CN103980096A - Method for separating methyl tert-butyl ether and dichloromethane through extractive distillation with salt - Google Patents
Method for separating methyl tert-butyl ether and dichloromethane through extractive distillation with salt Download PDFInfo
- Publication number
- CN103980096A CN103980096A CN201410187285.4A CN201410187285A CN103980096A CN 103980096 A CN103980096 A CN 103980096A CN 201410187285 A CN201410187285 A CN 201410187285A CN 103980096 A CN103980096 A CN 103980096A
- Authority
- CN
- China
- Prior art keywords
- tower
- butyl ether
- extractive distillation
- tertiary butyl
- methyl tertiary
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
- C07C17/386—Separation; Purification; Stabilisation; Use of additives by distillation with auxiliary compounds
Abstract
The invention discloses a method for separating methyl tert-butyl ether and dichloromethane through extractive distillation with salt. The method comprises the following steps: adding a mixed liquor raw material of methyl tert-butyl ether and dichloromethane and a composite extracting agent into an extractive distillation tower; carrying out extractive distillation and separation so as to obtain dichloromethane at the top of the tower and a mixture of methyl tert-butyl ether, the composite extracting agent and a trace amount of dichloromethane in the tower at the bottom of the tower; treating the mixture of methyl tert-butyl ether, the composite extracting agent and the trace amount of dichloromethane with a solvent recovery tower, allowing the trace amount of dichloromethane to be removed from the solvent recovery tower and to be distilled from the top of the solvent recovery tower and delivering the distilled trace amount of dichloromethane to the extractive distillation tower for cyclic separation; extracting methyl tert-butyl ether from the side at the upper part of the solvent recovery tower; and extracting the composite extracting agent from the bottom of the extractive distillation tower. The method provided by the invention can effectively separate methyl tert-butyl ether and dichloromethane; and after separation, dichloromethane with mass content of no less than 99.88% and methyl tert-butyl ether with mass content of no less than 99.50% are obtained.
Description
Technical field
The present invention relates to a kind of chemical separation technology, be specifically related to a kind of method of extractive distillation with salt separation methyl tertiary butyl ether and methylene dichloride.
Background technology
Methyl tertiary butyl ether english abbreviation is MTBE, has extensive use at chemical industry and biological field.The octane value of methyl tertiary butyl ether is higher, can well dissolve each other with gasoline, is the desirable blending component of producing white gasoline, high-octane rating, oxygenated gasoline, in worldwide, generally uses as gasoline dope.It can not only effectively improve gasoline octane rating and gasoline combustion efficiency, make in vehicle exhaust not leadedly, and can also improve automotive performance, reduce CO quantity discharged, reduce the discharge of other objectionable impuritiess (as ozone, benzene, divinyl etc.) simultaneously, reduce the cost of gasoline.Meanwhile, it is also a kind of important industrial chemicals, can prepare high-purity iso-butylene by cracking, also can be used for the production of Methylacrylaldehyde and methacrylic acid.But also studies have found that, it is easy to be integrated with water, and can infiltrate soil, destroy groundwater quality, think that it is a kind of possible pollutent.
Methylene dichloride has advantages of that dissolving power is strong and toxicity is low.In pharmaceutical industry, do reaction medium, for the preparation of penbritin, carbenicillin and cephalosporin etc.; Also as foam production whipping agent and metal cleaners etc. such as the solvent in film production, oil dewaxing solvent, aerosol propellants, organic synthesis-extraction agent, urethane.
In medicine production process, methyl tertiary butyl ether and methylene dichloride are two kinds of solvents wherein commonly using, due to the feature of production process, tend to produce the discarded solvent that contains in a large number methyl tertiary butyl ether and methylene dichloride, if these solvents are carried out directly discharging after biochemical treatment, not only pollute the environment, also can cause the waste of methyl tertiary butyl ether and these precious resources of methylene dichloride.If by these two kinds of solvent recuperation and be refined into high purity product realize recycle, will realize the double effects of changing waste into resources and environment protection.But, due to methyl tertiary butyl ether and methylene dichloride boiling-point difference of the two under normal pressure less, belong to the imperfection system of height, adopt conventional distillation method to be difficult to realize the separation and purification of the two.Therefore, developing efficient isolation technique for these two, to realize the dual role of its resource utilization and environment protection imperative.
