CN107286002A - The process for purification of polymethoxy dimethyl ether 2 - Google Patents
The process for purification of polymethoxy dimethyl ether 2 Download PDFInfo
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- CN107286002A CN107286002A CN201610223987.2A CN201610223987A CN107286002A CN 107286002 A CN107286002 A CN 107286002A CN 201610223987 A CN201610223987 A CN 201610223987A CN 107286002 A CN107286002 A CN 107286002A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/58—Separation; Purification; Stabilisation; Use of additives
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Abstract
Technical solution of the present invention is as follows：The process for purification of polymethoxy dimethyl ether 2, comprises the following steps：(a) following steps (a1) or (a2) are selected from；(a1) it will treat that refined material, in PODE2 knockout tower rectifying, obtains tower top material and essentially PODE2 materials at bottom of tower；It is described to treat that refined material is the thick materials of PODE2；(a2) it will treat that refined material, in PODE2 knockout tower rectifying, obtains tower top material and essentially PODE2 and DMM materials at bottom of tower；It is described to treat the DMM materials that refined material contains the thick materials of the PODE2 and introduced；(b) the tower top material that step (a) is obtained enters methanol/water rectifying column；Methanol/water rectifying column obtains tower top material and the essentially materials at bottom of tower of the low-pressure distillation heavy constituent of first alcohol and water through lock out operation；(c) the tower top material that step (b) is obtained returns to PODE2 knockout towers；The thick materials of PODE2 contain PODE2, water and methanol.
Description
Technical field
The present invention relates to the process for purification of polymethoxy dimethyl ether 2.
Background technology
Polyoxymethylene dimethyl ethers (PODE) are the common names of a class material, and its skeleton symbol can be expressed as CH3O(CH2O)nCH3。
PODE has higher oxygen content (42-51%) and Cetane number (more than 30), can improve diesel oil in engine
In combustion position, the thermal efficiency is improved, while reducing solid pollutant, COx and NOx discharge.It is reported that addition
5-30% CH3OCH2OCH3NOx emission 7-10%, PM reduction 5-35% can be reduced.Thus PODE is considered as
A kind of novel carbinol derivative that can be used for diesel oil mediation of great application prospect.
PODE can be synthesized by methanol and formaldehyde by acid-catalyzed dehydration.Industrially closed by coal gasification preparing synthetic gas, by synthesis gas
It has been the route of comparative maturity into methanol and by methanol oxidative synthesis formaldehyde.Additions of the PODE in diesel oil can be very high
(up to 30%), addition PODE can not only replace part diesel oil, moreover it is possible to improve the efficiency of combustion and discharge performance of diesel oil.
In terms of 1.16 hundred million tons of China's diesel oil consumption figure in 2006, if the diesel oil for having 30% is replaced by PODE, China's oil is entered
Mouth interdependency can reduce by 34,000,000 tons, and this is a considerable numeral.Therefore, PODE synthesis is studied, it is right
Alleviate the environmental protection pressure of China, the exploitation to coal resources, and then national energy security is of great importance.
PODE discovery is more early, but just starts to cause the interest of expert and scholar in recent years.Current mainly BP in the world,
Synthesis of the companies such as BASF to PODE has carried out correlative study, and has applied for a small amount of patent.And come from open source literature report
See, the reaction scheme is not yet paid close attention to by abroad academia, related basis or action oriented research are seldom, also do not see
To the report of industrialization.Under petroleum resources increasingly situation in short supply, compared to coal through methanol-to-olefins and coal through synthesis gas
The routes such as preparing ethylene glycol, coal base PODE synthesis is the New Coal Chemical route of a great application potential.
