CN116173884A - Device and method for removing residual olefin in refined solvent - Google Patents

Device and method for removing residual olefin in refined solvent Download PDF

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Publication number
CN116173884A
CN116173884A CN202211558945.6A CN202211558945A CN116173884A CN 116173884 A CN116173884 A CN 116173884A CN 202211558945 A CN202211558945 A CN 202211558945A CN 116173884 A CN116173884 A CN 116173884A
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hydrogen
solvent
low
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李姗姗
甄崇汀
徐小武
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Topen Technology Quzhou Co ltd
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Jinju Technology Ningbo Co ltd
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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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/2475—Membrane reactors
    • 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
    • B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
    • B01J10/007—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor in the presence of catalytically active bodies, e.g. porous plates
    • 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
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/2415—Tubular reactors
    • 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
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/2415—Tubular reactors
    • B01J19/2425—Tubular reactors in parallel
    • 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
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/248—Reactors comprising multiple separated flow channels

Abstract

An apparatus for removing residual olefins from a refined solvent, comprising: a hydrogen membrane module having a high pressure side flow path and a low pressure side flow path inside thereof, which are separated by a permeable membrane, and the high pressure side flow path has a hydrogen inlet connection pipe for the ingress and egress of hydrogen and a hydrogen outlet connection pipe, the low pressure side flow path has a solvent inlet connection pipe for the ingress and egress of solvent and a solvent outlet connection pipe, and the permeable membrane is arranged so that only hydrogen in the high pressure side flow path passes through; the catalyst module is loaded with a catalyst and is arranged in the low-pressure side stream; the inlet of the low-pressure separation tank is communicated with the solvent outlet connecting pipe of the hydrogen membrane component, the bottom of the low-pressure separation tank is provided with a liquid outlet for outputting solvent, and the top of the low-pressure separation tank is provided with an exhaust port. The invention also discloses a method for removing residual olefin in the refined solvent by adopting the device. Compared with the prior art, the method can remove the residual olefin in the solvent and reduce the loss of the solvent.

Description

Device and method for removing residual olefin in refined solvent
Technical Field
The invention belongs to the technical field of polymer preparation, and particularly relates to a device and a method for removing residual olefin in a refined solvent.
Background
Solution polymerization is a polymerization reaction performed in a solution state by dissolving monomers and comonomers in a solvent and adding an initiator (catalyst). In the process, the solvent does not participate in the reaction, but is used as a heat transfer medium, so that the reaction temperature is easy to control; the monomer, the comonomer and the polymer generated by the reaction are uniformly dispersed in the solvent, so that the polymer can react in the environment with lower concentration, and the molecular weight distribution and the structural state of the polymer can be easily controlled.
But at the same time, the cost of polymer purification, unreacted monomer recovery and solvent separation is increased due to the introduction of the solvent, and the monomer, the comonomer, the solvent and the polymer are separated by a common flash distillation rectification method in industry, and the refined solvent is obtained through multistage rectification and is recycled.
However, since the monomer or comonomer is very soluble in the solvent, monomer and comonomer cannot be thoroughly separated by distillation, and trace amounts of monomer or comonomer will dissolve in the solvent and follow the circulating solvent to the whole solvent system.
Once the monomer and comonomer enter the catalyst preparation unit along with the circulating solvent, the monomer and comonomer react in advance under the action of the catalyst to generate a polymer, and the polymer is blocked in a pipeline of the catalyst preparation system or adhered in the inner wall of the catalyst preparation tank, so that the conditions of unbalanced catalyst metering, degraded polymer quality and the like are seriously caused.
As shown in fig. 1, in the petrochemical industry, a hydrogenation reactor 1 'and a condensation degassing device 2' (tank, tower, etc.) are often used for separating residual monomers (olefins) from solvents, hydrogen and olefins undergo an addition reaction in the hydrogenation reactor 1 'to generate low-boiling-point alkanes, and then enter the degassing device 2' (tank, tower, etc.), and under the drive of inert gas (such as nitrogen), unreacted hydrogen and alkanes generated by the reaction can be removed with solvents through an exhaust system.