Summary of the invention
The object of the present invention is to provide a kind of technique simple, separation efficiency is high, and a kind of extractive distillation with salt that is applicable to suitability for industrialized production separates the method for methyl tertiary butyl ether and methylene dichloride.
Technical scheme of the present invention is as follows:
Extractive distillation with salt separates a method for methyl tertiary butyl ether and methylene dichloride, and it is made up of following steps substantially:
Step 1., by the mixed solution raw material of methyl tertiary butyl ether and methylene dichloride and the composite extractant that is made up of inorganic salt and polyoxyethylene glycol, joins in extractive distillation column at different positions place respectively in certain proportion.The number of theoretical plate of described extractive distillation column is 40-60 piece column plate, in composite extractant, inorganic salt are selected from least one in halide salt or nitrate or vitriol, preferably at least one in sodium-chlor or SODIUMNITRATE or sodium sulfate, inorganic salt account for 1～5% of extraction agent total mass, the ratio range of raw material and composite extractant is 1:0.5～2, raw material enters tower position and (counts from top to bottom at theoretical plate number place, 20～30, middle part of extractive distillation column, lower same), composite extractant enter tower position on extractive distillation column top 5～10 theoretical plate number places, tower top temperature is 36～41 DEG C, tower reactor temperature is 55～58 DEG C, trim the top of column ratio is 2～5.After separation of extractive distillation, tower top obtains methylene dichloride more than mass content >=99.88, in tower reactor, is the mixture of methyl tertiary butyl ether and composite extractant and micro-methylene dichloride.
The mixture of step 2. obtains step 1 methyl tertiary butyl ether from tower reactor and composite extractant and micro-methylene dichloride adopts solvent recovery tower processing, in solvent recovery tower, the low-boiling-point substances such as the methylene dichloride of trace are removed substantially, and distillate from tower top, owing to wherein containing methyl tertiary butyl ether, therefore delivered to the extractive distillation column separation that again circulates; Solvent recovery tower top side line can the highly purified methyl tertiary butyl ether of extraction; Tower reactor extraction composite extractant is delivered to extractive distillation column and is recycled.The number of theoretical plate of described solvent recovery tower is 40～50 column plates, the mixture of methyl tertiary butyl ether and composite extractant and micro-methylene dichloride enters tower position at solvent recovery tower middle and lower part 30～40 column plates, top temperature is 49～52 DEG C, tower reactor temperature is 191～193 DEG C, trim the top of column ratio is 20～50, is preferably 25～40;
When solvent recovery tower top side line extraction methyl tertiary butyl ether, extraction mode can be vapour phase, can be also liquid phase, preferred liquid phase extraction, and the number of theoretical plate of side line extraction positional distance tower top is 5～15 column plates.
Above-mentioned extractive distillation with salt separates the method for methyl tertiary butyl ether and methylene dichloride, and described extractive distillation column and solvent recovery tower can be tray column or packing tower, or are the combination tower of tray column and packing tower.
The present invention can effectively separate methyl tertiary butyl ether and methylene dichloride, obtains respectively methylene dichloride and mass content >=99.50% methyl tertiary butyl ether of mass content >=99.88% after separation.Composite extractant recyclable regenerative used utilizes, and loss is low; Whole flow operations simple and flexible, invests littlely, and energy consumption is low, and environmental friendliness is particularly suitable for the recycling of the discarded methyl tertiary butyl ether of pharmacy procedure and methylene dichloride.
Brief description of the drawings
Below in conjunction with drawings and Examples, the invention will be further described.
