CN114160056A - Device for circularly producing dimethyl carbonate - Google Patents
Device for circularly producing dimethyl carbonate Download PDFInfo
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- CN114160056A CN114160056A CN202111485646.XA CN202111485646A CN114160056A CN 114160056 A CN114160056 A CN 114160056A CN 202111485646 A CN202111485646 A CN 202111485646A CN 114160056 A CN114160056 A CN 114160056A
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- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 title claims abstract description 31
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 141
- 238000006243 chemical reaction Methods 0.000 claims abstract description 102
- 239000007788 liquid Substances 0.000 claims abstract description 87
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 86
- 238000003860 storage Methods 0.000 claims abstract description 61
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 43
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 43
- 238000010992 reflux Methods 0.000 claims abstract description 27
- 238000004064 recycling Methods 0.000 claims abstract description 11
- 239000000725 suspension Substances 0.000 claims description 27
- 125000004122 cyclic group Chemical group 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 238000003780 insertion Methods 0.000 claims description 6
- 230000037431 insertion Effects 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 4
- 238000005485 electric heating Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 20
- 239000007789 gas Substances 0.000 description 17
- 239000003054 catalyst Substances 0.000 description 12
- 239000012295 chemical reaction liquid Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 239000011949 solid catalyst Substances 0.000 description 7
- 230000009471 action Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000005431 greenhouse gas Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/16—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with particles being subjected to vibrations or pulsations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0033—Other features
- B01D5/0036—Multiple-effect condensation; Fractional condensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation
- B01D5/0063—Reflux condensation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/04—Preparation of esters of carbonic or haloformic acids from carbon dioxide or inorganic carbonates
-
- 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
- Y02P20/141—Feedstock
Abstract
The invention discloses a device for circularly producing dimethyl carbonate, which comprises: the device comprises a reaction tank, a first condenser, a condensate storage tank, a rectifying tower, a second condenser, a liquid storage tank and a reflux tank; wherein: a liquid inlet and an air inlet are formed in the side wall of the reaction tank; the top wall of the reaction tank is provided with an exhaust port, the first condenser and the condensate storage tank are sequentially connected, and the condensate storage tank is connected with the air inlet; the liquid outlet of the reaction tank is connected with a rectifying tower, the top of the rectifying tower is provided with a fraction collecting port, and the fraction collecting port, the second condenser and the liquid storage tank are sequentially connected; the liquid outlet of rectifying column is connected with the reflux tank, the reflux tank is connected with the inlet of retort. The device for circularly producing the dimethyl carbonate can realize the recycling of two raw materials of methanol and carbon dioxide, and can effectively improve the utilization rate of the raw materials.
Description
Technical Field
The invention relates to the technical field of dimethyl carbonate preparation, in particular to a device for circularly producing dimethyl carbonate.
Background
Dimethyl carbonate is an important chemical raw material and is widely applied to the fields of resin, nitrocellulose, cellulose ether production, printing and dyeing and the like. In addition to this, dimethyl carbonate is also used as an organic synthesis intermediate for synthesis of agricultural chemicals, medicines, and the like. Various methods have been developed for the synthesis of dimethyl carbonate, but each method is more or less deficient and some methods have even been eliminated. The one-step synthesis of dimethyl carbonate by using carbon dioxide and methanol under the action of a catalyst is a process with good application prospect, which can use greenhouse gas carbon dioxide as a synthesis raw material, not only is the raw material easily available, but also the emission of greenhouse gas is reduced if the process can be implemented by using industrially produced carbon dioxide. However, the existing process has the problems of low utilization rate of methanol and carbon dioxide and low product yield, so that the process is difficult to be applied industrially, and for this reason, besides the aspects of the process and the catalyst, the further improvement and the improvement of the utilization rate of raw materials are also very important to develop an effective production system.
Disclosure of Invention
In order to solve the problems, the invention provides a device for circularly producing dimethyl carbonate, which can realize the recycling of two raw materials, namely methanol and carbon dioxide, and can effectively improve the utilization rate of the raw materials. In order to achieve the purpose, the invention adopts the following technical scheme.