The pressurization is favorable for the forward hydrogenation reaction, the high temperature can improve the activity of the catalyst in the hydrogenation reactor, the hydrogenation reactor is an important oil refining process device which is used for high temperature and high pressure and works under the condition of hydrogen-containing medium, the operation condition is extremely harsh, and serious loss is caused once accidents occur. In addition, the hydrogenation reactor has relatively high cost and long production period.
In order to thoroughly remove olefin in the solvent, the hydrogenation reaction can raise the hydrogen pressure in the hydrogenation reactor as much as possible, and the high-pressure hydrogen is commonly used for reaction, but the high-pressure hydrogen flow is difficult to regulate and control, so that the hydrogen is extremely easy to lose due to excessive fluctuation, the hydrogen is wasted, and the excessive hydrogen is mixed with the solvent to be discharged when waste gas is discharged, so that the environment is polluted, and the energy is wasted. Therefore, it is important to obtain a purified solvent and to reduce the loss of the solvent in the solution polymerization.
Disclosure of Invention
The first technical problem to be solved by the present invention is to provide a device for removing residual olefin in refined solvent, so as to reduce the loss of solvent.
The second technical problem to be solved by the invention is to provide a method for removing residual olefin by adopting the device.
The technical scheme adopted by the invention for solving the first technical problem is as follows: an apparatus for removing residual olefins from a refined solvent, comprising:
a hydrogen membrane module having a high pressure side flow path and a low pressure side flow path inside thereof, which are separated by a permeable membrane, and the high pressure side flow path has a hydrogen inlet connection pipe for the ingress and egress of hydrogen and a hydrogen outlet connection pipe, the low pressure side flow path has a solvent inlet connection pipe for the ingress and egress of solvent and a solvent outlet connection pipe, and the permeable membrane is arranged so that only hydrogen in the high pressure side flow path passes through;
the catalyst module is loaded with a catalyst and is arranged in the low-pressure side stream;
the inlet of the low-pressure separation tank is communicated with the solvent outlet connecting pipe of the hydrogen membrane component, the bottom of the low-pressure separation tank is provided with a liquid outlet for outputting solvent, and the top of the low-pressure separation tank is provided with an exhaust port.
The permeable membrane is made of at least one of polyimide, polysulfone, polyethylene trimethyl silane, polyphenyl ether and polyamide.
The hydrogen membrane component relates to the following principle:
F＝A*k*(piH-piL)
f-penetration amount, the unit is kmol/h;
a-the area of the permeable membrane in m 2 ；
k-permeation factor in kmol/(m) 2 ·h·bar)；
piH-high-side component partial pressure in bar;
piL-the partial pressure of the low-pressure side components in bar;
the hydrogen membrane component increases the area of the permeable membrane by increasing the flow channel, greatly increases the hydrogen permeation quantity, ensures that turbulent hydrogen can be uniformly mixed with the solvent within the range of a specified Reynolds number, and completely reacts under the action of the catalyst.
The hydrogen membrane components can be one or two or more, when two or more hydrogen membrane components exist, the hydrogen membrane components can be connected in series or in parallel or both in series and in parallel, and the hydrogen membrane components are designed according to actual working conditions.
Preferably, the hydrogen membrane assembly comprises a housing, wherein the housing is hollow to form the high-pressure side flow passage; the permeable membrane is arranged in the shell and is a tubular body, and the inner space of the tubular body is the low-pressure side flow passage.
In addition, the permeable membrane may be formed in a sheet shape to partition the space in the casing into at least two spaces, i.e., the high-pressure side flow path and the low-pressure side flow path.
In order to improve the reaction efficiency, preferably, a plurality of tubular bodies are arranged side by side at intervals, and each tubular body is internally provided with the catalytic module. Thus, the plurality of tubular bodies can increase the area of the permeable membrane, thereby increasing the permeation quantity of hydrogen, enabling the hydrogen to be uniformly mixed with olefin in the solvent and react under the action of the catalyst.