Domestic relevant PODEnSynthetic technology research in recent years also gradually carry out got up, Chinese Academy of Sciences's Lanzhou Chemical Physics
Research institute, Shanghai Petroleum Chemical Engineering Institute, Chinese Academy of Sciences's Shanxi coal chemical institute, East China University of Science etc. are to PODEn
Synthesis carried out correlative study, and applied for a small amount of patent.From the point of view of open source literature report, the reaction scheme has begun to
Paid close attention to by academia, but related basis or action oriented research are seldom, and have that catalyst activity is relatively low, regeneration is tired
Difficult, product selectivity is low, the problems such as technique is cumbersome.
Ten thousand tons of report only Shandong (Heze) Chen Xin New Energy Corporation and orchidization institute of the Chinese Academy of Sciences Cooperative construction of industrialization are seen at present
Level PODEnDevice, its hundred ton unit completed pilot plant test in 2012 in Baiyin Pilot Base.This technology
Using methanol as raw material, using ionic liquid as catalyst, PODE is synthesized through metaformaldehyden.Its correlative study be concentrated mainly on
Ionic liquid is the homogeneous reaction system of catalyst, and the process haves the shortcomings that homogeneous catalytic reaction is intrinsic, such as ionic liquid
Catalyst is expensive, the problems such as being difficult to be kept completely separate with product during recycling.
Due in synthesis PODEn, n=1-6 each component can be generated.When n value is 1, polymethoxy two
Methyl ether is dimethoxym ethane (DMM), although the use of dimethoxym ethane as vehicle fuel addition group component can be raising energy utilization rate,
Exhaust emissions is reduced, but can still arrive causes vapour lock.Polymethoxy dimethyl ether (namely poly- first when n value is 2
Aldehyde dimethyl ether 2 or abbreviation PODE2) flash-point it is too low, be unfavorable for compression-ignition, so conventional in use is n=3-6
Component.
Synthesis and separation on PODE reported in the patent earliest, but until in recent years, due to oil price increasingly
It is surging and environmental protection requirement increasingly strictly just gradually to cause concern.It can be seen that from the international monopoly applied
The patent applied after 1998 accounts for the overwhelming majority.Most of patent is to obtain PODE by methanol and formaldehyde dehydration, but
It is that the presence of system reclaimed water can improve separating energy consumption, causes reaction intermediate hemiacetal to occur hydrolysis, reduces PODE
The yield of product.
In the presence of acidic, using dimethoxym ethane and metaformaldehyde (and/or paraformaldehyde) as raw material, PODE is produced,
Reaction product, first pass around DMM knockout towers 100~150kPa operating pressure, 90~120 DEG C of bottom temperature and
40~50 DEG C of tower top temperature by reaction product be separated into the overhead components containing DMM and containing n be more than wait 2 PODE, lack
The DMM tower kettle materials of water, a small amount of methanol and a small amount of metaformaldehyde are measured, DMM towers kettle material is through PODE product knockout towers
35~60kPa operating pressure, obtain PODE separation column overhead contain PODE2, a small amount of water (1~3%) (w)
With the thick materials of component-PODE2 of a small amount of methanol (1~4%) (w) (also containing as little as negligible DMM sometimes)
(being of the present invention to treat refined material after addition DMM), and PODE knockout towers tower reactor is containing the production including n=3~6
Product component.Reacted for cost efficiency, it is necessary to which the PODE2 in PODE knockout tower overhead components and/or DMM is returned
Device proceed reaction, but PODE knockout tower overhead components reclaimed waters and methanol it is unfavorable to the course of reaction, it is necessary to water with
Methanol is removed.
CN 104447221A (process for purification of polyoxymethylene dimethyl ethers) are specifically disclosed using hexamethylene, n-hexane, first
Sour methyl esters, ethyl acetate, methyl propionate or normal heptane are the method that azeotropic solvent removes methanol in PODE2.But do not have
Body discloses the method for removing water in interior light component material including DMM, PODE2, water and methanol.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of process for purification of new polymethoxy dimethyl ether 2, this method has
Can be while the advantage of methanol removal and water.