Fig. 1 is the process flow diagram of one embodiment of the invention;
Number in the figure: 1, the mixed solution raw material of methyl tertiary butyl ether and methylene dichloride; 2, composite extractant; 3, methylene dichloride; 4, the mixture of methyl tertiary butyl ether and composite extractant and micro-methylene dichloride; 5(6), methylene dichloride and a small amount of methyl tertbutyl ether mixture; 7, methyl tertiary butyl ether; 8, the composite extractant reclaiming; 9, extractive distillation column raw material feed entrance point; 10, extractant feed position; 11, solvent recovery tower raw material feed entrance point; 12, side line is adopted position; T1-extractive distillation column T2-solvent recovery tower;
Fig. 2 is extractive distillation column schematic diagram of the present invention;
Number in the figure: 21, tower reactor; 22 tower reactor charging openings; 23, material inlet; 24, extractant feed mouth; 25, condenser; 26, return tank; 27, refluxing opening; 28, filler or column plate; 29, heating coil; 30, tower reactor discharge port.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment and accompanying drawing, the invention will be further described, and this embodiment only, for explaining the present invention, does not form limiting the scope of the present invention.
Embodiment 1
Taking the mixed solution raw material of methyl tertiary butyl ether and methylene dichloride (stream strand 1) treatment capacity as 1000kg/h, it consists of 71.2wt% methyl tertiary butyl ether, 28.8 wt% methylene dichloride, as shown in Figure 1, extractive distillation column experimental installation as shown in Figure 2 for processing technological flow.
Composite extractant is made up of inorganic salt and polyoxyethylene glycol, and in composite extractant (stream thigh 2), the mass content of Repone K is 3%; Raw material and composite extractant mass ratio are 1:1.5.
Extracting rectifying column internals adopts 3 × 3 θ ring Stainless Steel Helicess, and theoretical plate number is 50, and tower diameter is 50mm, and tower reactor adopts coil pipe heating, and raw material and composite extractant inlet amount adopt the control of high pressure micro pump.Tower top working pressure is normal pressure, 37.1～41.1 DEG C of tower top temperatures, and tower reactor temperature 56.3～57.5, trim the top of column is than 3～4; Raw material enters tower at the 25th theoretical tray place, and composite extractant enters tower at the 6th column plate place, and extracting rectifying overhead fraction (stream thigh 3) produced quantity is 280 kg/h, wherein mass content >=99.76% of methylene dichloride; The mixture of the methyl tertiary butyl ether in tower reactor and composite extractant and micro-methylene dichloride enters solvent recovery tower.
Solvent recuperation column internals adopts glass spring silk filler, and number of theoretical plate is 40, and internal diameter is 50mm, and tower reactor adopts coil pipe heating, and raw material inlet amount adopts the control of high pressure micro pump.Tower top working pressure is normal pressure, 51.5～52.1 DEG C of tower top temperatures, and 191.5～192.8 DEG C of tower reactor temperature, trim the top of column is than 30; Raw material enters tower at the 30th theoretical tray place, side line extraction mouth is 7 apart from tower top number of theoretical plate, produced quantity is 244.8 kg/h, can obtain methyl tertiary butyl ether more than mass content >=99.50%, an overhead fraction part (stream thigh 5) extraction, another part (flowing thigh 6) is delivered to extractive distillation column circulation and is separated, and tower reactor extraction composite extractant (stream thigh 8) is delivered to extractive distillation column and recycled.
Embodiment 2
Taking the mixed solution raw material of methyl tertiary butyl ether and methylene dichloride (stream strand 1) treatment capacity as 1000kg/h, it consists of 68.7wt% methyl tertiary butyl ether, 31.3 wt% methylene dichloride, as shown in Figure 1, extractive distillation column experimental installation as shown in Figure 2 for processing technological flow.
Composite extractant is made up of inorganic salt and polyoxyethylene glycol, and in composite extractant (stream thigh 2), the mass content of sodium-chlor is 2.5%; Raw material and composite extractant mass ratio are 1:1.
Extracting rectifying column internals adopts 3 × 3 θ ring Stainless Steel Helicess, and theoretical plate number is 40, and tower diameter is 50mm, and tower reactor adopts coil pipe heating, and raw material and composite extractant inlet amount adopt the control of high pressure micro pump.Tower top working pressure is normal pressure, 37.1～38.4 DEG C of tower top temperatures, and tower reactor temperature 56.7～58.1, trim the top of column is than 2～3; Raw material enters tower at the 20th theoretical tray place, and composite extractant enters tower about the 5th column plate place, and extracting rectifying overhead fraction (stream thigh 3) produced quantity is 310 kg/h, wherein mass content >=99.88% of methylene dichloride; The mixture of the methyl tertiary butyl ether in tower reactor and composite extractant and micro-methylene dichloride enters solvent recovery tower.