An apparatus for the cyclic production of dimethyl carbonate, comprising: the device comprises a reaction tank, a first condenser, a condensate storage tank, a rectifying tower, a second condenser, a liquid storage tank and a reflux tank. Wherein: a liquid inlet and an air inlet are formed in the side wall of the reaction tank, so that methanol liquid and carbon dioxide gas can be conveniently pumped into the reaction tank. The top wall of the reaction tank is provided with an exhaust port, the first condenser and the condensate storage tank are sequentially connected, and the top of the condensate storage tank is connected with the air inlet so as to form a carbon dioxide circulation line and recycle carbon dioxide. The bottom of the condensate storage tank is connected with the liquid inlet and the rectifying tower. The liquid outlet and the rectifying column of retort are connected, the top of rectifying column has the fraction and collects the mouth, fraction is collected mouth, second condenser, liquid storage pot and is connected gradually, gets into the liquid storage pot after the diethyl carbonate condensation that obtains after the rectification becomes liquid and saves. The liquid outlet of rectifying column is connected with the reflux tank, the reflux tank is connected with the inlet of retort, and remaining liquid principal ingredients in the rectifying column after rectification is methyl alcohol, and it gets into and keeps in the reflux tank, supplies to the retort from the inlet as reaction raw materials when needing.
Furthermore, a suspension generator is arranged in the reaction tank and is fixed below the liquid inlet and the air inlet in a hanging manner. The suspension generator includes: barrel, ultrasonic vibrator stick and supersonic generator. Wherein: the bottom surface of the cylinder body is of a porous structure, strip-shaped supporting plates which are distributed in a radial shape are fixed in the upper end opening of the cylinder body, and gaps among the strip-shaped supporting plates are sealed through a pore plate. The strip-shaped supporting plate is provided with an insertion hole, the ultrasonic vibration rod is inserted into the insertion hole and is suspended in the cylinder body, and the ultrasonic generator is connected with the ultrasonic vibration rod. The suspension generator can enable the solid catalyst in the suspension generator to form a suspension with liquid under the action of the ultrasonic vibration rod, so that the reaction efficiency is improved.
Further, the liquid inlet is also connected with a methanol supply device so as to be convenient for supplementing the reaction tank with the methanol raw material.
Further, the condensate storage tank is also connected with a carbon dioxide supply device so as to supplement the carbon dioxide raw material to the reaction tank through the condensate storage tank.
Furthermore, a circulating fan and an exhaust control valve are arranged on a pipeline between the exhaust port and the first condenser. After the circulating fan and the exhaust control valve are opened, carbon dioxide in the reaction tank can be recycled among the reaction tank, the first condenser and the condensate storage tank conveniently.
Furthermore, a blower and a gas control valve are arranged on a pipeline between the gas inlet and the condensate storage tank, so that carbon dioxide in the condensate storage tank is sent to the reaction tank to participate in reaction.
Further, the air inlet is connected with the top wall of the condensate storage tank, so that carbon dioxide in the condensate storage tank enters the reaction tank through the condensate storage tank.
Furthermore, a first liquid feeding pump and a first liquid control valve are arranged on a connecting pipeline between the liquid outlet of the reaction tank and the rectifying tower, so that the reaction liquid in the reaction tank is fed into the rectifying tower to extract the target product dimethyl carbonate.
Furthermore, a second liquid feeding pump and a second liquid control valve are arranged on a connecting pipeline between the liquid outlet of the rectifying tower and the reflux tank, so that residual liquid in the rectifying tower can be conveniently fed into the reflux tank for temporary storage.
Furthermore, a third liquid feeding pump and a third liquid control valve are arranged on a connecting pipeline between the reflux tank and the liquid inlet of the reaction tank, so that the liquid in the reaction tank is fed into the reaction tank to realize cyclic utilization.
Further, the reaction tank has a heating function, and optionally, any suitable manner including electric heating, steam heating, and the like may be adopted.
Based on the technical scheme, the invention has the following beneficial effects:
(1) the device for producing the dimethyl carbonate can effectively improve the utilization rate of raw materials by recycling the carbon dioxide and the unreacted methanol in the reaction tank. Wherein, a circulation route is formed by the first condenser, the condensate storage tank and the reaction tank, the methanol volatilized from the carbon dioxide in the reaction tank enters the first condenser and then is condensed into liquid state to enter the bottom of the condensate storage tank for temporary storage, and can be used as a raw material for subsequent reaction, and the carbon dioxide still enters the condensate storage tank in the form of gas and enters the reaction tank again together with the supplemented carbon dioxide to participate in the reaction, the gas flow entering the reaction tank is kept the same as the discharged gas flow, so that the maximum carbon dioxide concentration is always kept in the reaction tank, the carbon dioxide consumed by participating in the reaction is compensated in real time, the reaction is promoted, meanwhile, the carbon dioxide can be utilized to the maximum extent through the recycling, and the carbon dioxide supply equipment connected with the condensate storage tank only needs to make up a small amount of carbon dioxide consumed by reaction. In addition, the residual liquid phase after rectification is reused by matching the rectification tower and the reflux tank, and the methanol can be recycled, because the main component of the residual liquid phase after the dimethyl carbonate in the reaction liquid is extracted by rectification is the methanol, the methanol is injected into the reflux tank for temporary storage, and the methanol is injected into the reaction tank again for recycling when needed.
