CN107286003A - The process of polymethoxy dimethyl ether separation - Google Patents
The process of polymethoxy dimethyl ether separation Download PDFInfo
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- CN107286003A CN107286003A CN201610224010.2A CN201610224010A CN107286003A CN 107286003 A CN107286003 A CN 107286003A CN 201610224010 A CN201610224010 A CN 201610224010A CN 107286003 A CN107286003 A CN 107286003A
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- 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
The present invention relates to the process of polymethoxy dimethyl ether separation, mainly solve in the prior art while production separation 8 products of PODE3, the problem of can not removing thick PODE2 and DMM materials reclaimed water and methanol simultaneously, by using treating containing DMM, PODE2, PODE3 8, water and methanol, system of the refined material (1) including PODE2 crude towers (A), PODE2 knockout towers (B), PODE products tower (C), DMM and PODE2 high-pressure separation columns (D), low pressure methanol and water separation column (E) is separated the present invention；The operating pressure of the DMM and PODE2 high-pressure separation columns (D) higher than the low pressure methanol and water separation column (E) operating pressure, available for polymethoxy dimethyl ether separate and the recycling of unreacted product in.
Description
Technical field
The present invention relates to the process of polymethoxy dimethyl ether separation, more particularly to PODE3-8 points of polymethoxy dimethyl ether
The method recycled from process for purification and unreacted product DMM, accessory substance PODE2.
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.
Under petroleum resources increasingly situation in short supply, compared to coal through methanol-to-olefins and coal through roads such as synthesis gas preparing ethylene glycols
Line, coal base PODE synthesis is the New Coal Chemical route of a great application potential.Domestic relevant PODEnSynthesis
The research of technology in recent years also gradually carry out got up, Lanzhou Chemical Physics research institute of the Chinese Academy of Sciences, Shanghai Petroleum Chemical Engineering Institute,
Chinese Academy of Sciences's Shanxi coal chemical institute, East China University of Science etc. are to PODEnSynthesis carried out correlative study, and apply
A small amount of patent.From the point of view of open source literature report, the reaction scheme has begun to be paid close attention to by academia, but related base
Plinth or action oriented research are seldom, and there is catalyst activity is relatively low, regeneration is difficult, product selectivity is low, and technique is cumbersome etc.
Problem.
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 exists through PODE product knockout towers
35~60kPa operating pressure, obtain PODE separation column overhead contain PODE2, a small amount of water (1~3w%) and on a small quantity
The component of methanol (1~4w%) (also containing as little as negligible DMM sometimes) (is this hair after addition DMM
Refined material is treated described in bright), and PODE knockout towers tower reactor is containing the product component including n=3~6.For cost efficiency,
Need PODE2 the and/or DMM Returning reactors in PODE knockout tower overhead components proceeding reaction, still
PODE knockout tower overhead components reclaimed waters and methanol are unfavorable to the course of reaction, it is necessary to which water and methanol are removed.
W02006/045506A1 introduces BASF AG and replaces methanol using carbinol derivatives, utilizes dimethoxym ethane, metaformaldehyde
For the method for Material synthesis paraformaldehyde dimethyl ether, the series product of n=1~10 has been obtained, wherein：DMM accounts for 33.5%,
PODE2Account for 23.6%, effective additive component PODE3-8Less than 28.3%；The raw material dimethoxym ethane of the technique not largeization
Product, and by PODE2It is recycled to together in reactor as the solvent of unreacted material, with high costs, product yield is low,
It is unfavorable for industrialization generation.
The A of CN 104447221 (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 separation method in interior light component material including DMM, PODE2-7, water and methanol, and how to utilize not anti-
DMM and accessory substance PODE2 are answered, separation problem and qualified products PODE3-5 also without reference to water during its patent is disclosed
Separation problem.
The content of the invention
The present invention is to solve in the prior art during PODE3-8 product purifications when obtaining product PODE3-8, nothing
Method removes remaining thick PODE2 and DMM materials reclaimed water and methanol simultaneously, so as to can not ensure original PODE synthesis
Reaction is separated using high quality P ODE2 and DMM reuse material there is provided polymethoxy dimethyl ether and unreacted product is circulated
Application way, this method can remove the water and methanol in PODE2 and DMM simultaneously, it is ensured that PODE synthetic reactions
Use high quality P ODE2, DMM reuse material.