Further, there are a plurality of catalytic modules within each tubular body and spaced apart along the length of the tubular body.
In order to further promote the gas-liquid mixing reaction, the catalyst system preferably further comprises a plurality of mixing modules which are arranged in the tubular body and pass through after the gas-liquid is mixed, and the mixing modules are alternately arranged with the catalyst modules in the length direction of the tubular body. The mixing module is an existing mixer so that the hydrogen and the olefin in the solvent can be fully mixed and reacted.
Preferably, the solvent inlet connection pipe and the solvent outlet connection pipe are respectively arranged corresponding to two ends of the tubular body, the hydrogen inlet connection pipe is arranged at the bottom of the shell and is close to the solvent inlet connection pipe, and the hydrogen outlet connection pipe is arranged at the bottom of the shell and is close to the solvent outlet connection pipe. In this way, it is ensured that the low pressure side stream is long enough that hydrogen can enter the low pressure side stream to react sufficiently with the olefin in the solvent.
In each of the above schemes, preferably, the hydrogen membrane module further comprises a compressor, wherein the output end of the compressor is connected with the hydrogen inlet connecting pipe of the hydrogen membrane module, and the input end of the compressor is simultaneously communicated with a hydrogen pipeline for conveying hydrogen and the hydrogen outlet connecting pipe of the hydrogen membrane module; the hydrogen pipeline is provided with a flow control valve and a pressure control valve. Thereby realizing the hydrogen circulation supply and ensuring the pressure of the hydrogen entering the hydrogen membrane component.
The invention solves the second technical problem by adopting the technical proposal that: a method for removing residual olefins in a solvent by using the device as described above, characterized by comprising the following steps:
1. inputting a solvent to be treated into a low-pressure side flow channel of a hydrogen membrane assembly through a solvent inlet connecting pipe, inputting hydrogen into a high-pressure side flow channel of the hydrogen membrane assembly through a hydrogen inlet connecting pipe, enabling at least part of hydrogen in the high-pressure side flow channel to enter the low-pressure side flow channel through a permeable membrane, reacting with olefin in the solvent to be treated at the temperature of 30-200 ℃, outputting the solvent after the reaction from a solvent outlet connecting pipe, and outputting hydrogen which does not permeate the permeable membrane in the high-pressure side flow channel from a hydrogen outlet connecting pipe; wherein the solvent to be treated is an inert solvent and is at least one of alkane and cycloalkane, and the alkene in the solvent to be treated is at least one of ethylene, propylene, butene, pentene, hexene and isomers thereof; to be at the siteThe double bond concentration of the olefin in the solvent is 1 to 200mol/m 3 The ratio between the molar flow of the hydrogen input into the hydrogen membrane component and the molar flow of the double bonds of the olefin in the solvent to be treated is 1-1.2, and the pressure of the hydrogen input into the hydrogen membrane component is 0.3-1.2 MPaG;
2. the solvent after reaction output from the solvent outlet connecting pipe enters the low-pressure separation tank for gas-liquid separation, the separated gas phase is discharged from the gas outlet of the low-pressure separation tank, and the separated liquid phase is discharged from the liquid outlet of the low-pressure separation tank, wherein the pressure in the low-pressure separation tank is recorded as P1, the pressure of the hydrogen gas input into the hydrogen membrane component is recorded as P2, and the pressure of 1.2MPaG is more than or equal to P2 and more than or equal to 3P1.
The term "inert" in the above inert solvents means that the hydrocarbon solvent does not interfere with the progress of the hydrogenation reaction, i.e., the hydrocarbon solvent does not react with the reactants and reaction products nor adversely affect the catalyst activation performance.
The hydrogenation process of the present invention may be a continuous operation or a batch operation. The method has the advantages that the method is more advantageous when in continuous operation, solvent and catalyst are fed intermittently during intermittent operation, hydrogen is fed continuously, and hydrogenation materials are discharged to a low-pressure separation tank after the hydrogenation reaction reaches the residence time required by the reaction.