(2) The invention arranges the suspension generator in the reaction tank, and the suspension generator can lead the solid catalyst in the suspension generator to form suspension with liquid under the action of the ultrasonic vibrating rod, thereby improving the reaction efficiency. Even if the reaction is carried out in the direction of generating the dimethyl carbonate by adding the catalyst in the reaction of the methanol and the carbon dioxide and then heating and pressurizing, the conversion rate of the reaction on the methanol is still low, and the adverse effect caused by serious accumulation of the catalyst is also caused, more than percent of the obtained reaction liquid is the methanol, a large amount of raw materials cannot be utilized, and a large amount of energy is consumed. Therefore, the invention arranges the suspension generator with the upper and lower ports sealed by the orifice plate, when in use, the solid catalyst is put in the suspension generator, and the solid catalyst forms suspension in methanol in the suspension generator under the action of the ultrasonic vibration rod after the methanol enters, so that the catalyst and the methanol can be in full contact reaction, and the catalyst can not be dispersed in the whole reaction liquid to cause the loss of the catalyst during the liquid outlet. In addition, the methanol molecules can be made more active by local liquid violent oscillation brought by the suspension generator, and can participate in the reaction more easily to promote the conversion rate of the methanol.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic structural diagram of an apparatus for the cyclic production of dimethyl carbonate according to the example.
Fig. 2 is a schematic structural diagram of a suspension generator in an embodiment.
Fig. 3 is a schematic structural diagram of the cartridge in the embodiment.
FIG. 4 is a schematic bottom structure of the cartridge in the example.
The labels in the figures represent: the device comprises a reaction tank 1, a first condenser 2, a condensate storage tank 3, a rectifying tower 4, a second condenser 5, a liquid storage tank 6, a reflux tank 7, a liquid inlet 8, an air inlet 9, an air outlet 10, a fraction collection port 11, a circulating fan 12, an exhaust control valve 13, a blower 14, a gas control valve 15, a first liquid feeding pump 16, a first liquid control valve 17, a second liquid feeding pump 18, a second liquid control valve 19, a third liquid feeding pump 20, a third liquid control valve 21, a cylinder 22, an ultrasonic vibration rod 23, an ultrasonic generator 24, a strip-shaped supporting plate 25, a pore plate 26 and a jack 27.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
In addition, the terms "mounted," "connected," "secured," and the like, as used herein, are intended to be broadly construed. For example, the connection can be fixed, detachable or integrated; the two components can be connected mechanically, directly or indirectly through an intermediate medium, or connected internally or in an interaction relationship, and the terms used in the description are understood by those skilled in the art as having specific meanings according to the specific situation. The technical scheme of the invention is further explained by combining the drawings and the embodiment of the specification.
With reference to fig. 1, the plant for the cyclic production of dimethyl carbonate, exemplified for this figure, comprises: retort 1, first condenser 2, condensate storage tank 3, rectifying column 4, second condenser 5, liquid storage pot 6 and reflux drum 7, wherein:
the reaction tank 1 has a heating function so as to heat the reaction tank 1 to promote the reaction. The heating function can adopt electric heating or steam heating, for example, an interlayer is arranged on the outer wall of the reaction tank 1, and then heating media such as high-temperature steam are introduced into the interlayer to heat the reaction tank 1. The upper part of the side wall of the reaction tank 1 is connected with a liquid inlet 8 and a gas inlet 9 so as to conveniently inject methanol liquid and carbon dioxide gas into the reaction tank 1. The liquid inlet 8 is also connected with a methanol supply device so as to supply methanol raw material to the reaction tank 1. The liquid inlet 8 is also connected with a methanol supply device so as to supply methanol raw materials to the reaction tank 1, the methanol supply device can be a methanol storage tank, and methanol in the methanol supply device is supplemented to the reaction tank 1 through an infusion pump to participate in the reaction when needed.