Solvent recuperation column internals adopts glass spring silk filler, and number of theoretical plate is 45, and internal diameter is 50mm, and tower reactor adopts coil pipe heating, and raw material inlet amount adopts the control of high pressure micro pump.Tower top working pressure is normal pressure, 50.1～51.89 DEG C of tower top temperatures, and 192.3～192.8 DEG C of tower reactor temperature, trim the top of column is than 35; Raw material enters tower at the 35th theoretical tray place, side line extraction mouth is 15 apart from tower top number of theoretical plate, produced quantity is 234.6 kg/h, can obtain methyl tertiary butyl ether more than mass content >=99.67%, an overhead fraction part (stream thigh 5) extraction, another part (flowing thigh 6) is delivered to extractive distillation column circulation and is separated, and tower reactor extraction composite extractant (stream thigh 8) is delivered to extractive distillation column and recycled.
Embodiment 3
Taking the mixed solution raw material of methyl tertiary butyl ether and methylene dichloride (stream strand 1) treatment capacity as 1000kg/h, it consists of 74.8wt% methyl tertiary butyl ether, 25.2 wt% methylene dichloride, as shown in Figure 1, extractive distillation column experimental installation as shown in Figure 2 for processing technological flow.
Composite extractant is made up of inorganic salt and polyoxyethylene glycol, and in composite extractant (stream thigh 2), the mass content of SODIUMNITRATE is 4%; Raw material and composite extractant mass ratio are 1:1.2.
Extracting rectifying column internals adopts 3 × 3 θ ring Stainless Steel Helicess, and theoretical plate number is 55, and tower diameter is 50mm, and tower reactor adopts coil pipe heating, and raw material and composite extractant inlet amount adopt the control of high pressure micro pump.Tower top working pressure is normal pressure, 36.8～37.6 DEG C of tower top temperatures, and tower reactor temperature 56.7～58.1, trim the top of column is than 2～3; Raw material enters tower at the 25th theoretical tray place, and composite extractant enters tower at the 8th column plate place, and extracting rectifying overhead fraction (stream thigh 3) produced quantity is 250 kg/h, wherein mass content >=99.79% of methylene dichloride; The mixture of the methyl tertiary butyl ether in tower reactor and composite extractant and micro-methylene dichloride enters solvent recovery tower.
Solvent recuperation column internals adopts glass spring silk filler, and number of theoretical plate is 50, and internal diameter is 50mm, and tower reactor adopts coil pipe heating, and raw material inlet amount adopts the control of high pressure micro pump.Tower top working pressure is normal pressure, 51.5～52.3 DEG C of tower top temperatures, and 192.5～192.9 DEG C of tower reactor temperature, trim the top of column is than 30; Raw material enters tower at the 40th theoretical tray place, side line extraction mouth is 10 apart from tower top number of theoretical plate, produced quantity is 255 kg/h, can obtain methyl tertiary butyl ether more than mass content >=99.53%, an overhead fraction part (stream thigh 5) extraction, another part (flowing thigh 6) is delivered to extractive distillation column circulation and is separated, and tower reactor extraction composite extractant (stream thigh 8) is delivered to extractive distillation column and recycled.
Embodiment 4
Taking the mixed solution raw material of methyl tertiary butyl ether and methylene dichloride (stream strand 1) treatment capacity as 1000kg/h, it consists of 74.8wt% methyl tertiary butyl ether, 25.2 wt% methylene dichloride, as shown in Figure 1, extractive distillation column experimental installation as shown in Figure 2 for processing technological flow.
Composite extractant is made up of inorganic salt and polyoxyethylene glycol, and in composite extractant (stream thigh 2), the mass content of SODIUMNITRATE is 1%, and sodium sulfate is 2%; Raw material and composite extractant mass ratio are 1:2.
