CN108484371B - Reaction system for synthesizing polymethoxy dimethyl ether - Google Patents
Reaction system for synthesizing polymethoxy dimethyl ether Download PDFInfo
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- CN108484371B CN108484371B CN201810391683.6A CN201810391683A CN108484371B CN 108484371 B CN108484371 B CN 108484371B CN 201810391683 A CN201810391683 A CN 201810391683A CN 108484371 B CN108484371 B CN 108484371B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/50—Preparation of compounds having groups by reactions producing groups
- C07C41/56—Preparation of compounds having groups by reactions producing groups by condensation of aldehydes, paraformaldehyde, or ketones
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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
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
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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
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
- B01J8/065—Feeding reactive fluids
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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
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
- B01J8/067—Heating or cooling the reactor
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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
Abstract
The invention discloses a reaction system for synthesizing polymethoxy dimethyl ether. Comprises a raw material mixer and a reactor; the reactor is a tube array type floating bed reactor, a discharge port of the raw material mixer is connected with the bottom end of the reactor through a feeding pipeline, a feeding pump is installed in the feeding pipeline, a circulating reflux pipeline and a separating pipeline are connected to the top end of the reactor in a branching mode, the other end of the circulating reflux pipeline is connected to the raw material mixer, and the other end of the separating pipeline is connected to a downstream separating system. The invention can not only ensure that the raw material mixture is fully and uniformly mixed, prolong the reaction residence time, quickly match the reaction heat, effectively control the temperature of the catalyst bed layer, has small pressure drop of the floating bed reactor, is not easy to block, fully contacts the raw material with the catalyst, and effectively separates the catalyst from the crude reaction liquid, thereby solving the problem of catalyst separation and recovery.
Description
Technical Field
The invention belongs to the field of environment-friendly fuel oil blending component technology and green solvents, and particularly relates to a reaction system for synthesizing polymethoxy dimethyl ether.
Background
Polyoxymethylene dimethyl ethers (DMM)3~6) As a novel environment-friendly fuel oil blending component with great application prospect, the diesel oil blending component has the advantages of high cetane number, high oxygen content, good low-temperature fluidity, capability of obviously improving the combustion performance of diesel oil, heat efficiency improvement, reduction of the emission of automobile exhaust and the like; polyoxymethylene dimethyl ethers (DMM)3-4Component) is an excellent low-toxicity green solvent.
At present, the key points for synthesizing polyoxymethylene dimethyl ethers mainly lie in the catalyst and the reactor. In the ionic liquid acid catalysis process, methylal, concentrated formaldehyde, etc. are used as initial reaction material in a kettle reactor to prepare polymethoxy dimethyl ether, which is then separated and refined in a series of distilling and extracting separation systems. The method has the advantages of simple reactor structure, high catalyst activity, high reaction conversion rate and the like, but has the defects of difficult separation of the catalyst and the product, long separation process, high energy consumption, catalyst loss and the like. The other tubular fixed bed reactor structure adopts a solid catalyst, methanol and formaldehyde are used as raw materials to synthesize polymethoxy dimethyl ether by a one-step method, the reactor structure solves the problem of bias flow of material flow in a large-scale reactor, and simultaneously solves the problems of catalyst fixation and separation, but a catalyst bed layer is easy to block, and the resistance of the catalyst bed layer in the later production stage is large.
Disclosure of Invention
In order to ensure that the raw material mixture is fully and uniformly mixed, the reaction residence time is shortened, the reaction heat can be quickly matched, the temperature of a catalyst bed layer is effectively controlled, the resistance of the bed layer is small, the catalyst is effectively separated from a crude reaction liquid, and the problem of catalyst separation and recovery is solved, the invention provides a reaction system for synthesizing polymethoxy dimethyl ether on the basis of a tubular reactor.
The specific technical scheme of the invention is as follows:
a reaction system for synthesizing polymethoxy dimethyl ether comprises a raw material mixer and a reactor; the reactor is a tube type floating bed reactor, the bottom of the reactor is provided with a reaction liquid inlet, and the top of the reactor is provided with a reaction liquid outlet; the discharge port of the raw material mixer is connected with the reaction liquid inlet of the reactor through a circulating pipeline, a circulating pump is installed in the circulating pipeline, the reaction liquid outlet of the reactor is respectively connected with one end of a return pipeline 6 and one end of a discharge pipe 7, the other end of the return pipeline 6 is connected with the raw material mixer, and the other end of the discharge pipe 7 is connected with a downstream rectification system;
when the method works, 2000kg of methylal with the purity not lower than 99.0wt% and 2400kg of trioxymethylene with the purity not lower than 99.0wt% are added into a raw material mixer, the materials are uniformly stirred and mixed in the raw material mixer, reaction raw liquid is sent to the tube pass of a reactor through a feed pump, catalytic reaction is carried out, polymethoxy dimethyl ether is obtained through synthesis, the reaction heat is removed through a coolant medium in the shell pass of the reactor, and the total conversion rate of the trioxymethylene is greater than 85%; and (3) recycling about 95% of reaction liquid discharged from the reactor back to the raw material mixer, feeding the rest 5% of reaction liquid as reaction discharge material to a rectification system for separation, obtaining a polymethoxy dimethyl ether product at the bottom of the rectification system, and returning light components at the top of the rectification system to the reaction system for recycling.
The technical scheme for further limiting is as follows:
the feeding speed of the methylal is 30-80kg/min, and the feeding speed of the trioxymethylene is 50-100 kg/min.
Reaction conditions are as follows: the temperature is 50-150 ℃, and the pressure of the reactor is 0.1-3.0 MpaG.
The reactor comprises a shell and reaction tubes arranged in parallel, and the reaction tubes are axially arranged in the middle of the shell; solid catalysts are filled in the reaction tubes which are arranged in parallel to form a catalyst bed layer, and a reserved floating space is formed in a cavity of the reaction tube above the catalyst bed layer; a solid-liquid phase separation cavity and a liquid outlet cavity are sequentially arranged in the shell adjacent to the axial top of the reaction tube array, and a liquid redistributor is arranged in the liquid outlet cavity to ensure that the solid catalyst carried out of the reaction tube array can be settled freely and return to the catalyst bed layer; an inlet liquid distributor is arranged in the shell adjacent to the axial bottom of the reaction tube array.
Four groups of temperature detectors are uniformly distributed in the tube array along the circumference of the reactor, and each group of temperature detectors is provided with an upper measuring point, a middle measuring point and a lower measuring point.
The reaction tubes arranged in parallel are hermetically arranged in the middle of the reactor shell; the lower part of the shell side of the reaction tube array is provided with a refrigerant inlet, and the upper part of the shell side of the reaction tube array is provided with a refrigerant outlet.
Compared with the prior art, the beneficial technical effects of the invention are embodied in the following aspects:
1. the reactor of the invention has good heat transfer effect, uniform temperature distribution and easy temperature control, and the temperature difference of each point of the section of the same bed layer of the catalyst bed layer of the reactor is within the range of +/-1 ℃.
2. The reactor of the invention has small pressure drop, good contact effect of the reaction materials and the catalyst, and is beneficial to improving the reaction conversion rate, and the single-pass conversion rate of trioxymethylene is more than 60 percent.
3. The reactor adopts a floating bed, strengthens convection mass transfer, is not easy to have dead zones, and can effectively reduce or reduce the blocking phenomenon caused by trioxymethylene and paraformaldehyde which are easy to polymerize.
4. The reactor of the invention avoids the phenomena of 'temperature runaway', 'short circuit' and the like which are often generated in a fixed bed reactor.
5. In the reactor, the solid catalyst and the liquid reaction mixture can be effectively separated, a solid catalyst and liquid phase separation space is reserved above the tubular reactor, and the settling velocity of the solid catalyst carried out of the tubular reactor in a separation section is controlled to be higher than the rising velocity of fluid through design, so that the solid catalyst carried out of the tubular reactor can freely settle and return to a catalyst bed layer.
6. The reaction system of the invention adopts forced circulation, and is provided with the raw material mixing tank, so that the full mixing of the reaction raw materials can be ensured, the total conversion rate of the reaction is improved, and the product yield is more than 70 percent (calculated by methanol group).
7. The reactor of the invention solves the defects of easy blockage of the catalyst bed layer, large resistance, uneven bed layer temperature and the like of the fixed bed reactor.
Drawings
FIG. 1 is a system block diagram of the present invention.
FIG. 2 is a view showing the structure of a reactor.
