CN111072481A - Device and method for producing high-concentration dimethyl carbonate - Google Patents
Device and method for producing high-concentration dimethyl carbonate Download PDFInfo
- Publication number
- CN111072481A CN111072481A CN202010017387.7A CN202010017387A CN111072481A CN 111072481 A CN111072481 A CN 111072481A CN 202010017387 A CN202010017387 A CN 202010017387A CN 111072481 A CN111072481 A CN 111072481A
- Authority
- CN
- China
- Prior art keywords
- tower
- dimethyl carbonate
- methanol
- reflux
- iii
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 title claims abstract description 160
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 435
- 238000010992 reflux Methods 0.000 claims abstract description 122
- 238000007670 refining Methods 0.000 claims abstract description 46
- 239000002828 fuel tank Substances 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 51
- 239000000463 material Substances 0.000 claims description 42
- 239000000047 product Substances 0.000 claims description 36
- 239000007788 liquid Substances 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 21
- 238000007599 discharging Methods 0.000 claims description 20
- 238000004064 recycling Methods 0.000 claims description 17
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 claims description 15
- 239000000446 fuel Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical group OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 12
- 239000012043 crude product Substances 0.000 claims description 9
- 239000002699 waste material Substances 0.000 claims description 9
- 125000004122 cyclic group Chemical group 0.000 claims description 8
- 238000010533 azeotropic distillation Methods 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 5
- 238000000746 purification Methods 0.000 abstract description 6
- 238000000605 extraction Methods 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 239000003245 coal Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 238000005810 carbonylation reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000006315 carbonylation Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229940050176 methyl chloride Drugs 0.000 description 1
- 230000011987 methylation Effects 0.000 description 1
- 238000007069 methylation reaction Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/08—Purification; Separation; Stabilisation
Abstract
The invention discloses a device and a method for producing high-concentration dimethyl carbonate. Separating the low-concentration dimethyl carbonate in a light component removal tower, wherein one part of light components reflows, and the other part and heavy components are all sent into a methanol fuel tank; the mixture of dimethyl carbonate and methanol is taken out at the side and sent into a pressurizing tower. Separating by a pressurizing tower, sending high-concentration dimethyl carbonate obtained at the tower bottom to a refining tower for further purification; a methanol azeotrope containing 15-18% of dimethyl carbonate is distilled from the top of the tower, one part of the methanol azeotrope is refluxed, and the other part of the methanol azeotrope is sent to an atmospheric tower. Separating by an atmospheric tower, distilling off a part of azeotrope containing 30 percent concentration of dimethyl carbonate and methanol from the tower top to reflux, and sending the other part of azeotrope to a pressurizing tower; methanol is discharged from the bottom of the tower and sent to a methanol fuel tank. Separating high-concentration dimethyl carbonate in a refining tower, wherein one part of light components reflows, and the other part of light components and heavy components in a tower kettle are all sent to a methanol fuel tank; high-purity dimethyl carbonate with the content of more than 99.9 percent is obtained as a product by side line extraction.
Description
Technical Field
The invention relates to a device and a method for producing high-concentration dimethyl carbonate, in particular to a device and a method for refining and recovering dimethyl carbonate from low-concentration dimethyl carbonate, and particularly relates to a device and a method for refining and recovering dimethyl carbonate from low-concentration dimethyl carbonate by-produced in an ethylene glycol device.
Background
In recent years, coal-made glycol projects are hot, and more than 40 coal-made glycol projects are produced and constructed at present. Most of the coal-made glycol adopts coal as a raw material, and CO and H2 are respectively obtained through gasification, transformation, purification, separation and purification, wherein the CO is synthesized through catalytic coupling and refined to produce oxalate, and then the oxalate and H2 are subjected to hydrogenation reaction and are refined to obtain the glycol. The process flow is short, the cost is low, and the technology is the technology for preparing the ethylene glycol by the coal, which is the highest in concern at home at present. However, in the practical process of the technology for preparing ethylene glycol from coal, the CO generates dimethyl carbonate as a byproduct when a carbonylation reaction occurs. The byproduct dimethyl carbonate accounts for about 5-10% of the ethylene glycol production capacity, and the yield of a common coal-to-ethylene glycol project is dozens of thousands of tons or even millions of tons, so that the yield of the byproduct dimethyl carbonate is considerable. However, the by-produced dimethyl carbonate has a low purity and can be sold as a waste.
While high purity dimethyl carbonate (DMC) is an excellent solvent. Is an environment-friendly green chemical product which is widely concerned in recent years. Dimethyl carbonate is very active in chemical property, can easily react with various hydroxyl compounds, can replace virulent phosgene, dimethyl sulfate, methyl chloride and the like as a carbonylation agent and a methylation agent, and is an important organic synthesis intermediate. Dimethyl carbonate has the characteristics of low toxicity and high evaporation speed, and has good compatibility with other solvents. It has been classified as a non-toxic chemical in western europe, and its application as a solvent, such as a solvent for special paints, a solvent for high-energy batteries, a solvent for medical production, etc., has been vigorously developed, and it can also be used as a spray. The dimethyl carbonate with higher purity can be used as a production raw material of the lithium battery electrolytic solution. However, the byproduct dimethyl carbonate produced in the process of preparing ethylene glycol from coal has more impurities, and the purification method is a problem which needs to be solved urgently.
Disclosure of Invention
The invention aims to solve the technical problem of providing a device and a method for producing high-concentration dimethyl carbonate aiming at the defects in the prior art. The method takes low-concentration dimethyl carbonate as a raw material, wherein the content of the dimethyl carbonate is more than 30 percent, and the dimethyl carbonate is a dimethyl carbonate-containing waste material generated in the production process of ethylene glycol; the invention relates to a technology for producing high-concentration dimethyl carbonate by using low-concentration dimethyl carbonate.
In order to achieve the purpose, the invention adopts the following technical scheme:
the utility model provides a device of production high concentration dimethyl carbonate, is including the lightness-removing tower, pressurization tower, the refining tower that connect gradually, and low concentration dimethyl carbonate raw materials flow through in proper order and get high-purity dimethyl carbonate product after lightness-removing, pressurization, refining, its characterized in that:
the light component removing tower is characterized in that the top of the light component removing tower is provided with an exhaust port I, the bottom of the light component removing tower is provided with a discharge port I, the middle lower part of one side of the tower wall is provided with a feed port I, the upper part of the other side of the tower wall is provided with a reflux port I, and the middle upper part of the other side of the tower wall is provided with: the feed inlet I is connected with a device capable of providing a low-concentration dimethyl carbonate raw material; the exhaust port I is connected with a condenser I and a reflux tank I, the outlet of the reflux tank I is divided into two paths, the first path is connected with the reflux port I, and the second path is connected with the methanol fuel storage tank; the discharge port I is connected with a methanol fuel storage tank;
pressurizing tower, the top be equipped with gas vent II, the bottom is equipped with discharge gate III, the well lower part of tower wall one side is equipped with feed inlet II, the upper portion of tower wall opposite side is equipped with backward flow mouth II, wherein: the feed inlet II is divided into two paths, and the first path is connected with the discharge outlet II of the lightness-removing column; the exhaust port II is connected with a condenser II and a reflux tank II, the outlet of the reflux tank II is divided into two paths, the first path is connected with a reflux port II, and the second path is connected with an atmospheric tower;
atmospheric tower, the top be equipped with gas vent III, the bottom is equipped with discharge gate IV, the well lower part of tower wall one side is equipped with feed inlet III, the upper portion of tower wall opposite side is equipped with backward flow mouth III, wherein: the feed inlet III is connected with the second path of the outlet of the reflux tank II; the exhaust port III is connected with a condenser III and a reflux tank III, the outlet of the reflux tank III is divided into two paths, the first path is connected with a reflux port III, and the second path is connected with the second path of the feed port II of the pressurizing tower; the discharge port IV is connected with a methanol fuel storage tank;
refining tower, the top is equipped with gas vent IV, the bottom is equipped with discharge gate V, the well lower part of tower wall one side is equipped with feed inlet IV, the upper portion of tower wall opposite side is equipped with backward flow mouth IV, well upper portion is equipped with discharge gate VI, wherein: the feed inlet IV is connected with a discharge outlet III of the pressurizing tower; the exhaust port IV is connected with a condenser IV and a reflux tank IV, the outlet of the reflux tank IV is divided into two paths, the first path is connected with the reflux port IV, and the second path is connected with the methanol fuel storage tank; the discharge port V is connected with a methanol fuel storage tank; and the discharge port VI is connected with a product storage tank.
The lightness-removing column, the pressurizing column, the atmospheric column and the refining column are all conventional equipment sold in the field or equipment with corresponding functions.
The invention also provides a method for producing high-concentration dimethyl carbonate, which comprises the following steps:
(1) light weight removal and heavy weight removal: the low-concentration dimethyl carbonate raw material enters a light component removal tower through a feed inlet I, is separated in the light component removal tower, and after separation, light components are obtained at the top of the tower, heavy components are obtained at the bottom of the tower, and a primary crude product is obtained at the middle upper part of the tower wall; the light components are methylal and partial methanol, the methylal and partial methanol are discharged from an exhaust port I at the top of the tower, condensed by a condenser I to obtain liquid methylal and partial methanol, and then enter a reflux tank I, one part of materials in the reflux tank I flow back to the light component removal tower from a reflux port I for recycling, and the other part of materials are sent to a methanol fuel tank; the heavy component is oxalate which is discharged from a discharge port I at the bottom of the tower and then sent into a methanol fuel tank; the primary crude product is a mixture of dimethyl carbonate and methanol, is discharged from a discharge port II at the middle upper part of the tower wall and is sent into a pressurizing tower through a feed port II;
(2) and (3) pressurized azeotropic distillation: the method comprises the following steps of feeding a primary crude product in a light component removal tower into a pressurizing tower, carrying out azeotropic distillation in the pressurizing tower through pressurization, wherein due to the fact that methanol and dimethyl carbonate are subjected to azeotropy, the azeotropic proportion of the methanol and the dimethyl carbonate can be improved through pressurization, almost all the methanol is taken out in an azeotropic mode through a minimum amount of dimethyl carbonate, methanol azeotrope containing the dimethyl carbonate with the mass content of 15-18% is obtained at the tower top, and the dimethyl carbonate with the mass concentration of 98.95% -99.05% is obtained at the tower bottom; discharging a methanol azeotrope containing dimethyl carbonate with the mass content of 15-18% from an exhaust port II at the top of the tower, condensing the methanol azeotrope by a condenser II to obtain a liquid methanol azeotrope containing dimethyl carbonate, and then feeding the liquid methanol azeotrope into a reflux tank II, wherein one part of materials in the reflux tank II flow back to the pressurizing tower from a reflux port II for recycling, and the other part of materials are discharged and enter the normal pressure tower from a feed port III; discharging dimethyl carbonate with the mass concentration of 98.95-99.05% from a discharge hole III at the bottom of the tower and feeding the dimethyl carbonate into a refining tower through a feed hole IV;
(3) pressure swing separation: the methanol azeotrope containing dimethyl carbonate with the mass content of 15-18% enters an atmospheric tower, the azeotropic ratio of methanol and dimethyl carbonate is reduced due to the reduction of pressure, the methanol azeotrope containing dimethyl carbonate with the mass content of 29.95-30.05% is obtained at the tower top, and the methanol with the purity of more than 99.5% is obtained at the tower bottom; discharging a methanol azeotrope containing dimethyl carbonate with the mass content of 29.95-30.05% from an exhaust port III at the top of the tower, condensing the methanol azeotrope by a condenser III to obtain a liquid methanol azeotrope containing dimethyl carbonate, and then feeding the methanol azeotrope into a reflux tank III, wherein one part of materials in the reflux tank III flow back to the normal pressure tower from a reflux port III for recycling, and the other part of materials are discharged and returned to the pressurizing tower from a feed port II for recycling; discharging the methanol with the purity of more than 99.5 percent from a discharge hole IV at the bottom of the tower, and then sending the methanol into a methanol fuel tank to be sold as a product or returned to an oxalate system of an ethylene glycol production device for use;
(4) refining: the dimethyl carbonate with the mass concentration of 98.95-99.05% enters a refining tower, and is separated in the refining tower, light components are obtained at the top of the tower, heavy components are obtained at the bottom of the tower, and products are obtained at the middle upper part of the tower wall; the light components are discharged from an exhaust port IV at the top of the tower, condensed by a condenser IV to obtain liquid light components, and then enter a reflux tank IV, one part of the materials in the reflux tank IV flow back to the refining tower from a reflux port IV for recycling, and the other part of the materials is discharged and then sent to a methanol fuel tank; discharging heavy components from a discharge port V at the bottom of the tower and then sending the heavy components into a methanol fuel tank; the product is high-purity dimethyl carbonate with the mass content of more than 99.9 percent, and is discharged from a discharge hole VI at the middle upper part of the side wall and sent into a product storage tank.