In order to solve the above technical problems, technical scheme is as follows：
The process of polymethoxy dimethyl ether separation, treating containing DMM, PODE2, PODE3-8, water and methanol refines
Raw material 1 is including PODE2 crude tower A, PODE2 knockout tower B, PODE product towers C, DMM and PODE2
High-pressure separation columns D, low pressure methanol and water separation column E system are separated；Step is as follows：
(a) it is described to treat that refined material 1 obtains tower top material 3 and base containing PODE2 in PODE2 crude tower A rectifying
This is free of DMM materials at bottom of tower 2；As non limiting example, PODE2 in the tower top material 3 containing PODE2
Content is 0.01~3%, preferably greater than 0.02 and less than 2% by weight；It is substantially free of in DMM materials at bottom of tower 2
DMM contents are 0~0.5% by weight；Preferably greater than 0 and less than 0.1%；
(b) step (a) materials at bottom of tower 2 is through the isolated tower top materials 5 of PODE2 knockout towers B and is essentially
PODE3-8 materials at bottom of tower 4；As non limiting example, PODE3-8 in the essentially PODE3-8 materials at bottom of tower 4
Content is 99~100%, preferably 99.5~100% by weight；
(c) step (a) and step (b) the tower top material 3 and 5 enter DMM and PODE2 high-pressure separation columns D,
Obtain tower top material and essentially DMM and PODE2 materials at bottom of tower 8；It is described to be essentially as non limiting example
In DMM and PODE2 materials at bottom of tower 8 DMM contents by weight for 20~80%, PODE2 contents by weight
For 10~60%；DMM contents by weight preferably 30~70%；PODE2 contents by weight preferably 20~50%；
(d) the tower top material that step (c) is obtained is through low pressure methanol and the isolated tower top materials of water separation column E and is essentially
The materials at bottom of tower 9 of first alcohol and water, obtained tower top material returns to DMM and PODE2 high-pressure separation columns D；It is used as non-limit
In property citing processed, the essentially materials at bottom of tower 9 of first alcohol and water by weight：Methanol content is 20~60%, water content
For 40~80%；It is preferred that methanol content is 20~50%, water content is 50~80%；More preferably methanol content is 30~40%,
Water content is 60~80%；
(e) materials at bottom of tower 4 that step (b) is obtained is separated through PODE product towers C, obtains essentially PODE3-4's
Overhead product material 7 and essentially PODE5-8 materials at bottom of tower 6；As non limiting example, the essentially PODE3-4
Product material 7 in PODE3-4 contents by weight be 99.5~100%, preferably 99.7~100%；Lifted as non-limiting
PODE5-8 contents are 99.6~100% by weight in example, the essentially PODE5-8 materials at bottom of tower 6, preferably
99.7~100%；
Behaviour of the operating pressure of the DMM and PODE2 high-pressure separation columns D higher than the low pressure methanol and water separation column E
Make pressure.
In above-mentioned technical proposal, preferably described DMM and PODE2 high-pressure separation columns D operating pressure is at least 470kPa；
The operating pressure more high effect of the DMM and PODE2 high-pressure separation columns D is better, but in view of equipment material and operation
Difficulty, preferably 470~700kPa.
In above-mentioned technical proposal, the operating pressure of preferably described low pressure methanol and water separation column E is below 200kPa；The pressure
The more poorly efficient fruit of power is better, but low pressure, which is operated, increases equipment investment if reaching negative pressure, therefore it is preferred that 100~200kPa.
In above-mentioned technical proposal, preferably described PODE2 crude towers A operating pressure is 85-115kPa, tower top operation temperature
Spend for 55-65 DEG C, tower reactor operation temperature is 110-140 DEG C.
In above-mentioned technical proposal, PODE2 knockout towers B operating pressure is 30-50kPa, and tower top operation temperature is 70-90 DEG C,
Tower reactor operation temperature is 125-150 DEG C.
In above-mentioned technical proposal, preferably PODE products tower C operating pressure is 35-55kPa, and tower top operation temperature is
140-160 DEG C, tower reactor operation temperature is 200-240 DEG C.
In above-mentioned technical proposal, preferably described DMM and PODE2 high-pressure separation columns D tower top operation temperature is
85-120 DEG C, tower reactor operation temperature is 90-140 DEG C.
In above-mentioned technical proposal, the tower top operation temperature of preferably described low pressure methanol and water separation column E is 38-50 DEG C, tower reactor
Operation temperature is 55-80 DEG C.