In order to solve the above technical problems, technical scheme is as follows：The process for purification of polymethoxy dimethyl ether 2, including
Following steps：
(a) following steps (a1) or (a2) are selected from:
(a1) refined material will be treated in PODE2 knockout tower A rectifying, tower top material 7 and essentially PODE2 is obtained
Materials at bottom of tower 3；It is described to treat that refined material is the thick materials 1 of PODE2；
(a2) refined material will be treated in PODE2 knockout tower A rectifying, obtain tower top material 7 and essentially PODE2 and
DMM materials at bottom of tower 3；It is described to treat the DMM materials 2 that refined material contains the thick materials 1 of the PODE2 and introduced；
As non limiting example, PODE2 materials at bottom of tower and DMM bottom of towe are essentially wherein described in step (a)
Material is by weight：PODE2 contents 70~100%, DMM contents are 5~40%；It is preferred that PODE2 contents 75~100%,
DMM contents are 10~30%；More preferably PODE2 contents 80~100%, DMM contents are 10~20%.
(b) the tower top material 7 that step (a) is obtained enters methanol/water rectifying column B；Methanol/water rectifying column B is grasped through separation
Obtain tower top material 6 and the essentially materials at bottom of tower 4 and 5 of the low-pressure distillation heavy constituent of first alcohol and water；As non-limiting
In citing, the essentially low-pressure distillation heavy constituent 4 of first alcohol and water by weight：Methanol content is 20~80%, and water contains
Measure as 20~80；It is preferred that methanol content is 30~70%, water content is 30~70%；More preferably methanol content is 40~60%,
Water content is 40~60%；
(c) the tower top material 6 that step (b) is obtained returns to PODE2 knockout towers A；
The thick materials 1 of PODE2 contain PODE2, water and methanol；The operating pressure of the PODE2 knockout towers A is higher than
The operating pressure of the methanol/water rectifying column B.Using the program, PODE2 materials reclaimed water and the content of methanol can be reduced.
In above-mentioned technical proposal, preferably described PODE2 knockout towers A operating pressure is at least 450kPa.For removing PODE2
Water in thick material, the operating pressure more high effect of the PODE2 knockout towers A is better, but in view of equipment material and behaviour
Make difficulty, preferably 450~700kPa.
In above-mentioned technical proposal, preferably methanol/water rectifying column B operating pressure is below 200kPa.The lower DMM of the pressure
Material and water and separating methanol effect are better, but low pressure, which is operated, increases equipment investment if reaching negative pressure, therefore it is preferred that
100~200kPa.
, can be on the basis of simple high-pressure rectification further using the operation and the operation of low-pressure distillation of above-mentioned high-pressure rectification
PODE2 materials reclaimed water and methanol are removed, while DMM process losses can also be reduced.
In above-mentioned technical proposal, the following component for treating refined material preferably containing PODE2 and in terms of weight/mass percentage composition：
H2O 1~4%；H2O is more preferably 1.3~4%；
Methanol 0.7~3%；
DMM, 0~40%.It is preferred that DMM, which is more than 0, DMM contents, can be such as, but not limited to 5%, 10%, 20%,
30% etc..DMM contents are higher, removing water and methanol it is more thorough, but DMM contents it is high when high energy consumption, consider example
10~30% can such as be selected.
In above-mentioned technical proposal, DMM materials 2 are described after being mixed to get with the thick materials of above-mentioned PODE2 1 to be waited to refine
Raw material, enters back into PODE2 knockout tower A, can respectively enter PODE2 with DMM materials 2 and the thick materials 1 of PODE2
Knockout tower A original positions, which are mixed to get, treats refined material.
In above-mentioned technical proposal, the theoretical cam curve of the PODE2 knockout towers A is preferably 20-60, and reflux ratio is preferably
1.5-8, tower top operation temperature is preferably 90-96 DEG C, and tower reactor operation temperature is preferably 150-170 DEG C.
In above-mentioned technical proposal, the theoretical cam curve of the methanol/water rectifying column B is preferably 15-70, and reflux ratio is preferably 1-6,
Tower top operation temperature is preferably 37-58 DEG C, and tower reactor operation temperature is preferably 80-110 DEG C.
In above-mentioned technical proposal, the tower top material of the PODE2 knockout towers A is preferably that the methanol/water rectifying column B is provided
Thermic load.Now, using the temperature difference between the tower of high-low pressure two, energy Integrated design has effectively been carried out, system energy is reduced
Consumption and operating cost.More preferably at least a portion materials at bottom of tower 5 of step (b) adds through PODE2 knockout tower A heat exchangers
Heat returns to methanol/water rectifying column B；
In above-mentioned technical proposal, described rectifying column is including described at least one described PODE2 knockout towers A and at least one
Methanol/water rectifying column B, as long as can realize high-pressure rectification with low-pressure distillation compounding practice in the scope of the present invention.
Using technical scheme, the content of first alcohol and water in PODE2 materials can be reduced simultaneously, in present invention tool
Under the process conditions of body embodiment, can whole methanol removals and water, beneficial technique effect is achieved, available for PODE2
Refined production in.
Below in conjunction with the accompanying drawings, by embodiment, the present invention will be further described.
Brief description of the drawings
Fig. 1 is a kind of schematic flow sheet of embodiment of the invention.
In Fig. 1：1 is the thick material chargings of PODE2, and 2 be the charging of DMM materials, and 3 be essentially PODE2 and DMM
High-pressure rectification heavy constituent, 4 be the alcohol and water containing first low-pressure distillation heavy constituent, 5 for PODE2 knockout towers A tower top it is cold
Condenser provides the material of thermic load for methanol/water rectifying column B, and 6 return to separation for methanol/water rectifying column B overhead
Tower A material, 7 be high pressure PODE2 knockout tower A rectifying light components.
A is PODE2 knockout towers, and B is methanol/water rectifying column, and C is PODE2 knockout tower condensers, and D is methanol/water
Rectifying column condenser, E is PODE2 knockout tower reboilers.
Embodiment
【Embodiment 1】
Operated according to the flow shown in Fig. 1, wherein PODE2 knockout towers are isolated containing polymethoxy dimethyl ether and DMM
Heavy constituent, return original system participate in reaction, it is miscellaneous that overhead isolates methanol and water etc. into methanol/water rectifying column B
Matter.For treating refined material containing DMM, PODE2, water and methanol, contained through PODE2 knockout tower high-pressure rectifications
PODE2 and DMM high-pressure rectification heavy constituent, and the high-pressure rectification light component containing DMM, water and methanol；The PODE2
The operating pressure of knockout tower A high-pressure rectifications is 505kPa operating pressure；The PODE2 knockout towers A high-pressure rectifications are light
Component preferably further obtains the low-pressure distillation light component containing DMM through methanol/water rectifying column B low-pressure distillations, and containing methanol
With the low-pressure distillation heavy constituent of water；The operating pressure of methanol/water rectifying column B low-pressure distillations is 102kPa；It treats refined material
It is preferred that the constituent content containing PODE2 and in terms of weight/mass percentage composition is shown in Table 1；From two rectifying columns, gone here and there between rectifying column
Connection connection, the overhead of previous rectifying column enters next rectifying column, and it is respectively PODE2 knockout towers A and first
Alcohol/crystal evaporate tower B, the high-pressure rectification is carried out in PODE2 knockout towers A, described in methanol/water rectifying column B progress
Low-pressure distillation；The PODE2 materials of DMM materials and the alcohol and water containing first are mixed into after entering back into PODE2 point after refined material
From tower A high-pressure rectifications；Now PODE2 knockout towers A theoretical cam curve is 20, and reflux ratio is 2.5, tower top operation temperature
Spend for 94 DEG C, tower reactor operation temperature is 145 DEG C；Methanol/water rectifying column B theoretical cam curve is 20, and reflux ratio is 1.9,
Tower top operation temperature is 42 DEG C, and tower reactor operation temperature is 87 DEG C；Methanol/water rectifying column B in operation overhead is excellent
Choosing returns to PODE2 knockout towers A；PODE2 knockout towers A overhead condenser is preferably that methanol/water rectifying column B is carried simultaneously
Heating demand.
The feed composition and separating effect fed in embodiment 1 is shown in Tables 1 and 2.By Tables 1 and 2 it can be found that returning
Almost there is no first alcohol and water in material, in routine operation, 2% typically is limited in the methanol content in the PODE2 of return
Hereinafter, and water is below 1%.It can be seen that use the inventive method, fullys meet the separation requirement needed for system, its advantage is bright
It is aobvious.
【Comparative example 1】
Replace DMM with hexamethylene, using single-tower operation, i.e., with patent CN 104447221A (polyoxymethylene dimethyl ethers
Process for purification) operating condition it is similar.Now without material 6 is returned in Fig. 1, overhead is 7, and tower reactor discharging is 3,
Now the number of theoretical plate of tower is 20, and reflux ratio is 6.8, and operating pressure is 103kPa, and tower top temperature is 66 DEG C, bottom temperature
For 105 DEG C.Charging is shown in Table 3, can be seen that by the separating effect of table 3 and table 4, although first can be deviate from by adding entrainer
Alcohol, but fully effective can not be removed for the water contained in charging.
【Comparative example 2】
DMM is replaced with hexamethylene, still using single-tower operation, i.e., with A (the polyformaldehyde dimethyl of patent CN 104447221
The process for purification of ether) operating condition it is similar.Now without material 6 is returned in Fig. 1, overhead is 7, tower reactor discharging
For 3, now the number of theoretical plate of tower is 20, and reflux ratio is 6.8, and operating pressure is high pressure 505kPa, and tower top temperature is 105 DEG C,
Bottom temperature is 159 DEG C.Charging is shown in Table 5, can be seen that by the separating effect of table 5 and table 6, although adding entrainer can
To deviate from methanol, but for the water contained in charging be under operation with high pressure still can not it is fully effective deviate from.
【Comparative example 3】
DMM simply is replaced with hexamethylene, other on year-on-year basis, are operated with embodiment 1 using high-low pressure tower, specific as follows：
Operated according to the flow shown in Fig. 1, wherein PODE2 knockout towers isolate polymethoxy dimethyl ether, trimerization first
The heavy constituents such as aldehyde, return to original system and participate in reaction, overhead isolates methanol and water etc. into methanol/water rectifying column B
Impurity.For treating refined material containing DMM, PODE2, water and methanol, obtain containing PODE2 and DMM through high-pressure rectification
High-pressure rectification heavy constituent, and the high-pressure rectification light component containing DMM, water and methanol；The PODE2 knockout towers A is high
The operating pressure that the operating pressure for pressing rectifying is 505kPa；The theoretical cam curve of the PODE2 knockout towers A is 20, is returned
Stream is than being 0.2, and operating pressure is 505kPa；The high-pressure rectification light component is preferably further through methanol/water rectifying column B low pressure
Rectifying obtains the low-pressure distillation light component containing DMM, and the alcohol and water containing first low-pressure distillation heavy constituent；Methanol/water rectifying column B
Theoretical cam curve be 20, reflux ratio is 0.15, and operating pressure is 102kPa；It treats that refined material preferably contains PODE2
7 are shown in Table with the constituent content in terms of weight/mass percentage composition；From two rectifying columns, it is connected in series between rectifying column, it is previous
The overhead of rectifying column enters next rectifying column, and it is respectively PODE2 knockout towers A and methanol/water rectifying column B,
The high-pressure rectification is carried out in PODE2 knockout towers A, described low-pressure distillation is carried out in methanol/water rectifying column B；DMM
The PODE2 materials of material and the alcohol and water containing first are mixed into and state high pressure PODE2 knockout towers A after being entered back into after refined material；This
When state PODE2 knockout towers A tower top operation temperature be 91 DEG C, excellent 132 DEG C of tower reactor operation temperature；Methanol/water rectifying column B
Tower top operation temperature be 51 DEG C, tower reactor operation temperature be 106 DEG C；Methanol/water rectifying column B in operation tower top is distillated
Thing is preferably returned to PODE2 knockout towers A；PODE2 knockout towers A overhead condenser is preferably methanol/water rectifying column simultaneously
B provides thermic load.
The feed composition and separating effect fed in comparative example 1 is shown in Table 7 and table 8.It is can be found that by table 7 and table 8, although
Introduce entrainer to reclaim PODE2, be stripped of water therein, but the methanol content in the PODE2 of return is simultaneously
Do not reduce, conversely also raised, be not reaching in returned material to methanol content be less than 2% requirement, and
New impurity-entrainer is also introduced in the PODE2 of return, and in low pressure methanol/crystal evaporate tower B tower reactor distillate
Partially azeotropic agent is taken away, this is not to allow.
【Comparative example 4】
Consider that PODE2 knockout tower A pressure uses 450kPa, methanol/water rectifying column B pressure is 102kPa.Consider such as table
9 charging, now PODE2 knockout towers A separating effect will be deteriorated, and methanol/water rectifying column B due to high pressure PODE2
Knockout tower A connects, because high pressure PODE2 knockout towers A separation can not complete separation task and cause low pressure methanol/crystal
Separation task can not be completed by evaporating tower B, and the separating effect of PODE2 knockout tower A tower reactors is shown in Table 10 last row, it is seen that water
Many DMM, i.e. related DMM is have lost also in the PODE2 of return, and in the PODE2 returned not fill
Divide and utilize.It can be seen that being pressed with strict requirements to the PODE2 knockout towers A of high-low pressure tower tower, recommend 500KPa with enterprising
Row lock out operation.
【Embodiment 2】
Similar to Example 1, it is considered to another charging situation, it feeds concrete numerical value referring to table 11, high pressure PODE2
Knockout tower A number of theoretical plates are 20, and reflux ratio is 1.7, and operating pressure is 555kPa；The high pressure PODE2 knockout towers A
Rectifying light component preferably further obtains the low-pressure distillation light component containing DMM through low pressure methanol/crystal evaporate tower B rectifying, and
The low-pressure distillation heavy constituent of the alcohol and water containing first；Low pressure methanol/crystal evaporate tower B number of theoretical plates are also 20, and reflux ratio is 1.3,
Operating pressure is still 102kPa；It treats that constituent content of the refined material preferably containing PODE2 and in terms of weight/mass percentage composition is shown in Table
11；Still from two rectifying columns, it is connected in series between rectifying column, the overhead of previous rectifying column enters next essence
Tower is evaporated, it is respectively PODE2 knockout towers A and methanol/water rectifying column B, and the high pressure is carried out in PODE2 knockout towers A
Rectifying, described low-pressure distillation is carried out in methanol/water rectifying column B；The PODE2 materials of DMM materials and the alcohol and water containing first
It is mixed into after entering back into high pressure PODE2 knockout towers A after refined material；Now PODE2 knockout towers A tower top operation is warm
Spend for 98 DEG C, tower reactor operation temperature is 151 DEG C；Methanol/water rectifying column B tower top operation temperature is 42 DEG C, tower reactor operation
Temperature is 84 DEG C；Other associative operations are similar with embodiment 1.
Now the corresponding separating effect of system is as shown in table 11 and table 12, by table it can be found that being directed to from the inventive method
Different feed needs, in suitable opereating specification, can reach expected separating effect, meet PODE2 and return to raw material
It is required that.
In the data of the table of description of the invention, E represents that the numerical value behind × 10, E represents 10 corresponding power.
The quality of material of table 1 constitutes structure
The quality of material point rate composition structure of table 2
The quality of material of table 3 constitutes structure
The quality of material point rate composition structure of table 4
The quality of material of table 5 constitutes structure
The quality of material point rate composition structure of table 6
The quality of material of table 7 constitutes structure
The quality of material point rate composition structure of table 8
The quality of material of table 9 constitutes structure
The quality of material point rate composition structure of table 10
The quality of material of table 11 constitutes structure
The quality of material point rate composition structure of table 12
Claims (10)
1. the process for purification of polymethoxy dimethyl ether 2, comprises the following steps：
(a) following steps (a1) or (a2) are selected from:
(a1) it will treat that refined material, in PODE2 knockout towers (A) rectifying, obtains tower top material (7) and essentially PODE2
Materials at bottom of tower (3)；It is described to treat that refined material is the thick materials of PODE2 (1)；
(a2) it will treat that refined material, in PODE2 knockout towers (A) rectifying, obtains tower top material (7) and essentially PODE2
With DMM materials at bottom of tower (3)；It is described to treat the DMM that refined material contains the thick materials of the PODE2 (1) and introduced
Material (2)；
(b) the tower top material (7) that step (a) is obtained enters methanol/water rectifying column (B)；Methanol/water rectifying column (B)
Tower top material (6) and the essentially materials at bottom of tower (4,5) of the low-pressure distillation heavy constituent of first alcohol and water are obtained through lock out operation；
(c) the tower top material (6) that step (b) is obtained returns to PODE2 knockout towers (A)；
The thick materials of PODE2 (1) contain PODE2, water and methanol；The operation pressure of the PODE2 knockout towers (A)
Power is higher than the operating pressure of the methanol/water rectifying column (B).
2. process for purification according to claim 1, it is characterized in that the operating pressure of the PODE2 knockout towers (A)
At least 450kPa.
3. process for purification according to claim 2, it is characterized in that the operating pressure of the PODE2 knockout towers (A)
For 450~700kPa.
4. process for purification according to claim 1, it is characterized in that the operating pressure of methanol/water rectifying column (B) is 200kPa
Below.
5. process for purification according to claim 4, it is characterized in that the operating pressure of methanol/water rectifying column (B) is
100~200kPa.
6. process for purification according to claim 1, it is characterized in that described treat refined material containing PODE2 and with quality hundred
Divide the following component of content meter：
H2O 1~4%；
Methanol 0.7~3%；
DMM, 0~40%.
7. process for purification according to claim 1, it is characterized in that the theoretical tray of the PODE2 knockout towers (A)
Number is 20-60, and reflux ratio is 1.5-8, and tower top operation temperature is 90-96 DEG C, and tower reactor operation temperature is 150-170 DEG C.
8. process for purification according to claim 1, it is characterized in that the theoretical tray of the methanol/water rectifying column (B)
Number is 15-70, and reflux ratio is 1-6, and tower top operation temperature is 37-58 DEG C, and tower reactor operation temperature is 80-110 DEG C.
9. process for purification according to claim 1, it is characterized in that the tower top material of the PODE2 knockout towers (A)
Thermic load is provided for the methanol/water rectifying column (B).
10. process for purification according to claim 9, it is characterized in that at least a portion materials at bottom of tower (5) of step (b)
Methanol/water rectifying column (B) is returned through the heating of PODE2 knockout towers (A) heat exchanger.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111087286A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Method for refining polymethoxy dimethyl ether dimer |
| CN111087288A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Method for purifying dimeric methoxy dimethyl ether |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111087286A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Method for refining polymethoxy dimethyl ether dimer |
| CN111087288A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Method for purifying dimeric methoxy dimethyl ether |
| CN111087288B (en) * | 2018-10-23 | 2023-05-02 | 中国石油化工股份有限公司 | Purification method of dimeric methoxy dimethyl ether |
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