Number in fig. 1: the device comprises a raw material mixer 1, a tube type floating bed reactor 2, a circulating pump 3, a rectifying tower 4, a circulating pipeline 5, a backflow pipeline 6, a discharge pipe 7, an inlet liquid distributor 8, an outlet liquid distributor 9, a catalyst support member 10, a reaction liquid inlet N1, a reaction liquid outlet N2, a refrigerant inlet N3, a refrigerant outlet N4, a first temperature measuring port TE1, a second temperature measuring port TE2, a third temperature measuring port TE3 and a fourth temperature measuring port TE 4.
Detailed Description
The invention will now be further described by way of example with reference to the accompanying drawings.
Example 1:
referring to fig. 1, a reaction system for synthesizing polymethoxy dimethyl ether comprises a raw material mixer 1 and a tubular floating bed reactor 2. The bottom of the tubular floating bed reactor 2 is provided with a reaction liquid inlet N1, and the top of the tubular floating bed reactor 2 is provided with a reaction liquid outlet N2; the discharge port of the raw material mixer 1 is connected with the reaction liquid inlet N1 of the tube type floating bed reactor 2 through a circulating pipeline 5, a circulating pump 3 is installed in the circulating pipeline 5, the reaction liquid outlet N2 of the tube type floating bed reactor 2 is respectively connected with one end of a return pipeline 6 and one end of a discharge pipe 7, the other end of the return pipeline 6 is connected with the raw material mixer 1, and the other end of the discharge pipe 7 is connected with a downstream rectifying tower 4.
Referring to fig. 2, the shell and tube floating bed reactor 2 comprises a shell, parallel reaction tubes, an inlet liquid distributor 8, an outlet liquid distributor 9 and a catalyst support 10. The reaction tubes arranged in parallel are axially arranged in the middle of the shell; solid catalysts are filled in the reaction tubes which are arranged in parallel to form a catalyst bed layer, and a reserved floating space is formed in a cavity of the reaction tube above the catalyst bed layer; a solid-liquid phase separation cavity and a liquid outlet cavity are sequentially arranged in the shell adjacent to the axial top of the reaction tube array, and a liquid redistributor is arranged in the liquid outlet cavity to ensure that the solid catalyst carried out of the reaction tube array can be settled freely and return to the catalyst bed layer; an inlet liquid distributor is arranged in the shell adjacent to the axial bottom of the reaction tube array.
Four groups of temperature detectors, namely a first temperature detector TE1, a second temperature detector TE2, a third temperature detector TE3 and a fourth temperature detector TE4 are uniformly distributed in the tube array along the circumference of the reactor; each group of temperature measuring devices is provided with an upper measuring point, a middle measuring point and a lower measuring point.
The reaction tubes which are arranged in parallel are hermetically arranged in the middle of the inner part of the shell of the reactor; the lower part of the shell side of the reaction tube array is provided with a refrigerant inlet N3, and the upper part of the shell side of the reaction tube array is provided with a refrigerant outlet N4.
When the device works, 2000kg of methylal with the purity not lower than 99.0wt% and 2400kg of trioxymethylene with the purity not lower than 99.0wt% are added into a raw material mixer 1, the feeding speeds are respectively 30-80kg/min and 50-100kg/min, and the materials are uniformly mixed in the raw material mixer 1 through a stirring measure and then are sent to a tubular floating bed reactor 2. The shell-side heat exchange medium of the tube array type floating bed reactor 2 is used for controlling the temperature in the tube array type floating bed reactor 2 to be 50-150 ℃ and the pressure to be 0.1-3.0 MPaG. After the reaction, most of the crude reaction liquid returns to the raw material mixing system for continuous circulation according to the circulation ratio of 10: 1-50: 1, and the total conversion rate of trioxymethylene is higher than 85%.