DMM the and PODE2 high-pressure separation columns D and the low pressure methanol and water separation column E height press-fit operations can
With methanol removal and water in the thick materials of DMM and PODE2.
When impurity level metaformaldehyde is contained in refined material 1, the PODE2 crude tower A rectifying through step (a) enters tower
Substrate material 2 and tower top material 3, the PODE2 knockout towers B through step (b) are segregated into tower top material 5, through step (c)
DMM and PODE2 high-pressure separation columns D be segregated into materials at bottom of tower 8, can be returned together with PODE2 and DMM thereafter
Return PODE synthesis procedure.
Using technical scheme, can with isolated qualified PODE3-8, and can reduce simultaneously PODE2 and
DMM returns to the content of first alcohol and water in material.Under the process conditions of the specific embodiment of the invention, it is qualified to can obtain
The requirement of PODE3-8 products and return material PODE2 and DMM to first alcohol and water, achieves effective technical result,
Available in the refined production of PODE products.
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 refined material for the treatment of containing DMM, PODE2, PODE3-8, water and methanol, and 2 be that PODE2 is thick
Tower A is divided to be substantially free of DMM materials at bottom of tower, 3 be that PODE2 crude tower A rectifying obtains the tower top containing PODE2
Material, 4 be that 5 be through PODE2 through essentially PODE3-8 materials at bottom of tower isolated PODE2 knockout towers B
The isolated tower top materials of knockout tower B, 6 be through essentially PODE5-8 bottom of towe isolated PODE product towers C
Material, 7 be that 8 be DMM and PODE2 through essentially PODE3-4 product material isolated PODE product towers C
Essentially PODE2 and DMM materials at bottom of tower isolated high-pressure separation columns D, 9 be low pressure methanol and water separation column
The materials at bottom of tower of essentially first alcohol and water isolated E.
A is PODE2 crude towers, and B is PODE2 knockout towers, and C is PODE product towers, and D is DMM and PODE2
High-pressure separation columns, E is low pressure methanol and water separation column.
Embodiment
【Embodiment 1】
Operated according to the flow shown in Fig. 1, step is as follows：
(a) it is described to treat that refined material 1 obtains tower top material 3 and base containing PODE2 in PODE2 crude tower A rectifying
This is free of DMM materials at bottom of tower 2；
(b) step (a) materials at bottom of tower 2 is through the isolated tower top materials 5 of PODE2 knockout towers B and is essentially
PODE3-8 materials at bottom of tower 4；
(c) step (a) and step (b) the tower top material 3 enter DMM and PODE2 high pressures with tower top material 5
Knockout tower D, obtains tower top material and essentially DMM and PODE2 materials at bottom of tower 8；
(d) the tower top material that step (c) is obtained is through low pressure methanol and the isolated tower top materials of water separation column E and is essentially
The materials at bottom of tower 9 of first alcohol and water, obtained tower top material returns to DMM and PODE2 high-pressure separation columns D；
(e) materials at bottom of tower 4 that step (b) is obtained is separated through PODE product towers C, obtains essentially PODE3-4's
Product material 7 and essentially PODE5-8 materials at bottom of tower 6；
The operating pressure of the PODE2 crude towers A is 110kPa, and tower top operation temperature is 57 DEG C, and tower reactor operation temperature is
119℃；PODE2 knockout towers B operating pressure is 50kPa, and tower top operation temperature is 84 DEG C, and tower reactor operation temperature is
144℃；PODE product towers C operating pressure is 55kPa, and tower top operation temperature is 157 DEG C, and tower reactor operation temperature is
228℃；DMM and PODE2 high-pressure separation columns D operating pressure is 700kPa, and tower top operation temperature is 109 DEG C, tower
Kettle operation temperature is 124 DEG C；Low pressure methanol and water separation column E operating pressure are 102kPa, and tower top operation temperature is 42 DEG C,
Tower reactor operation temperature is 69 DEG C.
Feed composition and separating effect are shown in Tables 1 and 2 in embodiment 1.In routine operation, the PODE2 typically to return
In methanol content be limited in less than 2%, and water is below 1%.By Tables 1 and 2 it can be found that returning to material PODE2
With almost there is no first alcohol and water in DMM, while using the present invention obtained qualified PODE3-8 products.It can be seen that with originally
Inventive method, fullys meet the separation requirement needed for system, and its is with the obvious advantage.
【Embodiment 2】
Operated according to the flow shown in Fig. 1, step is as follows：
(a) it is described to treat that refined material 1 obtains tower top material 3 and base containing PODE2 in PODE2 crude tower A rectifying
This is free of DMM materials at bottom of tower 2；
(b) step (a) materials at bottom of tower 2 is through the isolated tower top materials 5 of PODE2 knockout towers B and is essentially
PODE3-8 materials at bottom of tower 4；
(c) step (a) and step (b) the tower top material 3 enter DMM and PODE2 high pressures with tower top material 5
Knockout tower D, obtains tower top material and essentially DMM and PODE2 materials at bottom of tower 8；
(d) the tower top material that step (c) is obtained is through low pressure methanol and the isolated tower top materials of water separation column E and is essentially
The materials at bottom of tower 9 of first alcohol and water, obtained tower top material returns to DMM and PODE2 high-pressure separation columns D；
(e) materials at bottom of tower 4 that step (b) is obtained is separated through PODE product towers C, obtains essentially PODE3-4's
Product material 7 and essentially PODE5-8 materials at bottom of tower 6；
The operating pressure of the PODE2 crude towers A is 110kPa, and tower top operation temperature is 63 DEG C, and tower reactor operation temperature is
121℃；PODE2 knockout towers B operating pressure is 50kPa, and tower top operation temperature is 85 DEG C, and tower reactor operation temperature is
144℃；PODE product towers C operating pressure is 55kPa, and tower top operation temperature is 157 DEG C, and tower reactor operation temperature is
228℃；DMM and PODE2 high-pressure separation columns D operating pressure is 700kPa, and tower top operation temperature is 109 DEG C, tower
Kettle operation temperature is 124 DEG C；Low pressure methanol and water separation column E operating pressure are 102kPa, and tower top operation temperature is 42 DEG C,
Tower reactor operation temperature is 69 DEG C.
Feed composition and separating effect are shown in Table 3 and table 4 in embodiment 2.In routine operation, the PODE2 typically to return
In methanol content be limited in less than 2%, and water is below 1%.By table 3 and table 4 it can be found that returning to material PODE2
In almost there is no first alcohol and water, the DMM of return does not contain methanol, at the same using the present invention obtained qualified PODE3-4
Product.It can be seen that use the inventive method, fullys meet the separation requirement needed for system, its is with the obvious advantage.
【Comparative example 1】
Operated according to the flow shown in Fig. 1, step is as follows：
(a) it is described to treat that refined material 1 obtains tower top material 3 and base containing PODE2 in PODE2 crude tower A rectifying
This is free of DMM materials at bottom of tower 2；
(b) step (a) materials at bottom of tower 2 is through the isolated tower top materials 5 of PODE2 knockout towers B and is essentially
PODE3-8 materials at bottom of tower 4；
(c) step (a) and step (b) the tower top material 3 enter DMM and PODE2 high pressures with tower top material 5
Knockout tower D, obtains tower top material and essentially DMM and PODE2 materials at bottom of tower 8；
(d) the tower top material that step (c) is obtained is through low pressure methanol and the isolated tower top materials of water separation column E and is essentially
The materials at bottom of tower 9 of first alcohol and water, obtained tower top material returns to DMM and PODE2 high-pressure separation columns D；
(e) materials at bottom of tower 4 that step (b) is obtained is separated through PODE product towers C, obtains essentially PODE3-4's
Product material 7 and essentially PODE5-8 materials at bottom of tower 6；
The operating pressure of the PODE2 crude towers A is 110kPa, and tower top operation temperature is 63 DEG C, and tower reactor operation temperature is
121℃；PODE2 knockout towers B operating pressure is 50kPa, and tower top operation temperature is 85 DEG C, and tower reactor operation temperature is
144℃；PODE product towers C operating pressure is 55kPa, and tower top operation temperature is 157 DEG C, and tower reactor operation temperature is
228℃；DMM and PODE2 high-pressure separation columns D operating pressure is 450kPa, and tower top operation temperature is 99 DEG C, tower
Kettle operation temperature is 110 DEG C；Low pressure methanol and water separation column E operating pressure are 102kPa, and tower top operation temperature is 42 DEG C,
Tower reactor operation temperature is 69 DEG C.
The feed composition and separating effect fed in comparative example 1 is shown in Table 5 and table 6.In routine operation, typically to return
Methanol content in PODE2, DMM is limited in less than 2%, and water is below 1%.By table 5 and table 6 it can be found that
Because the high pressure due to DMM and PODE2 high-pressure separation columns D only has 450kPa, cause and follow-up low pressure methanol and water
Methanol content is higher in PODE2 and DMM that knockout tower E joint operations are returned, it is impossible to meets and returns to material PODE2
With the requirement in DMM to methanol content, it is impossible to recycle DMM, so must be in strict accordance with requirement pair of the invention
Each tower operation, the technique required based on invention and condition requirement can reach the separation requirement needed for system.
【Comparative example 2】
Operated according to the flow shown in Fig. 1, step is as follows：
(a) it is described to treat that refined material 1 obtains tower top material 3 and base containing PODE2 in PODE2 crude tower A rectifying
This is free of DMM materials at bottom of tower 2；
(b) step (a) materials at bottom of tower 2 is through the isolated tower top materials 5 of PODE2 knockout towers B and is essentially
PODE3-8 materials at bottom of tower 4；
(c) step (a) and step (b) the tower top material 3 enter DMM and PODE2 high pressures with tower top material 5
Knockout tower D, obtains tower top material and essentially DMM and PODE2 materials at bottom of tower 8；
(d) the tower top material that step (c) is obtained is through low pressure methanol and the isolated tower top materials of water separation column E and is essentially
The materials at bottom of tower 9 of first alcohol and water, obtained tower top material returns to DMM and PODE2 high-pressure separation columns D；
(e) materials at bottom of tower 4 that step (b) is obtained is separated through PODE product towers C, obtains essentially PODE3-4's
Product material 7 and essentially PODE5-8 materials at bottom of tower 6；
The operating pressure of the PODE2 crude towers A is 110kPa, and tower top operation temperature is 57 DEG C, and tower reactor operation temperature is
119℃；PODE2 knockout towers B operating pressure is 50kPa, and tower top operation temperature is 84 DEG C, and tower reactor operation temperature is
144℃；PODE product towers C operating pressure is 55kPa, and tower top operation temperature is 157 DEG C, and tower reactor operation temperature is
228℃；DMM and PODE2 high-pressure separation columns D operating pressure is 700kPa, and tower top operation temperature is 109 DEG C, tower
Kettle operation temperature is 124 DEG C；Low pressure methanol and water separation column E operating pressure are 220kPa, and tower top operation temperature is 55 DEG C,
Tower reactor operation temperature is 76 DEG C.
The feed composition and separating effect fed in comparative example 2 is shown in Table 7 and table 8.In routine operation, typically to return
Methanol content in PODE2, DMM is limited in less than 2%, and water is below 1%.By table 7 and table 8 it can be found that
, can not be with follow-up DMM and PODE2 high-pressure separation columns because the high pressure of low pressure methanol and water separation column E only has 220kPa
D joint operations so that methanol content is higher in the PODE2 and DMM of return, it is impossible to meet and return to material PODE2
With the requirement in DMM to methanol content, it is impossible to recycle DMM and PODE2, so must be in strict accordance with this hair
Bright requirement is operated to each tower, and technique and the condition requirement required based on invention can reach the separation requirement needed for system.
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
Claims (8)
1. the process of polymethoxy dimethyl ether separation, essence is treated containing DMM, PODE2, PODE3-8, water and methanol
Raw material (1) processed including PODE2 crude towers (A), PODE2 knockout towers (B), PODE products tower (C), DMM and
The system of PODE2 high-pressure separation columns (D), low pressure methanol and water separation column (E) is separated, and step is as follows：
(a) it is described to treat that refined material (1) obtains the tower top material (3) containing PODE2 in PODE2 crude towers (A) rectifying
With the materials at bottom of tower (2) for being substantially free of DMM；
(b) step (a) materials at bottom of tower (2) is through the isolated tower top material (5) of PODE2 knockout towers (B) and base
This is PODE3-8 materials at bottom of tower (4)；
(c) step (a) and step (b) the tower top material (3,5) enter DMM and PODE2 high-pressure separation columns
(D) tower top material and essentially DMM and PODE2 materials at bottom of tower (8), are obtained；
(d) the tower top material that step (c) is obtained is through low pressure methanol and the isolated tower top material of water separation column (E) and base
This is the materials at bottom of tower (9) of first alcohol and water, and obtained tower top material returns to DMM and PODE2 high-pressure separation columns (D)；
(e) materials at bottom of tower (4) that step (b) is obtained is separated through PODE products tower (C), obtains essentially PODE3-4
Overhead product material (7) and essentially PODE5-8 materials at bottom of tower (6)；
The operating pressure of the DMM and PODE2 high-pressure separation columns (D) is higher than the low pressure methanol and water separation column (E)
Operating pressure.
2. according to the method described in claim 1, it is characterized in that the behaviour of the DMM and PODE2 high-pressure separation columns (D)
Make pressure at least 470kPa.
3. according to the method described in claim 1, it is characterized in that the operating pressure of the low pressure methanol and water separation column (E)
For below 200kPa.
4. according to the method described in claim 1, it is characterized in that the operating pressure of PODE2 crude towers (A) is 85-115kPa,
Tower top operation temperature is 55-65 DEG C, and tower reactor operation temperature is 110-140 DEG C.
5. according to the method described in claim 1, it is characterized in that the operating pressure of PODE2 knockout towers (B) is 30-50kPa,
Tower top operation temperature is 70-90 DEG C, and tower reactor operation temperature is 125-150 DEG C.
6. according to the method described in claim 1, it is characterized in that the operating pressure of PODE products tower (C) is 35-55kPa,
Tower top operation temperature is 140-160 DEG C, and tower reactor operation temperature is 200-240 DEG C.
7. according to the method described in claim 1, it is characterized in that the tower of the DMM and PODE2 high-pressure separation columns (D)
It is 85-120 DEG C to push up operation temperature, and tower reactor operation temperature is 90-140 DEG C.
8. according to the method described in claim 1, it is characterized in that the tower top operation temperature of low pressure methanol and water separation column (E) is
38-50 DEG C, tower reactor operation temperature is 55-80 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610224010.2A CN107286003B (en) | 2016-04-12 | 2016-04-12 | Technological process for separating polymethoxy dimethyl ether |
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| CN201610224010.2A CN107286003B (en) | 2016-04-12 | 2016-04-12 | Technological process for separating polymethoxy dimethyl ether |
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| CN107286003B CN107286003B (en) | 2020-06-09 |
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| CN107935825A (en) * | 2017-12-28 | 2018-04-20 | 四川鑫达新能源科技有限公司 | Polymethoxy dimethyl ether refining spearation system and the method that polymethoxy dimethyl ether is prepared using the system |
| CN108218678A (en) * | 2018-01-31 | 2018-06-29 | 北京东方红升新能源应用技术研究院有限公司 | The separation and refining method and device of polymethoxy dimethyl ether |
| CN108358762A (en) * | 2018-01-31 | 2018-08-03 | 天津大学 | The Pyatyi separation method and device of polymethoxy dimethyl ether |
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| WO2006045506A1 (en) * | 2004-10-25 | 2006-05-04 | Basf Aktiengesellschaft | Method for producing polyoxymethylene dimethyl ethers |
| CN104230685A (en) * | 2013-06-17 | 2014-12-24 | 中国石油化工股份有限公司 | Process for producing polyoxymethylene dimethyl ether from methanol and paraformaldehyde |
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| WO2006045506A1 (en) * | 2004-10-25 | 2006-05-04 | Basf Aktiengesellschaft | Method for producing polyoxymethylene dimethyl ethers |
| CN104230685A (en) * | 2013-06-17 | 2014-12-24 | 中国石油化工股份有限公司 | Process for producing polyoxymethylene dimethyl ether from methanol and paraformaldehyde |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935825A (en) * | 2017-12-28 | 2018-04-20 | 四川鑫达新能源科技有限公司 | Polymethoxy dimethyl ether refining spearation system and the method that polymethoxy dimethyl ether is prepared using the system |
| CN108218678A (en) * | 2018-01-31 | 2018-06-29 | 北京东方红升新能源应用技术研究院有限公司 | The separation and refining method and device of polymethoxy dimethyl ether |
| CN108358762A (en) * | 2018-01-31 | 2018-08-03 | 天津大学 | The Pyatyi separation method and device of polymethoxy dimethyl ether |
| CN108218678B (en) * | 2018-01-31 | 2021-01-15 | 北京东方红升新能源应用技术研究院有限公司 | Method and device for separating and refining polymethoxy dimethyl ether |
| CN108358762B (en) * | 2018-01-31 | 2021-03-30 | 天津大学 | Five-stage separation method and device of polymethoxy dimethyl ether |
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| CN107286003B (en) | 2020-06-09 |
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