The olefin-removed purification solvent obtained by the method of the present invention is not limited to the catalyst configuration, and may be used for other purposes such as polymerization temperature adjustment, reaction flushing, and solvent dilution in solution polymerization of a reaction monomer.
Preferably, the solvent to be treated is at least one of cyclohexane, n-heptane, n-hexane and 1-octane; the double bond concentration of the olefin in the solvent to be treated is 5-100 mol/m 3 The method comprises the steps of carrying out a first treatment on the surface of the The ratio between the molar flow rate of hydrogen gas fed into the hydrogen membrane module and the molar flow rate of double bonds of olefin in the solvent to be treated is 1-1.05.
Compared with the prior art, the invention has the advantages that:
the hydrogen membrane component, the catalytic module and the low-pressure separation tank are arranged, so that high-pressure hydrogen in the high-pressure side flow passage of the hydrogen membrane component can be controllably permeated into the low-pressure side flow passage to react with olefin in the solvent in the low-pressure side flow passage under the action of the catalyst, double bonds of the olefin in the reaction system are approximately equimolar with hydrogen in the process, hydrogen and solvent loss and environmental pollution caused by excessive hydrogen are avoided, and the hydrogen utilization rate is improved;
the principle of the method for removing the residual olefin in the refined solvent is olefin addition reaction, the olefin addition reaction of the method occurs in a hydrogen membrane component, and the hydrogen membrane component is used for replacing high-temperature high-pressure hydrogenation equipment of hydrogenation reactors, so that harsh operating conditions are avoided;
the low-pressure separation tank does not need to be additionally provided with condensing equipment and degassing equipment, gas can be stably separated, inert gas is not required to be introduced from the bottom to be taken as power gas to carry out residual gas, and the condition that the inert gas carries out solvent to cause solvent loss can be avoided.
The invention has almost no hydrogen residue in the exhaust gas discharged from the exhaust port of the low-pressure separation tank, and the hydrogen content is less than 500ppm.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for removing residual olefins from a refined solvent according to the prior art;
FIG. 2 is a schematic structural view of an apparatus for removing residual olefins from a refining solvent according to example 1 of the present invention;
FIG. 3 is a longitudinal cross-sectional view of a hydrogen membrane module according to example 1 of the present invention;
fig. 4 is a transverse sectional view of the hydrogen membrane module in example 1 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the embodiments of the drawings.
Example 1:
as shown in fig. 2 to 4, a preferred embodiment 1 of an apparatus and a method for removing residual olefin in a refined solvent according to the present invention comprises a hydrogen membrane module 1, a catalyst-supporting catalytic module 2, a low pressure separation tank 3, a mixing module 4, and a compressor 5.
The hydrogen membrane module 1 is internally provided with a high-pressure side flow passage 11 and a low-pressure side flow passage 12 which are separated by a permeable membrane 13, the high-pressure side flow passage 11 is provided with a hydrogen inlet connecting pipe 11a and a hydrogen outlet connecting pipe 11b for the ingress and egress of hydrogen, the low-pressure side flow passage 12 is provided with a solvent inlet connecting pipe 12a and a solvent outlet connecting pipe 12b for the ingress and egress of solvent, and the permeable membrane 13 is arranged so that only the hydrogen in the high-pressure side flow passage 11 passes through. In this embodiment, the hydrogen membrane module 1 includes a housing 10, and the housing 10 is hollow to form the high pressure side stream 11; the permeable membrane 13 is disposed in the casing 10, and the permeable membrane 13 is a tubular body, and an inner space of the tubular body is the low pressure side flow 12. Meanwhile, a plurality of tubular bodies are arranged side by side at intervals. The solvent inlet connection pipe 12a and the solvent outlet connection pipe 12b are respectively arranged corresponding to two ends of each tubular body, the hydrogen inlet connection pipe 11a is arranged at the bottom of the shell 10 and is close to the solvent inlet connection pipe 12a, and the hydrogen outlet connection pipe 11b is arranged at the bottom of the shell 10 and is close to the solvent outlet connection pipe 12 b.
Each tubular body is internally provided with a plurality of the catalytic modules 2 and a plurality of the mixing modules 4, and the catalytic modules 2 and the mixing modules 4 are alternately arranged at intervals in the length direction of the tubular body. The catalyst on the catalytic module is the existing catalyst for hydrogenation reaction, and the mixing module 4 is the existing mixer through which the gas and the liquid are mixed.
The inlet 31 of the low pressure separator 3 is connected to the solvent outlet connection pipe 12b of the hydrogen membrane module 1, and the bottom of the low pressure separator 3 has a liquid outlet 32 for outputting the solvent and the top thereof has an exhaust port 33. Simultaneously, the exhaust port 33 at the top of the low-pressure separation tank 3 is also provided with a nitrogen seal pressure valve group and an exhaust control valve group, which are both in the prior art, so as to isolate air, improve safety, and control the pressure of the low-pressure side of the solvent, thereby controlling the osmotic pressure difference.
For recycling hydrogen, the output end of the compressor 5 is connected with the hydrogen inlet connecting pipe 11a of the hydrogen membrane component 1, and the input end is simultaneously communicated with a hydrogen pipeline 50 for conveying hydrogen and the hydrogen outlet connecting pipe 11b of the hydrogen membrane component 1; the hydrogen line 50 is provided with a flow control valve 51 and a pressure control valve 52.
The method for preparing the ethylene/1-butene copolymerized elastomer by using the solution polymerization process and taking normal hexane as a solvent comprises the following steps of:
1. inputting a solvent to be treated into a low-pressure side flow channel 12 of the hydrogen membrane assembly 1 through a solvent inlet connecting pipe 12a, inputting hydrogen into a high-pressure side flow channel 11 of the hydrogen membrane assembly 1 through a hydrogen inlet connecting pipe 11a, enabling at least part of hydrogen in the high-pressure side flow channel 11 to enter the low-pressure side flow channel 12 through a permeable membrane 13, reacting with olefin in the solvent to be treated at a temperature of 60 ℃ to generate low-boiling-point alkane, outputting the solvent after reaction from a solvent outlet connecting pipe 12b, and outputting hydrogen which does not permeate through the permeable membrane 13 in the high-pressure side flow channel 11 from a hydrogen outlet connecting pipe 11b; wherein the double bond concentration of the olefin in the solvent to be treated is 5mol/m 3 The ratio between the molar flow rate of hydrogen gas fed into the hydrogen membrane module 1 and the molar flow rate of double bonds of olefin in the solvent to be treated was 1.02, the pressure of hydrogen gas fed into the hydrogen membrane module 1 was 500KPaG, and the molar flow rate of hydrogen gas into the low pressure side flow path 12 (i.e., the consumption of hydrogen gas in the hydrogen membrane module 1) was 10.02mol/h;
2. the reacted solvent outputted from the solvent outlet connection pipe 12b enters the low-pressure separation tank 3 to be subjected to gas-liquid separation, the separated gas phase is discharged from the gas outlet 33 of the low-pressure separation tank 3, and the separated liquid phase is discharged from the liquid outlet 32 of the low-pressure separation tank 3, wherein the pressure in the low-pressure separation tank 3 is 50KPaG, the discharge amount of the gas phase discharged from the gas outlet 33 of the low-pressure separation tank 3 is 10.02mol/h, and the discharge amount of the hydrogen in the gas phase is 0.02mol/h.
Example 2:
substantially the same as in example 1, except that the parameters in the process were different, the double bond concentration of the olefin in the solvent to be treated in the first step of this example was 10mol/m 3 The consumption of hydrogen in the hydrogen membrane component 1 is 20.06mol/h; in the second step, the discharge amount of the gas phase discharged from the exhaust port 33 of the low-pressure separation tank 3 was 20.06mol/h, and the discharge amount of the hydrogen gas in the gas phase was 0.06mol/h.
Example 3:
substantially the same as in example 1, except that the parameters in the process were different, the pressure of the hydrogen fed into the hydrogen membrane module 1 in the first step of this example was 600KPaG, and the consumption of hydrogen in the hydrogen membrane module 1 was 10.03mol/h; in the second step, the discharge amount of the gas phase discharged from the exhaust port 33 of the low-pressure separation tank 3 was 10.03mol/h, and the discharge amount of the hydrogen gas in the gas phase was 0.03mol/h.
Example 4:
substantially the same as in example 1, except that the parameters in the process were different, the double bond concentration of the olefin in the solvent to be treated in the first step of this example was 10mol/m 3 The pressure of the hydrogen input into the hydrogen membrane component 1 is 600KPaG, and the consumption of the hydrogen in the hydrogen membrane component 1 is 20.08mol/h; in the second step, the discharge amount of the gas phase discharged from the exhaust port 33 of the low-pressure separation tank 3 was 20.08mol/h, and the discharge amount of the hydrogen gas in the gas phase was 0.08mol/h.
Example 5:
substantially the same as in example 1, except that the parameters in the process were different, the pressure of the hydrogen fed into the hydrogen membrane module 1 in the first step of this example was 700KPaG, and the consumption of hydrogen in the hydrogen membrane module 1 was 10.04mol/h; in the second step, the discharge amount of the gas phase discharged from the exhaust port 33 of the low-pressure separation tank 3 was 10.04mol/h, and the discharge amount of the hydrogen gas in the gas phase was 0.04mol/h.
Example 6:
substantially the same as in example 1, except that the parameters in the process were different, the double bond concentration of the olefin in the solvent to be treated in the first step of this example was 10mol/m 3 The pressure of the hydrogen input into the hydrogen membrane component 1 is 700KPaG, and the consumption of the hydrogen in the hydrogen membrane component 1 is 20.1mol/h; in the second step, the discharge amount of the gas phase discharged from the exhaust port 33 of the low-pressure separation tank 3 was 20.1mol/h, and the discharge amount of the hydrogen gas in the gas phase was 0.1mol/h.
Comparative example 1:
the method comprises the steps of preparing an ethylene/1-butene copolymerized elastomer by using normal hexane as a solvent through a solution polymerization process, removing residual olefin in a refined solvent by adopting a device shown in fig. 1 after the preparation, carrying out hydrogenation reaction (reaction temperature 200 ℃ and pressure 1.5 MPaG) on hydrogen and olefin in the solvent to be treated in a hydrogenation reactor 1 'to generate low-boiling-point alkane, then entering a degassing device 2', and removing unreacted hydrogen and alkane generated by the reaction with the solvent through an exhaust system under the drive of inert gas. Wherein, the liquid crystal display device comprises a liquid crystal display device,the flow rate of the solvent to be treated entering the hydrogenation reactor 1' was 2m 3 And/h, the double bond concentration of the olefin in the solvent to be treated is 5mol/m 3 The pressure of the hydrogen fed into the hydrogenation reactor 1' was 1.5MPaG, the consumption of the hydrogen was 41.9mol/h, the discharge amount of the off-gas removed through the exhaust system was 82.1mol/h, and the discharge amount of the hydrogen in the off-gas was 31.9mol/h.
Comparative example 2:
substantially the same as in comparative example 1, except that the parameters in the process were different, the double bond concentration of the olefin in the solvent to be treated in this comparative example was 10mol/m 3 The consumption of hydrogen was 52.04mol/h, the emission of exhaust gas removed through the exhaust system was 92.7mol/h, and the emission of hydrogen in the exhaust gas was 32.04mol/h.
Comparative example 3:
the procedure was substantially the same as in comparative example 1, except that the parameters in the process were different, the pressure of hydrogen fed into the hydrogenation reactor 1' in this comparative example was 2MPaG, the consumption of hydrogen was 43.2mol/h, the discharge amount of off-gas removed through the exhaust system was 85.3mol/h, and the discharge amount of hydrogen in the off-gas was 33.2mol/h.
Comparative example 4:
substantially the same as in comparative example 1, except that the parameters in the process were different, the double bond concentration of the olefin in the solvent to be treated in this comparative example was 10mol/m 3 The pressure of the hydrogen fed into the hydrogenation reactor 1' was 2MPaG, the consumption of the hydrogen was 54.8mol/h, the discharge amount of the off-gas removed through the exhaust system was 95.8mol/h, and the discharge amount of the hydrogen in the off-gas was 34.8mol/h.
Comparative example 5:
the procedure was substantially the same as in comparative example 1, except that the parameters in the process were different, the pressure of hydrogen fed into the hydrogenation reactor 1' in this comparative example was 3MPaG, the consumption of hydrogen was 50.7mol/h, the discharge amount of off-gas removed through the exhaust system was 97.7mol/h, and the discharge amount of hydrogen in the off-gas was 40.7mol/h.
Comparative example 6:
substantially the same as in comparative example 1, except that the parameters in the process are different, the double bond concentration of olefin in the solvent to be treated in this comparative exampleIs 10mol/m 3 The pressure of the hydrogen fed into the hydrogenation reactor 1' was 3MPaG, the consumption of the hydrogen was 62.1mol/h, the discharge amount of the off-gas removed through the exhaust system was 112.1mol/h, and the discharge amount of the hydrogen in the off-gas was 42.1mol/h.
The parameters and results of examples 1 to 6 and comparative examples 1 to 6 are shown in Table 1 below:
Figure BDA0003983785530000071
Figure BDA0003983785530000081
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as can be seen from comparing the results of the embodiment and the comparative example, the hydrogen membrane component is adopted to be matched with the hydrogen pressurizing force circulating device to replace the traditional flow of the hydrogenation reactor and the degassing and condensing equipment, and the hydrogen flow is controllable, so that the emission of hydrogen and waste gas of the subsequent unit is reduced, and the hydrogen membrane component has excellent environmental protection performance; the normal-pressure normal-temperature hydrogenation operation condition replaces the traditional high-temperature high-pressure condition, so that the severe operation condition of the hydrogenation reactor is avoided, the accident risk is reduced, and the safety of hydrogenation operation is improved.

Claims (10)

1. An apparatus for removing residual olefins from a refined solvent, comprising:
a hydrogen membrane module (1) having a high-pressure side flow path (11) and a low-pressure side flow path (12) inside thereof, which are separated by a permeable membrane (13), and the high-pressure side flow path (11) has a hydrogen inlet connection pipe (11 a) for hydrogen gas to enter and exit, a hydrogen outlet connection pipe (11 b), the low-pressure side flow path (12) has a solvent inlet connection pipe (12 a) for solvent to enter and exit, and a solvent outlet connection pipe (12 b), the permeable membrane (13) being arranged so that only hydrogen gas in the high-pressure side flow path (11) passes therethrough;
a catalyst-supporting catalytic module (2) provided in the low-pressure side stream (12);
the inlet (31) of the low-pressure separation tank (3) is communicated with a solvent outlet connecting pipe (12 b) of the hydrogen membrane component (1), the bottom of the low-pressure separation tank (3) is provided with a liquid outlet (32) for outputting solvent, and the top of the low-pressure separation tank is provided with an exhaust port (33).
2. The apparatus according to claim 1, wherein: the hydrogen membrane component (1) comprises a shell (10), wherein the inside of the shell (10) is hollow to form the high-pressure side flow channel (11); the permeable membrane (13) is arranged in the shell (10), the permeable membrane (13) is a tubular body, and the inner space of the tubular body is the low-pressure side flow (12).
3. The apparatus according to claim 2, wherein: the number of the tubular bodies is multiple, the tubular bodies are arranged side by side at intervals, and the catalytic modules (2) are arranged in each tubular body.
4. A device according to claim 3, characterized in that: the catalytic modules (2) in each tubular body are a plurality of and are arranged at intervals along the length direction of the tubular body.
5. The apparatus according to claim 4, wherein: the catalytic reactor also comprises a plurality of mixing modules (4) which are arranged in the tubular body and used for allowing the gas and the liquid to pass through after being mixed, wherein the plurality of mixing modules (4) are alternately arranged with the catalytic modules (2) in the length direction of the tubular body.
6. The apparatus according to claim 2, wherein: the solvent inlet connecting pipe (12 a) and the solvent outlet connecting pipe (12 b) are respectively arranged at two ends of the corresponding tubular body, the hydrogen inlet connecting pipe (11 a) is arranged at the bottom of the shell (10) and is close to the solvent inlet connecting pipe (12 a), and the hydrogen outlet connecting pipe (11 b) is arranged at the bottom of the shell (10) and is close to the solvent outlet connecting pipe (12 b).
7. The apparatus according to any one of claims 1 to 6, wherein: the device also comprises a compressor (5), the output end of which is connected with the hydrogen inlet connecting pipe (11 a) of the hydrogen membrane component (1), and the input end of which is simultaneously communicated with a hydrogen pipeline (50) for conveying hydrogen and a hydrogen outlet connecting pipe (11 b) of the hydrogen membrane component (1); the hydrogen pipeline (50) is provided with a flow control valve (51) and a pressure control valve (52).
8. A method for removing residual olefins in a solvent using the apparatus as claimed in any one of claims 1 to 7, characterized by the steps of:
1. inputting a solvent to be treated into a low-pressure side flow channel (12) of the hydrogen membrane assembly (1) through a solvent inlet connecting pipe (12 a), inputting hydrogen into a high-pressure side flow channel (11) of the hydrogen membrane assembly (1) through a hydrogen inlet connecting pipe (11 a), enabling at least part of the hydrogen in the high-pressure side flow channel (11) to enter the low-pressure side flow channel (12) through a permeable membrane (13), reacting with olefin in the solvent to be treated at the temperature of 30-200 ℃, outputting the solvent from a solvent outlet connecting pipe (12 b) after the reaction, and outputting hydrogen which does not permeate the permeable membrane (13) in the high-pressure side flow channel (11) from a hydrogen outlet connecting pipe (11 b); wherein the solvent to be treated is an inert solvent and is at least one of alkane and cycloalkane, and the alkene in the solvent to be treated is at least one of ethylene, propylene, butene, pentene, hexene and isomers thereof; the double bond concentration of the olefin in the solvent to be treated is 1-200 mol/m 3 The ratio between the molar flow of the hydrogen input into the hydrogen membrane component (1) and the molar flow of the double bonds of the olefin in the solvent to be treated is 1-1.2, and the pressure of the hydrogen input into the hydrogen membrane component (1) is 0.3-1.2 MPaG;
2. the solvent after reaction output from the solvent outlet connecting pipe (12 b) enters the low-pressure separation tank (3) for gas-liquid separation, separated gas phase is discharged from the exhaust port (33) of the low-pressure separation tank (3), separated liquid phase is discharged from the liquid outlet (32) of the low-pressure separation tank (3), wherein the pressure in the low-pressure separation tank (3) is recorded as P1, the pressure of hydrogen input into the hydrogen membrane assembly (1) is recorded as P2, and 1.2MPaG is more than or equal to P2 and more than or equal to 3P1.
9. The method according to claim 8, wherein: the solvent to be treated is at least one of cyclohexane, n-heptane, n-hexane and 1-octane; the double bond concentration of the olefin in the solvent to be treated is 5-100 mol/m 3 The method comprises the steps of carrying out a first treatment on the surface of the Inputting hydrogenThe ratio between the molar flow of hydrogen of the membrane module (1) and the molar flow of double bonds of the olefin in the solvent to be treated is 1 to 1.05.
10. The method according to claim 8, wherein: the permeable membrane (13) is made of at least one of polyimide, polysulfone, polyethylene trimethylsilane, polyphenyl ether and polyamide.
CN202211558945.6A 2022-12-06 2022-12-06 Device and method for removing residual olefin in refined solvent Pending CN116173884A (en)

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CN202211558945.6A CN116173884A (en) 2022-12-06 2022-12-06 Device and method for removing residual olefin in refined solvent

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CN202211558945.6A CN116173884A (en) 2022-12-06 2022-12-06 Device and method for removing residual olefin in refined solvent

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