclined plane to filter the catalyst carried in the material.
2. The catalyst-recyclable propylene carbonylation reaction system according to claim 1, wherein a plurality of grid plates are arranged between the first micro interface unit and the second micro interface unit and above the first micro interface unit.
3. The catalyst-recyclable propylene carbonylation reaction system according to claim 1, wherein the propylene line is divided into two branches, one branch being connected to the first micro-interface unit and the other branch being connected to a lower portion of the reaction section.
4. The catalyst-recyclable propylene carbonylation reaction system of claim 1, wherein the first micro-interface unit and the second micro-interface unit are one or a combination of a pneumatic micro-interface generator, a hydraulic micro-interface generator and a hybrid micro-interface generator.
5. The catalyst-recyclable propylene carbonylation reaction system according to claim 1, further comprising a liquid-solid separation column, wherein a partition is arranged in the liquid-solid separation column, a first separation section is arranged below the partition, and a second separation section is arranged below the partition; a first sprayer is arranged in the first separation section and connected with the bottom of the heating section; a first pressure reducing valve is arranged between the heating section and the first sprayer, and a product in the heating section is reduced in pressure by the first pressure reducing valve and then sprayed into the first separation section by the first sprayer.
6. The catalyst-recyclable propylene carbonylation reaction system according to claim 5, wherein a first filler is disposed above the first shower; a heating pipe is arranged below the first sprayer, and a grid plate is arranged between the heating pipe and the first sprayer; the bottom of the first separation section is connected with the bottom of the reaction section.
7. The catalyst-recyclable propylene carbonylation reaction system according to claim 6, wherein a separator outlet is provided above the first separation section, and the separator outlet is located above the second shower; a third sprayer is arranged in the second separation section, and a second filler is arranged above the third sprayer; the separator outlet is connected with the third sprayer; and a second pressure reducing valve is arranged between the separator outlet and the third sprayer, and the separator is decompressed and gasified by the second pressure reducing valve and then enters the second separation section through the third sprayer.
8. The catalyst-recyclable propylene carbonylation reaction system according to claim 5, further comprising a deep separation tower, wherein two layers of third packing are arranged in the deep separation tower, and a separator inlet is arranged on the side wall of the deep separation tower; said separator inlet is located between two of said layers of third packing; the separator inlet is connected with the top of the second separation section, a gas-liquid separator is arranged between the separator inlet and the second separation section, and products in the second separation section enter the deep separation tower through the separator inlet after being separated by the gas-liquid separator.
9. A process for the carbonylation of propylene using a catalyst according to any one of claims 1 to 8, comprising the steps of:
dispersing and crushing the synthesis gas through a micro interface, and then carrying out hydroxyl synthesis reaction with propylene in the presence of a catalyst.
10. The reaction method of claim 9, wherein the hydroxyl synthesis reaction temperature is 60 to 180 ℃ and the pressure is 0.5 to 5.0 MPa; preferably, the hydroxyl synthesis reaction temperature is 80-87 ℃, and the pressure is 1.1-1.6 MPa.
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