Extracting rectifying column internals adopts 3 × 3 θ ring Stainless Steel Helicess, and theoretical plate number is 55, and tower diameter is 50mm, and tower reactor adopts coil pipe heating, and raw material and composite extractant inlet amount adopt the control of high pressure micro pump.Tower top working pressure is normal pressure, 36.7～38.3 DEG C of tower top temperatures, and tower reactor temperature 57,2～58.1, trim the top of column is than 2～3; Raw material enters tower at the 25th theoretical tray place, and composite extractant enters tower at the 5th column plate place, and extracting rectifying overhead fraction (stream thigh 3) produced quantity is 250 kg/h, wherein mass content >=99.68% of methylene dichloride; The mixture of the methyl tertiary butyl ether in tower reactor and composite extractant and micro-methylene dichloride enters solvent recovery tower.
Solvent recuperation column internals adopts glass spring silk filler, and number of theoretical plate is 40, and internal diameter is 50mm, and tower reactor adopts coil pipe heating, and raw material inlet amount adopts the control of high pressure micro pump.Tower top working pressure is normal pressure, 50.9～52.1 DEG C of tower top temperatures, and 191.8～192.6 DEG C of tower reactor temperature, trim the top of column is than 35; Raw material enters tower at the 30th theoretical tray place, side line extraction mouth is 15 apart from tower top number of theoretical plate, produced quantity is 255 kg/h, can obtain methyl tertiary butyl ether more than mass content >=99.61%, an overhead fraction part (stream thigh 5) extraction, another part (flowing thigh 6) is delivered to extractive distillation column circulation and is separated, and tower reactor extraction composite extractant (stream thigh 8) is delivered to extractive distillation column and recycled.
The inventive method is not subject to the restriction of above-mentioned concrete device and processing parameter, those skilled in the art are according to processing condition, can adjust or implement within the scope of the present invention corresponding conversion to relevant parameters, also can, according to the size of stock liquid treatment capacity, amplify accordingly in proportion.
Claims (6)
1. extractive distillation with salt separates a method for methyl tertiary butyl ether and methylene dichloride, it is characterized in that: comprise the following steps:
(1) by the mixed solution raw material of methyl tertiary butyl ether and methylene dichloride and the composite extractant that formed by inorganic salt and polyoxyethylene glycol, join in extractive distillation column at different positions place respectively; After separation of extractive distillation, tower top obtains methylene dichloride, in tower reactor, is the mixture of methyl tertiary butyl ether and composite extractant and micro-methylene dichloride;
(2) methyl tertiary butyl ether step (1) being obtained from tower reactor and the mixture of composite extractant and micro-methylene dichloride adopt solvent recovery tower processing, in solvent recovery tower, the methylene dichloride of trace removes, and distillate from tower top, owing to wherein containing methyl tertiary butyl ether, therefore delivered to the extractive distillation column separation that again circulates; Extraction methyl tertiary butyl ether of solvent recovery tower top side line; Tower reactor extraction composite extractant is delivered to extractive distillation column and is recycled.
2. extractive distillation with salt according to claim 1 separates the method for methyl tertiary butyl ether and methylene dichloride, it is characterized in that: inorganic salt account for 1～5% of extraction agent total mass, and described inorganic salt are at least one in sodium-chlor, SODIUMNITRATE, sodium sulfate.
3. extractive distillation with salt according to claim 1 and 2 separates the method for methyl tertiary butyl ether and methylene dichloride, it is characterized in that: the number of theoretical plate of described extractive distillation column is 40-60 piece column plate, the mass ratio of mixed solution raw material and composite extractant is 1:0.5～2, raw material enters tower position at 20～30 theoretical plate number places, extractive distillation column middle part, composite extractant enter tower position on extractive distillation column top 5～10 theoretical plate number places, tower top temperature is 36～41 DEG C, tower reactor temperature is 55～58 DEG C, and trim the top of column ratio is 2～5.
4. extractive distillation with salt according to claim 1 and 2 separates the method for methyl tertiary butyl ether and methylene dichloride, it is characterized in that: the number of theoretical plate of described solvent recovery tower is 40～50 column plates, the mixture of methyl tertiary butyl ether and composite extractant and micro-methylene dichloride enters tower position at solvent recovery tower middle and lower part 30～40 column plates, top temperature is 49～52 DEG C, tower reactor temperature is 191～193 DEG C, trim the top of column ratio is 20～50, is preferably 25～40.