In the above technical scheme, in the step (1), the mass concentration of dimethyl carbonate in the low-concentration dimethyl carbonate raw material is more than 30%, and dimethyl carbonate-containing waste materials generated in the ethylene glycol production process are preferred.
In the above technical scheme, in the step (1), the operation conditions of the light component removal tower are as follows: the temperature at the top of the tower is 95-105 ℃, and the pressure is 0.00-0.03 MpaG; the temperature of the tower bottom is 110-130 ℃, and the pressure is 0.00-0.0.05 MpaG.
In the technical scheme, in the step (1), the reflux ratio of the light component removal tower is 50-60.
In the above technical solution, in the step (2), the operation conditions of the pressurizing tower are as follows: the temperature at the top of the tower is 130-140 ℃, and the pressure is 0.80-1.00 MpaG; the temperature of the tower bottom is 170-190 ℃, and the pressure is 0.80-1.00 MpaG.
In the technical scheme, in the step (2), the reflux ratio of the pressurizing tower is 2-4.
In the above technical scheme, in the step (3), the operating conditions of the atmospheric tower are as follows: the temperature at the top of the tower is 60-65 ℃, and the pressure is 0.00-0.03 MpaG; the temperature of the tower bottom is 60-70 ℃, and the pressure is 0.00-0.05 MpaG.
In the technical scheme, in the step (3), the reflux ratio of the atmospheric tower is 1.5-3.
In the above technical solution, in the step (4), the refining tower has the following operating conditions: the temperature at the top of the tower is 80-100 ℃, and the pressure is 0.00-0.03 MpaG; the temperature of the tower bottom is 85-95 ℃, and the pressure is 0.00-0.05 MpaG.
In the technical scheme, in the step (4), the reflux ratio of the refining tower is 25-35.
The technical scheme of the invention has the advantages that:
(1) the raw material low-concentration dimethyl carbonate can be waste material generated in the production process of ethylene glycol, the waste material is dangerous waste, the waste material can be sold only at low price, the waste of dimethyl carbonate is caused, and the economic benefit is reduced and the environmental protection pressure is brought, so the invention has obvious economic benefit and environmental protection advantage.
(2) The raw material dimethyl carbonate with low concentration has low requirement on the concentration of dimethyl carbonate, and the concentration of the dimethyl carbonate is not less than 30%.
(3) The product of the invention has excellent quality: the product meets the requirements of national standard superior products of dimethyl carbonate.
Drawings
FIG. 1: a process flow diagram of the method of the invention;
FIG. 2 is a schematic view of the overall structure of the apparatus of the present invention;
wherein: 1 is a lightness-removing tower, 2 is a pressurizing tower, 3 is an atmospheric tower, and 4 is a refining tower.
Detailed Description
The following detailed description of the embodiments of the present invention is provided, but the present invention is not limited to the following descriptions:
the invention provides a device for producing high-concentration dimethyl carbonate, which comprises a light component removing tower 1, a pressurizing tower 2 and a refining tower 4 which are connected in sequence, wherein a low-concentration dimethyl carbonate raw material sequentially flows through light component removing, pressurizing and refining to obtain a high-purity dimethyl carbonate product, as shown in figure 2:
take off light tower 1, the top is equipped with gas vent I, the bottom is equipped with discharge gate I, the well lower part of tower wall one side is equipped with feed inlet I, the upper portion of tower wall opposite side is equipped with backward flow mouth I, well upper portion is equipped with discharge gate II, wherein: the feed inlet I is connected with a device capable of providing a low-concentration dimethyl carbonate raw material; the exhaust port I is connected with a condenser I and a reflux tank I, the outlet of the reflux tank I is divided into two paths, the first path is connected with the reflux port I, and the second path is connected with the methanol fuel storage tank; the discharge port I is connected with a methanol fuel storage tank;
pressurizing tower 2, the top is equipped with gas vent II, the bottom is equipped with discharge gate III, the well lower part of tower wall one side is equipped with feed inlet II, the upper portion of tower wall opposite side is equipped with backward flow mouth II, wherein: the feed inlet II is divided into two paths, and the first path is connected with the discharge outlet II of the lightness-removing tower 1; the exhaust port II is connected with a condenser II and a reflux tank II, the outlet of the reflux tank II is divided into two paths, the first path is connected with a reflux port II, and the second path is connected with an atmospheric tower 3;
atmospheric tower 3, the top is equipped with gas vent III, the bottom is equipped with discharge gate IV, the well lower part of tower wall one side is equipped with feed inlet III, the upper portion of tower wall opposite side is equipped with backward flow mouth III, wherein: the feed inlet III is connected with the second path of the outlet of the reflux tank II; the exhaust port III is connected with a condenser III and a reflux tank III, the outlet of the reflux tank III is divided into two paths, the first path is connected with a reflux port III, and the second path is connected with the second path of the feed port II of the pressurizing tower 2; the discharge port IV is connected with a methanol fuel storage tank;
refining tower 4, the top is equipped with gas vent IV, the bottom is equipped with discharge gate V, the well lower part of tower wall one side is equipped with feed inlet IV, the upper portion of tower wall opposite side is equipped with backward flow mouth IV, well upper portion is equipped with discharge gate VI, wherein: the feed inlet IV is connected with a discharge outlet III of the pressurizing tower 2; the exhaust port IV is connected with a condenser IV and a reflux tank IV, the outlet of the reflux tank IV is divided into two paths, the first path is connected with the reflux port IV, and the second path is connected with the methanol fuel storage tank; the discharge port V is connected with a methanol fuel storage tank; and the discharge port VI is connected with a product storage tank.
The invention also provides a method for producing high-concentration dimethyl carbonate, a flow chart is shown in figure 1, and the method comprises the following steps:
(1) light weight removal and heavy weight removal: the low-concentration dimethyl carbonate raw material enters a light component removal tower 1 through a feed inlet I, is separated in the light component removal tower, light components are obtained at the top of the tower after separation, heavy components are obtained at the bottom of the tower, and a primary crude product is obtained at the middle upper part of the tower wall; the light components are methylal and partial methanol, the methylal and partial methanol are discharged from an exhaust port I at the top of the tower, condensed by a condenser I to obtain liquid methylal and partial methanol, and then enter a reflux tank I, one part of materials in the reflux tank I flow back to the light component removal tower from a reflux port I for recycling, and the other part of materials are sent to a methanol fuel tank; the heavy component is oxalate which is discharged from a discharge port I at the bottom of the tower and then sent into a methanol fuel tank; the primary crude product is a mixture of dimethyl carbonate and methanol, is discharged from a discharge port II at the middle upper part of the tower wall and is sent into a pressurizing tower 2 through a feed port II;
(2) and (3) pressurized azeotropic distillation: the primary crude product in the light component removal tower enters a pressurizing tower 2, azeotropic distillation is carried out in the pressurizing tower through pressurization, the azeotropic proportion of methanol and dimethyl carbonate can be improved through the pressurization due to the azeotropic boiling of the methanol and the dimethyl carbonate, so that almost all the methanol is taken out in an azeotropic way by the least amount of dimethyl carbonate, methanol azeotrope containing the dimethyl carbonate with the mass content of 15-18% is obtained at the tower top, and the dimethyl carbonate with the mass concentration of 98.95-99.05% is obtained at the tower bottom; discharging a methanol azeotrope containing dimethyl carbonate with the mass content of 15-18% from an exhaust port II at the top of the tower, condensing the methanol azeotrope by a condenser II to obtain a liquid methanol azeotrope containing dimethyl carbonate, and then feeding the liquid methanol azeotrope into a reflux tank II, wherein one part of materials in the reflux tank II flow back to the pressurizing tower from a reflux port II for recycling, and the other part of materials are discharged and enter the atmospheric tower 3 from a feed port III; discharging dimethyl carbonate with the mass concentration of 98.95-99.05% from a discharge hole III at the bottom of the tower and feeding the dimethyl carbonate into a refining tower 4 through a feed hole IV;
(3) pressure swing separation: the dimethyl carbonate-containing methanol azeotrope with the mass content of 15-18% enters an atmospheric tower 3, the azeotropic ratio of methanol and dimethyl carbonate is reduced due to pressure reduction, the dimethyl carbonate-containing methanol azeotrope with the mass content of 29.95-30.05% is obtained at the tower top, and the methanol with the purity of more than 99.5% is obtained at the tower bottom; discharging a methanol azeotrope containing dimethyl carbonate with the mass content of 29.95-30.05% from an exhaust port III at the top of the tower, condensing the methanol azeotrope by a condenser III to obtain a liquid methanol azeotrope containing dimethyl carbonate, and then feeding the methanol azeotrope into a reflux tank III, wherein one part of materials in the reflux tank III flow back to the normal pressure tower from a reflux port III for recycling, and the other part of materials are discharged and returned to the pressurizing tower from a feed port II for recycling; discharging the methanol with the purity of more than 99.5 percent from a discharge hole IV at the bottom of the tower, and then sending the methanol into a methanol fuel tank to be sold as a product or returned to an oxalate system of an ethylene glycol production device for use;
(4) refining: the dimethyl carbonate with the mass concentration of 98.95-99.05% enters a refining tower 4, and is separated in the refining tower, light components are obtained at the top of the tower, heavy components are obtained at the bottom of the tower, and products are obtained at the middle upper part of the tower wall; the light components are discharged from an exhaust port IV at the top of the tower, condensed by a condenser IV to obtain liquid light components, and then enter a reflux tank IV, one part of the materials in the reflux tank IV flow back to the refining tower from a reflux port IV for recycling, and the other part of the materials is discharged and then sent to a methanol fuel tank; discharging heavy components from a discharge port V at the bottom of the tower and then sending the heavy components into a methanol fuel tank; the product is high-purity dimethyl carbonate with the mass content of more than 99.9 percent, and is discharged from a discharge hole VI at the middle upper part of the side wall and sent into a product storage tank.
The invention is illustrated below with reference to specific examples:
example 1:
a method for producing high-concentration dimethyl carbonate specifically comprises the following steps:
(1) light weight removal and heavy weight removal: the low-concentration dimethyl carbonate raw material (raw material composition, see table 1) enters a light component removal tower through a feed inlet I and is separated in the light component removal tower; separating to obtain light components at the top of the tower, wherein the light components are methylal and part of methanol, discharging from an exhaust port I, condensing by a condenser I to obtain liquid methylal and part of methanol, and feeding the liquid methylal and part of methanol into a reflux tank I; one part of the materials in the reflux tank returns to the lightness-removing column for recycling from a reflux opening I (the reflux ratio is 56), and the other part of the materials is connected with a methanol fuel tank; heavy components are obtained at the bottom of the tower after separation, and the heavy components are oxalate and are discharged from a discharge port I and sent into a methanol fuel tank; the mixture of dimethyl carbonate and methanol is taken from the side line of the light component removal tower and is sent into the pressurizing tower 2 through a discharge port II and a feed port II.
TABLE 1 composition of low concentration dimethyl carbonate feed
The light component removal tower has the following operating conditions: the temperature at the top of the tower is 97 ℃, and the pressure is 0.02 MpaG; the column bottom temperature was 118 ℃ and the pressure was 0.02 MpaG.
(2) And (3) pressurized azeotropic distillation: the material at the discharge port II of the light component removal tower enters a pressurizing tower 2, and in the pressurizing tower, because methanol and dimethyl carbonate are subjected to azeotropy, the azeotropic ratio of the methanol and the dimethyl carbonate can be improved by pressurizing, so that almost all the methanol is taken out in an azeotropy way by using the least amount of dimethyl carbonate. Dimethyl carbonate with the concentration of 99% is obtained at the bottom of the tower and is sent to a refining tower 4 through a discharge hole III for further purification. And (3) discharging 15-18% of azeotrope of dimethyl carbonate and methanol from an exhaust port II at the top of the tower, condensing the azeotrope by a condenser II to obtain a liquid azeotrope of methanol containing dimethyl carbonate, and then feeding the liquid azeotrope into a reflux tank II, wherein one part of materials in the reflux tank II reflux from a reflux port II (the reflux ratio is 3) to a pressurizing tower for cyclic utilization, and the other part of materials are discharged and enter an atmospheric tower 3 from a feed port III.