Have gas vent 10 on retort 1's the roof, gas vent 10, first condenser 2, condensate storage tank 3 connect gradually, condensate storage tank 3 is connected with air inlet 9 to form carbon dioxide circulation circuit, carry out cyclic utilization to carbon dioxide. A circulating fan 12 and an exhaust control valve 13 are arranged on a pipeline between the exhaust port 10 and the first condenser 2. After the circulating fan 12 and the exhaust control valve 13 are opened, the carbon dioxide in the reaction tank 1 can be recycled among the reaction tank 1, the first condenser 2 and the condensate storage tank 3. A blower 14 and a gas control valve 15 are arranged on a pipeline between the air inlet 9 and the condensate storage tank 3 so as to send the carbon dioxide in the condensate storage tank 3 into the reaction tank 1 to participate in reaction. The gas inlet 9 is connected with the top wall of the condensate storage tank 3, so that carbon dioxide in the condensate storage tank 3 enters the reaction tank 1 through the condensate storage tank 3. The condensate storage tank 3 is also connected with a carbon dioxide supply device so as to supplement the carbon dioxide raw material to the reaction tank 1 through the condensate storage tank 4. The utilization rate of the raw materials can be effectively improved by recycling the carbon dioxide and the unreacted methanol in the reaction tank 1. Wherein, a circulation route is formed by the first condenser 2, the condensate storage tank 3 and the reaction tank 1, the methanol volatilized from the carbon dioxide in the reaction tank 1 enters the first condenser 2, is condensed into a liquid state and enters the bottom of the condensate storage tank 3 for temporary storage, and can be used as a raw material for subsequent reaction, and the carbon dioxide still enters the condensate storage tank 3 in the form of gas and enters the reaction tank 1 again together with the supplemented carbon dioxide to participate in the reaction, the gas flow entering the reaction tank 1 is kept the same as the discharged gas flow, so that the maximum carbon dioxide concentration is always kept in the reaction tank 1, the carbon dioxide consumed by the participation in the reaction is compensated in real time, the reaction is promoted, meanwhile, the carbon dioxide can be utilized to the maximum extent through the recycling, and the carbon dioxide supply equipment connected with the condensate storage tank 3 only needs to make up a small amount of carbon dioxide consumed by reaction.
The bottom of the condensate storage tank 3 is connected with the liquid inlet 8, so that condensed methanol is pumped into the reaction tank for recycling. The liquid outlet of the reaction tank 1 is connected with the rectifying tower 4, and a first liquid feeding pump 16 and a first liquid control valve 17 are arranged on a connecting pipeline between the liquid outlet of the reaction tank 1 and the rectifying tower 4, so that the reaction liquid in the reaction tank 1 is fed into the rectifying tower 4 to extract the target product dimethyl carbonate. The top of rectifying column 4 has fraction collection mouth 11, second condenser 5, liquid storage pot 6 connect gradually, get into liquid storage pot 6 after the condensation of the diethyl carbonate that obtains after the rectification and store. The liquid outlet of the rectifying tower 4 is connected with the reflux tank 7, and a second liquid feeding pump 18 and a second liquid control valve 19 are arranged on a connecting pipeline between the liquid outlet of the rectifying tower 4 and the reflux tank 7, so that residual liquid in the rectifying tower 4 is fed into the reflux tank 7 for temporary storage. The reflux tank 7 is connected with the liquid inlet 8 of the reaction tank 1, and a third liquid feeding pump 20 and a third liquid control valve 21 are arranged on a connecting pipeline between the reflux tank 7 and the liquid inlet 8 of the reaction tank 1, so that the liquid in the reaction tank 1 is fed into the reaction tank 1 to realize cyclic utilization. The main component of the liquid remaining in the rectifying tower 4 after rectification is methanol, which enters the reflux tank 7 for temporary storage and is supplied to the reaction tank 1 from the liquid inlet 8 as a reaction raw material when needed. The residual liquid phase after rectification is reused by matching the rectification tower 4 and the reflux tank 7, and the methanol can be recycled, because the main component of the residual liquid phase after the dimethyl carbonate in the reaction liquid is extracted by rectification is methanol, the methanol is temporarily stored in the reflux tank 7, and is repeatedly used in the reaction tank 1 when needed.
Referring to fig. 2 to 4, in another preferred embodiment, a suspension generator is disposed in the reaction tank 1 and suspended below the liquid inlet 8 and the gas inlet 9. The suspension generator includes: a cylinder 22, an ultrasonic vibration rod 23 and an ultrasonic generator 24. Wherein: the bottom surface of the cylinder body 22 is of a porous structure, strip-shaped supporting plates 25 which are distributed in a radial shape are fixed in the upper end opening of the cylinder body 22, and gaps among the strip-shaped supporting plates 25 are sealed through a pore plate 26. The strip-shaped supporting plate 25 is provided with an insertion hole 27, the ultrasonic vibration rod 23 is inserted into the insertion hole 27 and enables the ultrasonic vibration rod 23 to be suspended in the cylinder body 22, and the ultrasonic generator 24 is connected with the ultrasonic vibration rod 23. The suspension generator can make the solid catalyst in the suspension generator form a suspension with the liquid under the action of the ultrasonic vibration rod 23, and the reaction efficiency is improved. Even if the reaction is carried out in the direction of generating the dimethyl carbonate by adding the catalyst in the reaction of the methanol and the carbon dioxide and then heating and pressurizing, the conversion rate of the reaction on the methanol is still low, and the adverse effect caused by serious accumulation of the catalyst is added, more than 70 percent of the obtained reaction liquid is the methanol, a large amount of raw materials cannot be utilized, and a large amount of energy is consumed. Therefore, the invention arranges the suspension generator with the upper and lower ports sealed by the orifice plate, when in use, the solid catalyst is put in the suspension generator, and the solid catalyst forms suspension in methanol in the suspension generator under the action of the ultrasonic vibration rod 24 after the methanol enters, so that the catalyst and the methanol are subjected to sufficient contact reaction, and the catalyst is not dispersed in the whole reaction liquid to cause the loss of the catalyst during the liquid outlet. In addition, the methanol molecules can be made more active by local liquid violent oscillation brought by the suspension generator, and can participate in the reaction more easily to promote the conversion rate of the methanol.
Finally, it should be understood that 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. Although the embodiments of the present invention have been described with reference to the accompanying drawings, it is not intended to limit the scope of the present invention, and it should be understood by those skilled in the art that various modifications and variations can be made without inventive efforts by those skilled in the art based on the technical solution of the present invention.
Claims (10)
1. An apparatus for the cyclic production of dimethyl carbonate, comprising: the device comprises a reaction tank, a first condenser, a condensate storage tank, a rectifying tower, a second condenser, a liquid storage tank and a reflux tank; wherein: a liquid inlet and an air inlet are formed in the side wall of the reaction tank; the top wall of the reaction tank is provided with an exhaust port, the first condenser and the condensate storage tank are sequentially connected, and the top of the condensate storage tank is connected with the air inlet; the bottom of the condensate storage tank is connected with the rectifying tower and the liquid inlet; the liquid outlet of the reaction tank is connected with a rectifying tower, the top of the rectifying tower is provided with a fraction collecting port, and the fraction collecting port, the second condenser and the liquid storage tank are sequentially connected; the liquid outlet of rectifying column is connected with the reflux tank, the reflux tank is connected with the inlet of retort.
2. The plant for the cyclic production of dimethyl carbonate according to claim 1, characterized in that the liquid inlet is also connected to a methanol supply; preferably, the condensate storage tank is further connected to a carbon dioxide supply.
3. The apparatus for recycling dimethyl carbonate according to claim 1, wherein a recycle blower and a vent control valve are provided on the pipeline between the vent and the first condenser.
4. The plant for the cyclic production of dimethyl carbonate according to claim 1, characterized in that a blower and a gas control valve are provided on the piping between the gas inlet and the condensate storage tank.
5. The plant for the cyclic production of dimethyl carbonate according to claim 1, characterized in that the gas inlet is connected to the top wall of the condensate storage tank.
6. The apparatus for circularly producing dimethyl carbonate according to claim 1, wherein a first liquid feeding pump and a first liquid control valve are arranged on a connecting pipeline between the liquid outlet of the reaction tank and the rectifying tower.
7. The apparatus for recycling dimethyl carbonate according to claim 1, wherein a second liquid feeding pump and a second liquid control valve are arranged on a connecting pipeline between the liquid outlet of the rectifying tower and the reflux tank.
8. The apparatus for recycling dimethyl carbonate according to claim 1, wherein a third liquid feeding pump and a third liquid control valve are arranged on the connecting pipeline between the reflux tank and the liquid inlet of the reaction tank.
9. The plant for the cyclic production of dimethyl carbonate according to claim 1, characterized in that the reaction tank has a heating function, preferably with electric heating or steam heating.
10. The device for cyclically producing the dimethyl carbonate according to any one of claims 1 to 9, wherein a suspension generator is arranged in the reaction tank and is fixed below the liquid inlet and the gas inlet in a suspending way; the suspension generator includes: the ultrasonic vibration device comprises a cylinder, an ultrasonic vibration rod and an ultrasonic generator; wherein: the bottom surface of the cylinder body is of a porous structure, strip-shaped supporting plates which are distributed in a radial shape are fixed in the upper end opening of the cylinder body, and gaps among the strip-shaped supporting plates are sealed through a pore plate; the strip-shaped supporting plate is provided with an insertion hole, the ultrasonic vibration rod is inserted into the insertion hole and is suspended in the cylinder body, and the ultrasonic generator is connected with the ultrasonic vibration rod.
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2021
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Application publication date: 20220311 |