5. extractive distillation with salt according to claim 1 and 2 separates the method for methyl tertiary butyl ether and methylene dichloride, it is characterized in that: when solvent recovery tower top side line extraction methyl tertiary butyl ether, extraction mode is vapour phase or liquid phase, and the number of theoretical plate of side line extraction positional distance tower top is 5～15 column plates.
6. extractive distillation with salt according to claim 1 and 2 separates the method for methyl tertiary butyl ether and methylene dichloride, it is characterized in that: described extractive distillation column and solvent recovery tower are tray column or packing tower, or the combination tower of tray column and packing tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410187285.4A CN103980096B (en) | 2014-05-06 | 2014-05-06 | Extractive distillation with salt is separated the method for methyl tertiary butyl ether and methylene dichloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410187285.4A CN103980096B (en) | 2014-05-06 | 2014-05-06 | Extractive distillation with salt is separated the method for methyl tertiary butyl ether and methylene dichloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103980096A true CN103980096A (en) | 2014-08-13 |
| CN103980096B CN103980096B (en) | 2016-02-10 |
Family
ID=51272300
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410187285.4A Expired - Fee Related CN103980096B (en) | 2014-05-06 | 2014-05-06 | Extractive distillation with salt is separated the method for methyl tertiary butyl ether and methylene dichloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103980096B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926595A (en) * | 2015-05-15 | 2015-09-23 | 大连理工大学 | Separation process of removing dimethyl ether impurities in chloromethane through water absorption |
| CN113292389A (en) * | 2021-06-16 | 2021-08-24 | 江苏超跃化学有限公司 | Method for separating 2, 4-dichlorotoluene from dichlorotoluene mixed solution |
| CN113402360A (en) * | 2021-06-16 | 2021-09-17 | 江苏超跃化学有限公司 | Method for separating 2, 5-dichlorotoluene from dichlorotoluene mixed solution |
| CN116332720A (en) * | 2022-07-28 | 2023-06-27 | 四川熔增环保科技有限公司 | Recovery and purification method of waste solvent |
| CN117682946A (en) * | 2024-02-02 | 2024-03-12 | 烟台国邦化工机械科技有限公司 | Continuous recovery process and device for high-purity MTBE |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6413043A (en) * | 1987-07-07 | 1989-01-17 | Mitsui Toatsu Chemicals | Distillation and purification of neophyl halide |
| JPS6461439A (en) * | 1987-09-01 | 1989-03-08 | Mitsui Toatsu Chemicals | Method for distilling and purifying neophyl halides |
| CN1169415A (en) * | 1996-06-25 | 1998-01-07 | 赫彻斯特股份公司 | Process for preparation and fractionation of mixture of dimethyl ether and chloromethane with methanol as extractant |
| CN1169414A (en) * | 1996-06-25 | 1998-01-07 | 赫彻斯特股份公司 | Process for preparation and fractionation of mixture of dimethyl ether and chloromethane with water as extractant |
| WO2010043161A1 (en) * | 2008-10-13 | 2010-04-22 | 微宏动力系统（湖州）有限公司 | Methods for preparing methyl bromide, higher hydrocarbon, methanol and dimethyl ether from methane |
-
2014
- 2014-05-06 CN CN201410187285.4A patent/CN103980096B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6413043A (en) * | 1987-07-07 | 1989-01-17 | Mitsui Toatsu Chemicals | Distillation and purification of neophyl halide |
| JPS6461439A (en) * | 1987-09-01 | 1989-03-08 | Mitsui Toatsu Chemicals | Method for distilling and purifying neophyl halides |
| CN1169415A (en) * | 1996-06-25 | 1998-01-07 | 赫彻斯特股份公司 | Process for preparation and fractionation of mixture of dimethyl ether and chloromethane with methanol as extractant |
| CN1169414A (en) * | 1996-06-25 | 1998-01-07 | 赫彻斯特股份公司 | Process for preparation and fractionation of mixture of dimethyl ether and chloromethane with water as extractant |
| EP0816313A1 (en) * | 1996-06-25 | 1998-01-07 | Hoechst Aktiengesellschaft | Process for the preparation and separation of a mixture of dimethyl ether and chloromethane using methanol as the extractant |