The operation conditions of the pressurizing tower 2 are as follows: the temperature at the top of the tower is 136 ℃, and the pressure is 0.90 MpaG; the column bottom temperature was 177 ℃ and the pressure was 0.90 MpaG.
(3) Pressure swing separation: and (2) introducing 15-18% dimethyl carbonate and methanol azeotrope into an atmospheric tower 3 through a feed inlet III, wherein the azeotropic ratio of methanol and dimethyl carbonate is reduced due to pressure reduction, the dimethyl carbonate and methanol azeotrope containing about 30% concentration is discharged from a gas outlet III at the top of the tower and condensed by a condenser III to obtain liquid dimethyl carbonate-containing methanol azeotrope, and then the liquid dimethyl carbonate-containing methanol azeotrope enters a reflux tank III, one part of the material in the reflux tank III is refluxed from a reflux inlet III (the reflux ratio is 2) to the atmospheric tower for cyclic utilization, and the other part of the material is discharged and returned to a pressurizing tower through a feed inlet II for cyclic treatment. The methanol with the purity of about 99.5 percent flows out of the tower kettle and is sent out of the battery limits through a discharge port IV to be sold as a product or returned to an oxalate system of the ethylene glycol production device for use.
The normal pressure tower (3) has the operating conditions that: the temperature at the top of the tower is 63 ℃ and the pressure is 0.01 MpaG; the temperature at the bottom of the column was 65 ℃ and the pressure 0.03 MpaG.
(4) Refining: dimethyl carbonate with the concentration of 99 percent from the bottom of the pressurizing tower enters a refining tower 4 and is separated in the refining tower; the light components are discharged from an exhaust port IV at the top of the tower, condensed by a condenser IV to obtain liquid light components, and then enter a reflux tank IV, one part of the materials in the reflux tank IV reflux from a reflux port IV (the reflux ratio is 30) to a refining tower for cyclic utilization, and the other part of the materials are discharged and then sent to a methanol fuel tank; discharging heavy components from a discharge port V at the bottom of the tower and then sending the heavy components into a methanol fuel tank; high-purity dimethyl carbonate with the content of more than 99.9 percent is obtained by side line extraction and is taken as a product, and the product is sent into a product tank through a discharge port VI.
The refining tower 4 has the following operating conditions: the temperature at the top of the tower is 83 ℃ and the pressure is 0.01 MpaG; the temperature at the bottom of the column was 90 ℃ and the pressure was 0.02 MpaG.
In the product of this example, the quality of dimethyl carbonate is higher than that of the high-grade product in the national standard of dimethyl carbonate (GB/T33107-2016), and the composition is shown in Table 2.
TABLE 2 dimethyl carbonate product composition
| Serial number | Composition of | Content (wt.) |
| 1 | Carbonic acid dimethyl ester | ≧99.9％ |
| 2 | Water (W) | ≤0.015％ |
| 3 | Methanol | ≤0.010％ |
Example 2:
a method for producing high-concentration dimethyl carbonate specifically comprises the following steps:
(1) removing light and heavy components: the low-concentration dimethyl carbonate raw material (raw material composition, see table 3) enters a light component removal tower 1 through a feed inlet I and is separated in the light component removal tower; separating to obtain light components at the top of the tower, wherein the light components are methylal and partial methanol, discharging the light components from an exhaust port I at the top of the tower, condensing the light components by a condenser I to obtain liquid methylal and partial methanol, and then feeding the liquid methylal and partial methanol into a reflux tank I, wherein one part of materials in the reflux tank I flows back from a reflux port I (the reflux ratio is 57) to a light component removal tower for recycling, and the other part of materials is fed into a methanol fuel tank; heavy components are obtained at the bottom of the tower after separation, and the heavy components are oxalate and are discharged from a discharge port I and sent into a methanol fuel tank; the mixture of dimethyl carbonate and methanol is taken from the side line of the light component removal tower and is sent into the pressurizing tower 2 through a discharge port II and a feed port II.
TABLE 3 Low concentration dimethyl carbonate feed composition
The light component removal tower (1) has the following operating conditions: the temperature at the top of the tower is 96 ℃, and the pressure is 0.019 MpaG; the column bottom temperature was 117 ℃ and the pressure 0.02 MpaG.
(2) Azeotropic distillation: the material at the discharge hole II of the light component removal tower enters a pressurizing tower, and the azeotropic ratio of methanol and dimethyl carbonate can be improved by pressurizing because the methanol and the dimethyl carbonate are subjected to azeotropy in the pressurizing tower, so that almost all the methanol is taken out by azeotropy with the least amount of dimethyl carbonate. Dimethyl carbonate with the concentration of 99% is obtained at the bottom of the tower and is sent to a refining tower 4 through a discharge hole III for further purification. And (3) discharging 15-18% of azeotrope of dimethyl carbonate and methanol from an exhaust port II at the top of the tower, condensing the azeotrope by a condenser II to obtain a liquid azeotrope of methanol containing dimethyl carbonate, and then feeding the liquid azeotrope into a reflux tank II, wherein one part of materials in the reflux tank II reflux from a reflux port II (the reflux ratio is 3) to a pressurizing tower for cyclic utilization, and the other part of materials are discharged and enter an atmospheric tower 3 from a feed port III.
The operation conditions of the pressurizing tower 2 are as follows: the temperature at the top of the tower is 134 ℃, and the pressure is 0.88 MpaG; the column bottom temperature was 175 ℃ and the pressure was 0.91 MpaG.
(3) Pressure swing separation: dimethyl carbonate and methanol azeotrope with the mass content of 15-18% enters an atmospheric tower 3 through a feed inlet III, the azeotropic ratio of methanol and dimethyl carbonate is reduced due to pressure reduction, the dimethyl carbonate and methanol azeotrope with the concentration of about 30% is discharged from a gas outlet III at the top of the tower and condensed by a condenser III to obtain liquid dimethyl carbonate-containing methanol azeotrope, the liquid dimethyl carbonate-containing methanol azeotrope enters a reflux tank III, one part of materials in the reflux tank III reflux from a reflux inlet III (the reflux ratio is 2) to the atmospheric tower for cyclic utilization, and the other part of materials are discharged and returned to a pressurizing tower through a feed inlet II for cyclic treatment; the methanol with the purity of about 99.5 percent flows out of the tower kettle and is sent out of the battery limits through a discharge port IV to be sold as a product or returned to an oxalate system of the ethylene glycol production device for use.
The operation conditions of the atmospheric tower 3 are as follows: the temperature at the top of the tower is 63 ℃ and the pressure is 0.01 MpaG; the temperature at the bottom of the column was 65 ℃ and the pressure 0.03 MpaG.
(4) Refining: dimethyl carbonate with the concentration of 99 percent enters a refining tower 4, after separation in the refining tower, light components are discharged from an exhaust port IV at the top of the tower and condensed by a condenser IV to obtain liquid light components, then the liquid light components enter a reflux tank IV, one part of materials in the reflux tank IV reflux from a reflux port IV (the reflux ratio is 30) to the refining tower for recycling, and the other part of the materials are discharged and then sent to a methanol fuel tank; discharging heavy components from a discharge port V at the bottom of the tower and then sending the heavy components into a methanol fuel tank; high-purity dimethyl carbonate with the content of more than 99.9 percent is obtained by side line extraction and is taken as a product, and the product is sent into a product tank through a discharge port VI.
The refining tower 4 has the following operating conditions: the temperature at the top of the tower is 83 ℃ and the pressure is 0.01 MpaG; the temperature at the bottom of the column was 90 ℃ and the pressure was 0.02 MpaG.
The refining tower (1).
In the product of this example, the quality of dimethyl carbonate is higher than that of the high-grade product in the national standard of dimethyl carbonate (GB/T33107-2016), and the composition is shown in Table 4.
TABLE 4 dimethyl carbonate product composition
| Serial number | Composition of | Content (wt.) |
| 1 | Carbonic acid dimethyl ester | ≧99.9％ |
| 2 | Water (W) | ≤0.015％ |
| 3 | Methanol | ≤0.010％ |
The above examples are only for illustrating the technical concept and features of the present invention, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (8)
1. A method for producing high-concentration dimethyl carbonate, which is characterized by comprising the following steps:
(1) light weight removal and heavy weight removal: the low-concentration dimethyl carbonate raw material enters a light component removal tower (1) through a feed inlet I, is separated in the light component removal tower (1), light components are obtained at the top of the tower after separation, heavy components are obtained at the bottom of the tower, and a primary crude product is obtained at the middle upper part of the tower wall; the light components are methylal and partial methanol, the methylal and partial methanol are discharged from an exhaust port I at the top of the tower, condensed by a condenser I to obtain liquid methylal and partial methanol, and then enter a reflux tank I, one part of materials in the reflux tank I flow back to the light component removal tower (1) from a reflux port I for recycling, and the other part of materials are sent to a methanol fuel tank; the heavy component is oxalate which is discharged from a discharge port I at the bottom of the tower and then sent into a methanol fuel tank; the primary crude product is a mixture of dimethyl carbonate and methanol, is discharged from a discharge port II at the middle upper part of the tower wall and is sent into a pressurizing tower (2) through a feed port II;
(2) and (3) pressurized azeotropic distillation: the method comprises the following steps that a primary crude product in a light component removal tower (1) enters a pressurizing tower (2), azeotropic rectification is carried out in the pressurizing tower (2) through pressurization, due to the fact that methanol and dimethyl carbonate are azeotropic, the azeotropic proportion of the methanol and the dimethyl carbonate can be improved through pressurization, almost all methanol is azeotropically taken out by the least amount of dimethyl carbonate, methanol azeotrope containing dimethyl carbonate with the mass content of 15-18% is obtained at the tower top, and dimethyl carbonate with the mass concentration of 98.95% -99.05% is obtained at the tower bottom; discharging a methanol azeotrope containing dimethyl carbonate with the mass content of 15-18% from an exhaust port II at the top of the tower, condensing the methanol azeotrope by a condenser II to obtain a liquid methanol azeotrope containing dimethyl carbonate, and then feeding the liquid methanol azeotrope into a reflux tank II, wherein one part of materials in the reflux tank II flow back to the pressurizing tower from a reflux port II for cyclic utilization, and the other part of the materials are discharged and enter the atmospheric tower (3) from a feed port III; the dimethyl carbonate with the mass concentration of 98.95-99.05 percent is discharged from a discharge hole III at the bottom of the tower and is sent into a refining tower (4) through a feed hole IV;
(3) pressure swing separation: the dimethyl carbonate-containing methanol azeotrope with the mass content of 15-18% enters an atmospheric tower (3), the azeotropic ratio of methanol and dimethyl carbonate is reduced due to pressure reduction, the dimethyl carbonate-containing methanol azeotrope with the mass content of 29.95-30.05% is obtained at the tower top, and the methanol with the purity of more than 99.5% is obtained at the tower bottom; discharging a methanol azeotrope containing dimethyl carbonate with the mass content of 29.95-30.05% from an exhaust port III at the top of the tower, condensing the methanol azeotrope by a condenser III to obtain a liquid methanol azeotrope containing dimethyl carbonate, and then feeding the methanol azeotrope into a reflux tank III, wherein one part of materials in the reflux tank III flow back to the normal pressure tower from a reflux port III for recycling, and the other part of materials are discharged and returned to the pressurizing tower from a feed port II for recycling; discharging the methanol with the purity of more than 99.5 percent from a discharge hole IV at the bottom of the tower, and then sending the methanol into a methanol fuel tank to be sold as a product or returned to an oxalate system of an ethylene glycol production device for use;
(4) refining: the dimethyl carbonate with the mass concentration of 98.95-99.05% enters a refining tower (4), and is separated in the refining tower (4), so that light components are obtained at the top of the tower, heavy components are obtained at the bottom of the tower, and products are obtained at the middle upper part of the tower wall; the light components are discharged from an exhaust port IV at the top of the tower, condensed by a condenser IV to obtain liquid light components, and then enter a reflux tank IV, one part of the materials in the reflux tank IV flow back to the refining tower from a reflux port IV for recycling, and the other part of the materials is discharged and then sent to a methanol fuel tank; discharging heavy components from a discharge port V at the bottom of the tower and then sending the heavy components into a methanol fuel tank; the product is high-purity dimethyl carbonate with the mass content of more than 99.9 percent, and is discharged from a discharge hole VI at the middle upper part of the side wall and sent into a product storage tank.
2. The method for producing high-concentration dimethyl carbonate according to claim 1, wherein in the step (1), the mass concentration of dimethyl carbonate in the low-concentration dimethyl carbonate raw material is more than 30%.
3. The method for producing high concentration dimethyl carbonate according to claim 2, wherein the low concentration dimethyl carbonate raw material is dimethyl carbonate-containing waste generated in the process of producing ethylene glycol.
4. The method for producing high concentration dimethyl carbonate according to claim 1, wherein in the step (1), the light component removal column (1) is operated under the following conditions: the temperature at the top of the tower is 95-105 ℃, and the pressure is 0.00-0.03 MpaG; the temperature of the tower bottom is 110-130 ℃, and the pressure is 0.00-0.0.05 MpaG; the reflux ratio of the light component removal tower (1) is 50-60.
5. The method for producing high concentration dimethyl carbonate according to claim 1, wherein in the step (2), the pressurized column (2) is operated under the following conditions: the temperature at the top of the tower is 130-140 ℃, and the pressure is 0.80-1.00 MpaG; the temperature of the tower bottom is 170-190 ℃, and the pressure is 0.80-1.00 MpaG; the reflux ratio of the pressurizing tower (2) is 2-4.
6. The method for producing high concentration dimethyl carbonate according to claim 1, wherein in the step (3), the atmospheric tower (3) is operated under the following conditions: the temperature at the top of the tower is 60-65 ℃, and the pressure is 0.00-0.03 MpaG; the temperature of the tower bottom is 60-70 ℃, and the pressure is 0.00-0.05 MpaG; the reflux ratio of the atmospheric tower (3) is 1.5-3.
7. The method for producing high concentration dimethyl carbonate according to claim 1, wherein in the step (4), the refining column (4) is operated under the following conditions: the temperature at the top of the tower is 80-100 ℃, and the pressure is 0.00-0.03 MpaG; the temperature of the tower bottom is 85-95 ℃, and the pressure is 0.00-0.05 MpaG; the reflux ratio of the refining tower (1) is 25-35.
8. The utility model provides a device of production high concentration dimethyl carbonate, is including lightness-removing tower (1), pressurized column (2), refining tower (4) that connect gradually, and low concentration dimethyl carbonate raw materials flow through in proper order and get high-purity dimethyl carbonate product after lightness-removing, pressurization, refining, its characterized in that:
take off light tower (1), the top is equipped with gas vent I, the bottom is equipped with discharge gate I, the well lower part of tower wall one side is equipped with feed inlet I, the upper portion of tower wall opposite side is equipped with backward flow mouth I, well upper portion is equipped with discharge gate II, wherein: the feed inlet I is connected with a device capable of providing a low-concentration dimethyl carbonate raw material; the exhaust port I is connected with a condenser I and a reflux tank I, the outlet of the reflux tank I is divided into two paths, the first path is connected with the reflux port I, and the second path is connected with the methanol fuel storage tank; the discharge port I is connected with a methanol fuel storage tank;
pressurizing tower (2), the top is equipped with gas vent II, the bottom is equipped with discharge gate III, the well lower part of tower wall one side is equipped with feed inlet II, the upper portion of tower wall opposite side is equipped with backward flow mouth II, wherein: the feed inlet II is divided into two paths, and the first path is connected with the discharge outlet II of the lightness-removing tower (1); the exhaust port II is connected with a condenser II and a reflux tank II, the outlet of the reflux tank II is divided into two paths, the first path is connected with a reflux port II, and the second path is connected with an atmospheric tower (3);
atmospheric tower (3), the top is equipped with gas vent III, the bottom is equipped with discharge gate IV, the well lower part of tower wall one side is equipped with feed inlet III, the upper portion of tower wall opposite side is equipped with backward flow mouth III, wherein: the feed inlet III is connected with the second path of the outlet of the reflux tank II; the exhaust port III is connected with a condenser III and a reflux tank III, the outlet of the reflux tank III is divided into two paths, the first path is connected with a reflux port III, and the second path is connected with the second path of the feed port II of the pressurizing tower (2); the discharge port IV is connected with a methanol fuel storage tank;
refined tower (4), the top is equipped with gas vent IV, the bottom is equipped with discharge gate V, the well lower part of tower wall one side is equipped with feed inlet IV, the upper portion of tower wall opposite side is equipped with backward flow mouth IV, well upper portion is equipped with discharge gate VI, wherein: the feed inlet IV is connected with a discharge outlet III of the pressurizing tower (2); the exhaust port IV is connected with a condenser IV and a reflux tank IV, the outlet of the reflux tank IV is divided into two paths, the first path is connected with the reflux port IV, and the second path is connected with the methanol fuel storage tank; the discharge port V is connected with a methanol fuel storage tank; and the discharge port VI is connected with a product storage tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010017387.7A CN111072481A (en) | 2020-01-08 | 2020-01-08 | Device and method for producing high-concentration dimethyl carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010017387.7A CN111072481A (en) | 2020-01-08 | 2020-01-08 | Device and method for producing high-concentration dimethyl carbonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111072481A true CN111072481A (en) | 2020-04-28 |
Family
ID=70322862
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010017387.7A Pending CN111072481A (en) | 2020-01-08 | 2020-01-08 | Device and method for producing high-concentration dimethyl carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111072481A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010755A (en) * | 2020-09-16 | 2020-12-01 | 贵州东华工程股份有限公司 | System for pressure swing double-effect rectification purification coarse dimethyl carbonate |
| CN114507136A (en) * | 2022-04-13 | 2022-05-17 | 太原理工大学 | Efficient synthesis method of lithium ion battery electrolyte mixed solvent |
| CN116531789A (en) * | 2023-07-06 | 2023-08-04 | 山东海科新源材料科技股份有限公司 | Purification device and method for dimethyl carbonate |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0920727A (en) * | 1995-07-07 | 1997-01-21 | Ube Ind Ltd | Distillation and separation of dimethyl carbonate |
| CN1903828A (en) * | 2006-08-15 | 2007-01-31 | 中国石油天然气股份有限公司 | Technology of producing dimethyl carbonate by alcoholysis of urea |
| CN101381309A (en) * | 2008-10-24 | 2009-03-11 | 华东理工大学 | Method for separating low concentration dimethyl carbonate by double-column process in dimethyl oxalate process |
| CN103980124A (en) * | 2014-05-09 | 2014-08-13 | 天津大学 | Synthetic method of diphenyl carbonate from propylene carbonate by catalysis of ionic liquid |
| CN105272857A (en) * | 2014-07-03 | 2016-01-27 | 中国石油化工股份有限公司 | Method for separating low-concentration dimethyl carbonate during process of synthesizing dimethyl oxalate with coal-based synthetic gas as raw material |
| CN106278896A (en) * | 2015-06-12 | 2017-01-04 | 中国石油化工股份有限公司 | The device of separating dimethyl carbonate during synthesizing dimethyl oxalate |
| CN110372512A (en) * | 2019-07-29 | 2019-10-25 | 太原理工大学 | A kind of process for separating and purifying of dimethyl carbonate |
| CN211814215U (en) * | 2020-01-08 | 2020-10-30 | 凯瑞环保科技股份有限公司 | Device for producing high-concentration dimethyl carbonate |
-
2020
- 2020-01-08 CN CN202010017387.7A patent/CN111072481A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0920727A (en) * | 1995-07-07 | 1997-01-21 | Ube Ind Ltd | Distillation and separation of dimethyl carbonate |
| CN1903828A (en) * | 2006-08-15 | 2007-01-31 | 中国石油天然气股份有限公司 | Technology of producing dimethyl carbonate by alcoholysis of urea |
| CN101381309A (en) * | 2008-10-24 | 2009-03-11 | 华东理工大学 | Method for separating low concentration dimethyl carbonate by double-column process in dimethyl oxalate process |
| CN103980124A (en) * | 2014-05-09 | 2014-08-13 | 天津大学 | Synthetic method of diphenyl carbonate from propylene carbonate by catalysis of ionic liquid |
| CN105272857A (en) * | 2014-07-03 | 2016-01-27 | 中国石油化工股份有限公司 | Method for separating low-concentration dimethyl carbonate during process of synthesizing dimethyl oxalate with coal-based synthetic gas as raw material |
| CN106278896A (en) * | 2015-06-12 | 2017-01-04 | 中国石油化工股份有限公司 | The device of separating dimethyl carbonate during synthesizing dimethyl oxalate |
| CN110372512A (en) * | 2019-07-29 | 2019-10-25 | 太原理工大学 | A kind of process for separating and purifying of dimethyl carbonate |
| CN211814215U (en) * | 2020-01-08 | 2020-10-30 | 凯瑞环保科技股份有限公司 | Device for producing high-concentration dimethyl carbonate |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010755A (en) * | 2020-09-16 | 2020-12-01 | 贵州东华工程股份有限公司 | System for pressure swing double-effect rectification purification coarse dimethyl carbonate |
| CN112010755B (en) * | 2020-09-16 | 2023-10-27 | 贵州东华工程股份有限公司 | System for purifying crude dimethyl carbonate by pressure-variable double-effect rectification |
| CN114507136A (en) * | 2022-04-13 | 2022-05-17 | 太原理工大学 | Efficient synthesis method of lithium ion battery electrolyte mixed solvent |
| CN114507136B (en) * | 2022-04-13 | 2022-06-21 | 太原理工大学 | Efficient synthesis method of lithium ion battery electrolyte mixed solvent |
| CN116531789A (en) * | 2023-07-06 | 2023-08-04 | 山东海科新源材料科技股份有限公司 | Purification device and method for dimethyl carbonate |
| CN116531789B (en) * | 2023-07-06 | 2023-09-19 | 山东海科新源材料科技股份有限公司 | Purification method of dimethyl carbonate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111072481A (en) | Device and method for producing high-concentration dimethyl carbonate | |
| CN106588599A (en) | Purification method of PODE (polyoxymethylene dimethyl ether) | |
| CN105111079A (en) | Method and device for separating acetic acid sec-butyl ester and sec-butyl alcohol | |
| CN111377800B (en) | Separation device and separation method for coal-to-ethanol liquid phase product | |
| CN109970565B (en) | Process for refining battery liquid-grade dimethyl carbonate by coupling of pressurization method and melt crystallization | |
| CN104725191A (en) | Ethylene glycol refining and separating method and system | |
| CN111100004B (en) | Method and integrated device for refining dimethyl carbonate | |
| CN113354540A (en) | Method for efficiently and continuously preparing methyl ethyl carbonate | |
| CN114163333B (en) | Method for synthesizing methyl ethyl carbonate in one step | |
| CN111377802A (en) | Preparation method and system of sec-butyl alcohol | |
| CN211814215U (en) | Device for producing high-concentration dimethyl carbonate | |
| CN111170863A (en) | Energy-saving process method and device for purifying dimethyl carbonate by adopting four-tower heat integration | |
| CN107556172B (en) | Process method for producing ethylene glycol mono-tert-butyl ether | |
| CN112010755B (en) | System for purifying crude dimethyl carbonate by pressure-variable double-effect rectification | |
| CN111377801B (en) | Method and system for refining low carbon alcohol | |
| CN115057761A (en) | Method for producing purified ethyl tert-butyl ether by reactive distillation coupled extraction distillation dividing wall tower technology | |
| CN110878006B (en) | Method and device for separating ethanol and ethyl acetate | |
| CN116265056A (en) | Product separation refining device and method for preparing dimethyl carbonate by CO esterification | |
| CN115400441B (en) | Device system and method for separating Fischer-Tropsch synthesis byproduct low-carbon alcohol | |
| CN106588655B (en) | Device and production process for synthesizing dimethyl carbonate by using reaction of urea and methanol | |
| CN113429261B (en) | System, method and application for separating and purifying ethanol from crude ethanol product | |
| CN111620843A (en) | Method for separating tetrahydrofuran-ethanol-water ternary azeotropic system by combining reactive distillation with side line extractive distillation | |
| CN111285755A (en) | Separation method of reaction product for preparing dimethyl ether by methanol dehydration | |
| CN219848214U (en) | Recovery device for dimethyl carbonate as byproduct of dimethyl oxalate synthesis | |
| CN114456069B (en) | Energy-saving process and system for producing and separating ethyl methyl carbonate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |