CN212954952U - Propylene oxidation system acrylic acid pilot-scale plant with tail gas circulation - Google Patents
Propylene oxidation system acrylic acid pilot-scale plant with tail gas circulation Download PDFInfo
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- CN212954952U CN212954952U CN202020712091.2U CN202020712091U CN212954952U CN 212954952 U CN212954952 U CN 212954952U CN 202020712091 U CN202020712091 U CN 202020712091U CN 212954952 U CN212954952 U CN 212954952U
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- 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
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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
- C07C45/33—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 of CHx-moieties
- C07C45/34—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 of CHx-moieties in unsaturated compounds
- C07C45/35—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 of CHx-moieties in unsaturated compounds in propene or isobutene
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C47/00—Compounds having —CHO groups
- C07C47/20—Unsaturated compounds having —CHO groups bound to acyclic carbon atoms
- C07C47/21—Unsaturated compounds having —CHO groups bound to acyclic carbon atoms with only carbon-to-carbon double bonds as unsaturation
- C07C47/22—Acryaldehyde; Methacryaldehyde
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C57/00—Unsaturated compounds having carboxyl groups bound to acyclic carbon atoms
- C07C57/02—Unsaturated compounds having carboxyl groups bound to acyclic carbon atoms with only carbon-to-carbon double bonds as unsaturation
- C07C57/03—Monocarboxylic acids
- C07C57/04—Acrylic acid; Methacrylic acid
Abstract
The utility model discloses a propylene oxidation system acrylic acid pilot scale device with tail gas circulation. The pilot plant comprises the following units: the device comprises a feeding unit, a reaction product separation unit and a tail gas treatment unit; all units are connected in sequence according to the material flow direction; wherein the reaction unit comprises a first acrolein reactor and a second acrylic acid reactor; the tail gas treatment unit comprises a dryer and a gas circulation compressor, and the tail gas discharged from the reaction product separation unit enters the dryer and then returns to the feeding unit through the gas circulation compressor. The utility model discloses make pilot scale reaction feeding simulation use the industrial grade feeding of circulation tail gas to constitute, when the steady operation of reaction process, really appraise catalyst performance.
Description
This application claims priority from the following prior applications: the invention discloses a prior application with the name of 'a pilot plant and a process for preparing acrylic acid by propylene oxidation with tail gas circulation', wherein the patent application number is 202010346538.3 which is submitted to the intellectual property office of China at 27.4.4.2020. The entire contents of said prior application are incorporated by reference into the present application.
Technical Field
The utility model belongs to acrylic acid production field, concretely relates to propylene oxidation system acrylic acid pilot scale device with tail gas circulation.
Background
The process for preparing acrylic acid by mixing propylene with air and steam and performing two-step oxidation under the action of a catalyst. In the acrylic acid production device, in order to operate more stably, tail gas generated in the reaction process can be recycled to the reaction system to replace steam as diluent gas in the reaction process to adjust the concentration of propylene, so that the aim of operating more stably is fulfilled. For example, CN200720094566.0 reports that, for a process route and an automatic control system for directly recycling reaction tail gas without incineration treatment to a reaction system, the circulation amount of the circulation tail gas is adjusted by on-line analysis and detection in cooperation with DCS, so as to solve the problem of reaction mixture ratio interference caused by complex components of the circulation tail gas and avoid explosion hazard.
CN2008801004789.8 reports a method for producing acrylic acid by oxidizing propane on an industrial scale, wherein the gaseous reaction product after separation of acrylic acid contains unreacted propane, and at least a part of carbon dioxide is removed therefrom and recycled to the reaction system as a recycle gas. The control of the recycle gas is not described in detail.
The pilot plant as a means of evaluating the performance of the reaction was aimed at bringing the process flow and operating conditions as close as possible to those of an industrial plant. However, the tail gas has a complex composition, contains a large amount of water vapor, and is difficult to control the flow rate, and although the tail gas recycling technology is already applied to industrial production, the tail gas recycling technology has not been reported in a pilot plant scale device. Because the tail gas circulation amount is difficult to control, in the prior art, the tail gas is generally treated as waste gas after product separation. Therefore, the existing pilot plant test technology cannot well simulate actual production and better evaluate the performance of the catalyst.
SUMMERY OF THE UTILITY MODEL
The utility model provides a pilot plant of propylene oxidation system acrylic acid, it includes following unit: the device comprises a feeding unit, a reaction product separation unit and a tail gas treatment unit; all units are connected in sequence according to the material flow direction;
wherein the reaction unit comprises a first acrolein reactor and a second acrylic acid reactor;
the tail gas treatment unit comprises a dryer and a gas circulation compressor, and the tail gas discharged from the reaction product separation unit enters the dryer and then returns to the feeding unit through the gas circulation compressor.
According to an embodiment of the present invention, the feeding unit comprises a feeding and flow control system of propylene, nitrogen and/or air and water, a preheater, a vaporizer and a mixer;
the propylene feeding and flow control system, the nitrogen feeding and flow control system and/or the air feeding and flow control system and the water feeding and flow control system are connected in parallel;
the nitrogen feeding and flow control system and/or the air feeding and flow control system are/is connected with the preheater, the water feeding and flow control system is connected with the vaporizer, and the propylene feeding and flow control system is connected with the mixer; the material from the preheater and the water vapor from the vaporizer were mixed with propylene in a mixer.
According to the utility model discloses an embodiment, the material export of a acrolein reactor and the material entry of two acrylic acid reactors are connected, a acrolein reactor and two acrylic acid reactors all include the heating furnace and the reactor of connecting in order, an acrolein reactor with the material exit linkage of blender. The first acrolein reaction vessel comprises an acrolein reactor and a molten salt heating system, and the second acrylic acid reaction vessel comprises an acrylic acid reactor and a molten salt heating system.
Optionally, a sample collector for the collected products is provided between the feed outlet of a acrolein reactor and the feed inlet of a diacrylic acid reactor.
According to an embodiment of the present invention, the reverse product collecting sampler comprises a first condenser, a first gas sample collector, a first liquid sample collector; and a material outlet of the first inverse acrolein reactor is connected with a first condenser, a gas phase outlet of the first condenser is connected with the first gas sample collector, and a liquid phase outlet of the first condenser is connected with the first liquid sample collector. The collected gas and liquid samples were analyzed by chromatography and chemical titration to measure the gas sample composition and the liquid sample composition for yield calculation. Wherein, during acrolein detection, a hard glass tube or stainless steel tube chromatographic column with the inner diameter of 3mm and the length of 3.1-4.1m is adopted, wherein the granularity of the filled monomer chromosorb W is 80-100 meshes, and the stationary liquid Thermon-1000 (5%) + H3PO4(0.5%), the column temperature is 50-70 deg.C, and the vaporization chamber temperature is 100-150 deg.C.
According to the utility model discloses an embodiment, reaction product separation element is including the heat exchanger and the absorption tower of connecting in order, the material entry of heat exchanger with the material exit linkage of two anti acrylic acid reactors, absorption tower exhaust tail gas with the material entry linkage of desicator.
Optionally, a secondary reaction product collecting sampler is arranged between the material outlet of the secondary reaction acrylic acid reactor and the material inlet of the heat exchanger.
According to an embodiment of the present invention, the second reaction product collecting sampler comprises a second condenser, a second gas sample collector, a second liquid sample collector; and a material outlet of the second anti-acrylic acid reactor is connected with a second condenser, a gas phase outlet of the second condenser is connected with the second gas sample collector, and a liquid phase outlet of the second condenser is connected with the second liquid sample collector. The collected gas and liquid samples were analyzed by chromatography and chemical titration to measure the gas sample composition and the liquid sample composition for calculating the product yield. Wherein, when detecting acrylic acid, a hard glass tube chromatographic column with the inner diameter of 3mm and the length of 3.1-4.1m is adopted, wherein the granularity of monomer chromosorb W is 80-100 meshes, and fixing liquid Thermon-1000 (5%) + H is filled3PO4(0.5%), the column temperature is 120 ℃ and 150 ℃, and the vaporization chamber temperature is 150 ℃ and 180 ℃.
According to the utility model discloses an embodiment, reaction product separator still includes parallelly connected heavy ends collecting system and acrylic acid collecting system, absorption tower exhaust heavy ends gets into heavy ends collecting system, absorption tower exhaust acrylic acid gets into acrylic acid collecting system.
According to the utility model discloses an embodiment, optionally, is provided with the circulation tail gas sample thief between the export of desicator and gas circulation compressor entry. And the gas sample collected by the circulating tail gas sampler is subjected to chromatographic analysis to test the composition of the tail gas sample.
According to the utility model discloses an embodiment, the tail gas processing unit still includes exhaust emission system, exhaust emission system with the desicator is parallelly connected relation, and with the tail gas discharge mouth of absorption tower is connected.
According to an embodiment of the invention, the connection is a connection known in the art, such as a pipeline connection.
In accordance with embodiments of the present invention, one skilled in the art can appreciate that valves may be provided on the pipeline, and/or pumps may be provided between the devices, as desired.
The utility model also provides a process of propylene oxidation system acrylic acid pilot scale, the process includes following step:
and after preheating, mixing nitrogen and/or air and water vapor with propylene, carrying out two-step oxidation reaction on the mixed material, carrying out heat exchange on a reaction product obtained in the second step, separating to obtain tail gas, acrylic acid and heavy components, drying the tail gas part, returning the dried tail gas part to the reaction system as a feed, and allowing the rest tail gas to enter a tail gas discharge system.
According to an embodiment of the present invention, the pilot plant process is performed in the above pilot plant.
According to the embodiment of the utility model, in the initial reaction stage, the feeding amount of propylene is 5-20% (e.g. 10-20%) of the design load, after the temperature of the feeding bed layer is stabilized for the first time, the flow of propylene is gradually increased to 50-80% (e.g. 50-70%) of the design load, and after the feeding of propylene is increased each time, the feeding of propylene is continuously increased after the temperature of the bed layer is determined to be stabilized; then part of tail gas is circularly returned to the system to be used as feed, and the consumption of the circulating tail gas is 10-100% (such as 30-70%) of the total amount of the tail gas discharged by heat exchange; and continuously adjusting the flow of the propylene to the designed load, and entering a stable period of the reaction.
According to the embodiment of the present invention, after the reaction enters the stable period, the feed ratio of the raw material gas is not particularly limited, and the general volume ratio of propylene, oxygen, nitrogen and water vapor of the industrial device is 1:1.7:2.4: 1.
According to an embodiment of the present invention, the loading of the catalyst in the above two oxidation steps is 500ml to 5L, preferably 1 to 2.5L. Wherein, the catalyst can be selected from catalysts known in the field. The reaction conditions for the oxidation of the monopropylene to acrolein and the oxidation of the dipropylaldehyde to acrylic acid, including space velocity, reaction temperature and pressure, are not particularly limited and those skilled in the art can select the known reaction conditions for the oxidation of propylene to acrylic acid.
According to an embodiment of the present invention, in the two-step oxidation reaction, the first oxidation reaction is performed in the first acrolein reaction vessel, and the second oxidation reaction is performed in the second acrylic acid reaction vessel.
According to an embodiment of the invention, the acrylic acid and heavy ends respectively enter the corresponding collection system.
According to an embodiment of the invention, the process further comprises: collecting the products of the first oxidation reaction, and performing chromatographic and chemical titration analysis on the collected gas sample and liquid sample, and testing the gas sample composition and the liquid sample composition to calculate the yield.
According to an embodiment of the invention, the process further comprises: collecting the products of the second oxidation reaction, and performing chromatographic and chemical titration analysis on the collected gas sample and liquid sample to test the gas sample composition and the liquid sample composition for calculating the yield.
According to an embodiment of the invention, the process further comprises: and a circulating tail gas sampler is arranged between the outlet of the dryer and the inlet of the gas circulating compressor, and the gas sample collected by the circulating tail gas sampler is subjected to chromatographic analysis to test the composition of the tail gas sample.
The utility model has the advantages that:
the utility model discloses an in pilot scale propylene oxidation technology, through increasing gas dryer and gas circulation compressor at tail gas processing unit, after one of them part of tail gas that will separate out takes off vapor, return reaction system, accurate control reaction charge-in system propylene, steam, air and circulation tail gas ratio, make pilot scale reaction feeding simulation use the industrial grade feeding of circulation tail gas and constitute, in the steady operation of reaction process, really appraise catalyst performance.
The utility model discloses a dry turns into dry tail gas with moisture tail gas, has avoided under less flow operating mode, and the flow that makes tail gas circulation compressor operation difficulty cause is wayward because of the interference of vapor. And because the pilot plant process adopts stable propylene raw materials, the composition change of tail gas caused by the fluctuation of the raw materials is avoided, the process can well simulate an industrial production device with circulating tail gas, and the performance of the catalyst is more truly evaluated.
Drawings
FIG. 1 is a schematic view showing the structure of a pilot plant for producing acrylic acid by oxidizing propylene in example 1.
Reference numerals: 1-preheater, 2-vaporizer, 3-mixer, 4-first acrolein reaction vessel, 5-second acrylic acid reaction vessel, 6-heat exchanger, 7-absorption tower, 8-drier and 9-gas circulation compressor.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the following embodiments. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention. All the technologies realized based on the above mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
In the following examples and comparative examples, acrolein was detected by using a hard glass tube column having an inner diameter of 3mm and a length of 3.1m, packed with a monomer chromosorb W of 90 mesh size, a stationary liquid Thermon-1000 (5%) + H3PO4(0.5%), column temperature 60 deg.C, vaporization chamber temperature 140 deg.C;
when detecting acrylic acid, a hard glass tube chromatographic column with the inner diameter of 3mm and the length of 3.1m is adopted, and monomer chromosorb W with the granularity of 90 meshes and stationary liquid Thermon-1000 (5%) + H are filled3PO4(0.5%), column temperature 130 deg.C, vaporization chamber temperature 140 deg.C.
Example 1
As shown in FIG. 1, the pilot plant for producing acrylic acid by propylene oxidation comprises: the device comprises a feeding unit, a reaction unit, a separation unit and a tail gas treatment unit. The units are connected by pipelines.
Wherein, the feeding unit consists of a propylene feeding and flow control system, an air feeding and flow control system and a preheater 1, a water feeding and flow control system and a vaporizer 2, and a mixer 3;
the propylene feed and flow control system, the air feed and flow control system, and the water feed and flow control system are in a parallel relationship. The propylene feeding and flow control system is connected with the mixer 3, the air feeding and flow control system is connected with the preheater 1, the water feeding and flow control system is connected with the vaporizer 2, and the material from the preheater and the water vapor from the vaporizer jointly enter the mixer 3 to be mixed with the propylene.
The reaction unit comprises a acrolein reaction vessel 4 and a diacrylic acid reaction vessel 5 connected with the acrolein reaction vessel, wherein the acrolein reaction vessel 4 comprises an acrolein reaction vessel and a molten salt heating system, and the diacrylic acid reaction vessel 5 comprises an acrylic acid reaction vessel and a molten salt heating system. The feed inlet of the acrolein reactor is connected to the feed outlet of the mixer 3, and the feed outlet of the acrylic acid reactor is connected to the heat exchanger in the separation unit.
The separation unit comprises a heat exchanger 6 connected with the material outlet of the acrylic acid reactor, an absorption tower 7 connected with the material outlet of the heat exchanger, a heavy component collection system and an acrylic acid collection system. The tail gas discharged from the absorption tower 7 is connected with a material inlet of a dryer 8. The heavy component collecting system and the acrylic acid collecting system are in parallel connection, heavy components discharged from the absorption tower 7 enter the heavy component collecting system, and acrylic acid discharged from the absorption tower 7 enters the acrylic acid collecting system.
The tail gas treatment unit consists of a tail gas discharge system, a dryer 8 and a gas circulating compressor 9. The tail gas discharge system is connected in parallel with the dryer 8 and is connected to the tail gas discharge port of the absorption tower 7. The tail gas discharge outlet of the absorption tower 7 is also connected with a dryer 8, and after passing through a gas circulation compressor 9, part of the tail gas returns to the preheater 2.
This example is preferably an embodiment in which a stripping product collection sampler is provided between the feed outlet of a acrolein reactor and the feed inlet of a diacrylic acid reactor. The anti-product collection sampler comprises a first condenser, a first gas sample collector and a first liquid sample collector; a material outlet of the acrolein reaction vessel is connected with a first condenser, a gas phase outlet of the first condenser is connected with a first gas sample collector, and a liquid phase outlet of the first condenser is connected with a first liquid sample collector; the collected gas and liquid samples were analyzed by chromatography and chemical titration to measure the gas sample composition and the liquid sample composition for yield calculation.
A secondary reaction product collecting sampler is arranged between the material outlet of the secondary reaction acrylic acid reactor and the material inlet of the heat exchanger. The second anti-product collection sampler comprises a second condenser, a second gas sample collector and a second liquid sample collector; a material outlet of the second anti-acrylic acid reactor is connected with a second condenser, a gas phase outlet of the second condenser is connected with a second gas sample collector, and a liquid phase outlet of the second condenser is connected with a second liquid sample collector; the collected gas and liquid samples were analyzed by chromatography and chemical titration to measure the gas sample composition and the liquid sample composition for calculating the product yield.
And a circulating tail gas sampler is arranged between the outlet of the dryer and the inlet of the gas circulating compressor, and a gas sample collected by the circulating tail gas sampler is subjected to chromatographic analysis to test the composition of the tail gas sample.
The pilot plant is adopted to evaluate the catalyst for preparing the acrolein and the acrylic acid by the propylene oxidation, and the specific process is as follows:
1.25L of acrolein and acrylic acid catalysts were measured, respectively, and charged into the corresponding reactors according to a conventional catalyst loading method, and the reaction system was connected as shown in FIG. 1:
propylene, air and water vapor are parallelly connected, enter a mixer and are mixed, then sequentially enter an acrolein reactor and an acrylic acid reactor, reaction products from the acrylic acid reactor enter an absorption tower after passing through a heat exchanger and are separated into heavy components, acrylic acid and tail gas, the heavy components and the acrylic acid respectively enter corresponding collecting systems, part of the tail gas enters an exhaust system, and the rest of the tail gas enters a water vapor feeding unit after passing through a dryer and a gas circulation compressor.
The mono-trans acrolein catalyst for propylene oxidation and the di-trans acrylic acid catalyst for acrolein oxidation are industrial catalysts. The metal element composition of the one-reaction catalyst except oxygen and the carrier is Mo according to the atomic ratio12Bi1.4Ni1. 5Co6.2Fe1.2W0.1K0.1(ii) a The component of the double reaction catalyst is Mo12V4.09Cu2.56Sb0.30Ti0.15Si1.00. After setting the reaction temperature (the temperature of the primary molten salt is 315 ℃ and the temperature of the secondary molten salt is 250 ℃) and the pressure according to the reaction requirements, starting feeding propylene, air and water vapor, and enabling the propylene, the air and the water vapor to be in a standard gas space velocity (the amount of gas treated by the catalyst in unit volume per unit time) relative to the primary catalyst for 2000h-1Introducing reaction gas mixture, wherein the ratio of the propylene to the oxygen to the nitrogen to the water vapor is 1:1.7:2.4:1 (volume ratio). At the moment, the tail gas completely enters an exhaust system. When the propylene feeding is gradually increased to 70% from 10% of the set load, after the propylene feeding is increased each time, the bed temperature needs to be determined to be stable, and then the propylene feeding is continuously increased; and (3) beginning partial tail gas circulation, emptying 70 percent of the tail gas, drying 30 percent of the tail gas, mixing with a steam feed, and then entering the reactor. The propylene feed was then gradually increased to 100% load and the propylene oxidation reaction started to proceed steadily.
After the reaction was stabilized, the yield of acrylic acid was analyzed, as well as the composition of the recycle off-gas.
The acrylic acid yield is (molar amount of acrylic acid produced by the reaction)/propylene supplied (molar amount) × 100.
Example 2
The pilot plant for the production of acrylic acid by the oxidation of propylene differs from example 1 in that the feed unit consists of a propylene feed and flow control system, a nitrogen and air feed and flow control and preheater, a water and flow control and vaporizer, and a mixer. The catalyst loading was 2.5L. The rest is the same as in example 1.
After the reaction temperature and pressure are set according to the reaction requirement, feeding of propylene, nitrogen, air and water vapor is started, and at the moment, all tail gas enters an exhaust system. When the propylene feed is gradually increased to 50% from the set load of 10%, 90% of tail gas is discharged, and 10% of tail gas is mixed with the steam feed after being dried and enters the reactor. The propylene feed was then gradually increased to 100% load and the propylene oxidation reaction started to proceed steadily.
After the reaction was stabilized, the yield of acrylic acid was analyzed, as well as the composition of the recycle off-gas.
Example 3
The pilot plant of this example was identical to that of example 1. The catalyst loading was 3.5L.
After the reaction temperature and pressure are set according to the reaction requirement, feeding of propylene, air and steam is started, and at the moment, all tail gas enters an exhaust system. When the propylene feeding is gradually increased to 60% from 10% of the set load, 50% of tail gas is discharged, and 50% of the tail gas is mixed with the steam feeding after being dried and then enters the reactor. The propylene feed was then gradually increased to 100% load and the propylene oxidation reaction started to proceed steadily.
After the reaction was stabilized, the yield of acrylic acid was analyzed, as well as the composition of the recycle off-gas.
Comparative example 1
The pilot plant of this comparative example differs from example 1 in that the off-gas treatment unit does not have a dryer. The catalyst loading and reaction process were the same as in example 1.
After the reaction was stabilized, the yield of acrylic acid was analyzed, and the composition of the circulating off-gas was as shown in Table 1.
TABLE 1
The circulating tail gas contains a large amount of water vapor under the condition of no dryer, the flow of the circulating tail gas is not easy to control and stabilize, and the yield of the product acrylic acid is low.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A pilot plant for the oxidation of propylene to acrylic acid, characterized in that it comprises the following units: the device comprises a feeding unit, a reaction product separation unit and a tail gas treatment unit; all units are connected in sequence according to the material flow direction;
wherein the reaction unit comprises a first acrolein reactor and a second acrylic acid reactor;
the tail gas treatment unit comprises a dryer and a gas circulation compressor, and the tail gas discharged from the reaction product separation unit enters the dryer and then returns to the feeding unit through the gas circulation compressor.
2. The pilot plant according to claim 1, characterized in that the feed unit comprises a feed and flow control system for propylene, nitrogen and/or air and water, a preheater, a vaporizer and a mixer;
the propylene feeding and flow control system, the nitrogen feeding and flow control system and/or the air feeding and flow control system and the water feeding and flow control system are connected in parallel;
the nitrogen feeding and flow control system and/or the air feeding and flow control system are/is connected with the preheater, the water feeding and flow control system is connected with the vaporizer, and the propylene feeding and flow control system is connected with the mixer; the material from the preheater and the water vapor from the vaporizer were mixed with propylene in a mixer.
3. The pilot plant according to claim 2, wherein the feed outlet of the first acrolein reactor is connected to the feed inlet of the second acrylic acid reactor, the first acrolein reactor and the second acrylic acid reactor each comprising a heating furnace and a reactor connected in series, the first acrolein reactor being connected to the feed outlet of the mixer.
4. The pilot plant of claim 1, wherein the first acrolein reactor comprises an acrolein reactor and a molten salt heating system, and the second acrylic acid reactor comprises an acrylic acid reactor and a molten salt heating system.
5. The pilot plant according to claim 3, characterized in that a sample collector for the stripping product is provided between the outlet of the feed of a acrolein reactor and the inlet of the feed of a diacrylic acid reactor.
6. The pilot plant according to claim 3, characterized in that a double back product collecting sampler is arranged between the feed outlet of the double back acrylic acid reactor and the feed inlet of the heat exchanger.
7. The pilot plant of claim 1, wherein the reaction product separation unit comprises a heat exchanger and an absorption column connected in series, the heat exchanger is connected to the feed outlet of the di-methacrylic acid reactor, and the tail gas discharged from the absorption column is connected to the feed inlet of the dryer.
8. The pilot plant of claim 7, wherein the reaction product separation unit further comprises a heavies collection system and an acrylic acid collection system connected in parallel, the heavies discharged from the absorber entering the heavies collection system, the acrylic acid discharged from the absorber entering the acrylic acid collection system.
9. Pilot plant according to claim 1, characterized in that a recycle off-gas sampler is arranged between the dryer outlet and the gas recycle compressor inlet.
10. The pilot plant according to claim 7 or 8, characterized in that the off-gas treatment unit further comprises an off-gas discharge system in parallel relationship with the dryer and connected to the off-gas discharge of the absorption tower.
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| CN202020712091.2U Active CN212954952U (en) | 2020-04-27 | 2020-04-30 | Propylene oxidation system acrylic acid pilot-scale plant with tail gas circulation |
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