Claims (3)
1. A reaction system for synthesizing polymethoxy dimethyl ether comprises a raw material mixer and a reactor, and is characterized in that: the reactor is a tube type floating bed reactor, the bottom of the reactor is provided with a reaction liquid inlet, and the top of the reactor is provided with a reaction liquid outlet; the discharge port of the raw material mixer is connected with the reaction liquid inlet of the reactor through a circulating pipeline, a circulating pump is installed in the circulating pipeline, the reaction liquid outlet of the reactor is respectively connected with one end of a return pipeline 6 and one end of a discharge pipe 7, the other end of the return pipeline 6 is connected with the raw material mixer, and the other end of the discharge pipe 7 is connected with a downstream rectification system;
the reactor comprises a shell and reaction tubes arranged in parallel, and the reaction tubes are axially arranged in the middle of the shell; solid catalysts are filled in the reaction tubes which are arranged in parallel to form a catalyst bed layer, and a reserved floating space is formed in a cavity of the reaction tube above the catalyst bed layer; a solid-liquid phase separation cavity and a liquid outlet cavity are sequentially arranged in the shell adjacent to the axial top of the reaction tube array, and a liquid redistributor is arranged in the liquid outlet cavity to ensure that the solid catalyst carried out of the reaction tube array can be settled freely and return to the catalyst bed layer; an inlet liquid distributor is arranged in the shell adjacent to the axial bottom of the reaction tube array;
the reaction tubes arranged in parallel are hermetically arranged in the middle of the reactor shell; the lower part of the shell side of the reaction tube array is provided with a refrigerant inlet, and the upper part of the shell side of the reaction tube array is provided with a refrigerant outlet;
four groups of temperature detectors are uniformly distributed in the tube array along the circumference of the reactor, and each group of temperature detectors is provided with an upper measuring point, a middle measuring point and a lower measuring point; when the method works, 2000kg of methylal with the purity not lower than 99.0wt% and 2400kg of trioxymethylene with the purity not lower than 99.0wt% are added into a raw material mixer, the materials are stirred and mixed uniformly, reaction raw liquid is sent to a reactor tube side through a feed pump, polymethoxy dimethyl ether is synthesized through catalytic reaction, reaction heat is removed through a reactor shell coolant medium, and the total conversion rate of trioxymethylene is more than 85%; and (3) recycling 95% of reaction liquid out of the reactor back to the raw material mixer, feeding the rest 5% of reaction liquid as reaction discharge material to a rectification system for separation, obtaining polymethoxy dimethyl ether product at the bottom of the rectification system, and returning light components at the top of the rectification system to the reaction system for recycling.
2. The reaction system for synthesizing polymethoxy dimethyl ether according to claim 1, wherein: the feeding speed of the methylal is 30-80kg/min, and the feeding speed of the trioxymethylene is 50-100 kg/min.
3. The reaction system for synthesizing polymethoxy dimethyl ether according to claim 1, wherein the reaction conditions are as follows: the temperature is 50-150 ℃, and the pressure of the reactor is 0.1-3.0 MpaG.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810391683.6A CN108484371B (en) | 2018-04-27 | 2018-04-27 | Reaction system for synthesizing polymethoxy dimethyl ether |
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| CN201810391683.6A CN108484371B (en) | 2018-04-27 | 2018-04-27 | Reaction system for synthesizing polymethoxy dimethyl ether |
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| CN109225114A (en) * | 2018-11-01 | 2019-01-18 | 葛沁怡 | A kind of self-loopa tubulation reaction unit with Hi-mixer and the reaction method using it |
| CN110787740A (en) * | 2019-11-08 | 2020-02-14 | 西安航天华威化工生物工程有限公司 | Gas, liquid and solid three-phase hydrogenation reaction system |
| CN112876390B (en) * | 2021-03-10 | 2024-03-26 | 昆明理工大学 | Production device for synthesizing multi-carbon mercaptan by using multi-carbon olefin |
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| WO2006045506A1 (en) * | 2004-10-25 | 2006-05-04 | Basf Aktiengesellschaft | Method for producing polyoxymethylene dimethyl ethers |
| CN203508030U (en) * | 2013-08-15 | 2014-04-02 | 北京科尔帝美工程技术有限公司 | Circulating device for preparing polymethoxy dimethyl ether |
| CN104974025B (en) * | 2014-04-11 | 2017-12-08 | 清华大学 | A kind of method for producing polymethoxy dimethyl ether |
| CN106390866A (en) * | 2016-10-08 | 2017-02-15 | 江苏凯茂石化科技有限公司 | Isothermal reactor for synthesizing polyoxymethylene dimethyl ether |
| CN206337198U (en) * | 2016-12-22 | 2017-07-18 | 淄博津昌助燃材料科技有限公司 | A kind of process units for producing polymethoxy dimethyl ether |
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