| WO2010043161A1 (en) * | 2008-10-13 | 2010-04-22 | 微宏动力系统（湖州）有限公司 | Methods for preparing methyl bromide, higher hydrocarbon, methanol and dimethyl ether from methane |
Non-Patent Citations (1)
| Title |
|---|
| 汪申等: "《CHEMCAD典型应用实例 下 化学工业与炼油工业》", 31 August 2006, article "加盐萃取精馏", pages: 24-27 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926595A (en) * | 2015-05-15 | 2015-09-23 | 大连理工大学 | Separation process of removing dimethyl ether impurities in chloromethane through water absorption |
| CN113292389A (en) * | 2021-06-16 | 2021-08-24 | 江苏超跃化学有限公司 | Method for separating 2, 4-dichlorotoluene from dichlorotoluene mixed solution |
| CN113402360A (en) * | 2021-06-16 | 2021-09-17 | 江苏超跃化学有限公司 | Method for separating 2, 5-dichlorotoluene from dichlorotoluene mixed solution |
| CN116332720A (en) * | 2022-07-28 | 2023-06-27 | 四川熔增环保科技有限公司 | Recovery and purification method of waste solvent |
| CN116332720B (en) * | 2022-07-28 | 2024-03-12 | 四川熔增环保科技有限公司 | Recovery and purification method of waste solvent |
| CN117682946A (en) * | 2024-02-02 | 2024-03-12 | 烟台国邦化工机械科技有限公司 | Continuous recovery process and device for high-purity MTBE |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103980096B (en) | 2016-02-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103980096B (en) | Extractive distillation with salt is separated the method for methyl tertiary butyl ether and methylene dichloride | |
| CN103709124B (en) | A kind of method of producing epoxy chloropropane | |
| CN106397363A (en) | Purifying method for 1,2-epoxybutane | |
| CN103449981A (en) | Azeotropic rectification device and method for separating propylene glycol monomethyl ether and water | |
| CN105016554A (en) | Semi-coke wastewater treatment process | |
| CN101898952A (en) | Method and device for treating low-concentration acetic acid wastewater | |
| CN101362692A (en) | Technology method for producing isopropyl trifluoroacetate and apparatus | |
| CN103827072A (en) | Method for recovering acetic acid | |
| CN105555772A (en) | Alkylene oxide separation systems, methods, and apparatuses | |
| CN103215058A (en) | Method for extracting and separating light component from coal tar at low temperature | |
| CN106008186B (en) | A kind of separation method of isopropanol, acetone and water mixed solution | |
| CN105348035A (en) | Method for integrated purification of chloroform and ethyl acetate mixed solution through azeotropic extractive distillation and liquid-liquid delamination | |
| CN103539663B (en) | Separating method of ethyl acetate and cyclohexane | |
| CN105218305A (en) | A kind of byproduct recovery process of synthetic gas preparing ethylene glycol | |
| CN102161008B (en) | Method for recovering catalyst in preparation of cyclohexene by partial hydrogenation of benzene | |
| CN205011671U (en) | Butyl's octanol apparatus for producing industrial waste uses multipurposely device | |
| CN106397365B (en) | 1,2- epoxy butane purification devices | |
| CN103772185A (en) | Device and method for removing moisture and heteroacids in acetic acid | |
| CN104557447B (en) | A kind of tetrafluoroethylene and R 1216 produce raffinate combined recovery Application way | |
| CN102911139A (en) | Recovery and separation method for solvent containing tetrahydrofuran-carbinol system | |
| RU2408569C2 (en) | Method of producing allyl alcohol | |
| CN101955410A (en) | Reclaim cinnamic method and system from containing cinnamic raw material | |
| CN204727810U (en) | A kind of purification and recover device for acetonitrile in ceftriaxone sodium synthesis | |
| CN106146374A (en) | A kind of method recycling cyclohexanone-oxime vapour phase rearrangement product fractionation weight residual liquid | |
| CN111362778B (en) | Gas-phase desorption separation process of glycerol distillate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160210 Termination date: 20170506 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |