CN109776288A - A kind of separation method and device of polymethoxy dimethyl ether - Google Patents
A kind of separation method and device of polymethoxy dimethyl ether Download PDFInfo
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Abstract
It is methyl formate, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE in charging that the present invention relates to a kind of separation method of polymethoxy dimethyl ether and devices using multistage rectification2Mixed material rectifying column in introduce supplement water, formalin and metaformaldehyde realize the purpose of separating formaldehyde and metaformaldehyde from the tower bottom of rectifying tower or the extraction of subsequent tower bottom of rectifying tower.Formaldehyde will not polymerize blocking condenser and pipeline after technique separation, improve equipment using continuity, and can effectively recycle unreacted raw material formaldehyde, byproduct of reaction methyl formate and PODE2Deng.
Description
Technical field
The invention belongs to technical field of chemical engineering, it is related to synthesizing poly- first with formalin using multistage rectification separation methanol
The technology of the synthetic product mixture of oxygroup dimethyl ether, it is especially a kind of to feed as methyl formate, dimethoxym ethane, methanol, water, first
Aldehyde, metaformaldehyde and PODE2Mixed material rectifying column introduce supplement water realize polymethoxy dimethyl ether separation and purification
Method and apparatus.
Background technique
Polymethoxy dimethyl ether is a kind of novel diesel fuel additives, and chemical formula is expressed as CH3O(CH2O)nCH3(wherein n
Greatly >=1, general value is less than 10), oxygen content (42%~51%) with higher and Cetane number (being averagely up to 76),
In, PODE3-5It is optimal diesel fuel additives, PODE is added into diesel oil3-5Soot, the particulate matter of diesel engine can be effectively reduced
(PM) it discharges, improve fuel economy.PODEn is to be urged by the raw material of offer etherate end group and the raw material of offer methoxyl group in acid
The homologous components formed under change through polycondensation reaction.The compound for providing end group includes methanol, dimethyl ether and dimethoxym ethane etc., is provided
The compound of methoxyl group has formaldehyde, metaformaldehyde and paraformaldehyde etc..
For many years, the domestic and international research team based on BASF AG has carried out greatly the synthesis and separation process of PODEn
Quantifier elimination, the dimethoxym ethane for having BASF AG mainly reported and metaformaldehyde route (US 20070260094), Tsinghua University
It is anhydrous trimerization with the dimethoxym ethane of Jade Emperor chemical industry cooperation and paraformaldehyde route (CN104974025A) but due to its reaction raw materials
Formaldehyde and paraformaldehyde, reaction product composition is simple, and separating technology can not be suitable for methanol and the synthesis of formalin produces
The separation of object；In addition there are the methanol of BASF AG and formalin react and separation process (US 2008207954,
US20080221368, US 7671240, US 7700809), conversion per pass is low, and separation process is complicated, and material heats repeatedly
Separating energy consumption is big, and equipment seriously corroded strongly limits the industrialization of its process flow.
Summary of the invention
It is divided into two steps using methanol and formalin as the synthesis process of raw material PODEn, the first step is formaldehyde and methanol
Reaction generates the stage of reaction of dimethoxym ethane, and second step is that dimethoxym ethane reacts the stage of reaction for generating PODEn with formaldehyde.
It is methyl formate, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde that the purpose of the present invention is to provide one kind in charging
And PODE2Mixed material rectifying column introduce supplement water realize polymethoxy dimethyl ether separation and purification method and apparatus.
It uses distillating method separation using methanol and formalin as the synthetic product of raw material PODEn, is refining to obtain suitable diesel oil group
The PODEn divided, while recovery section raw material returns to above-mentioned first stage and second stage reaction process respectively.
One kind of the invention is methyl formate, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE in charging2Mixing
The rectifying column of material introduces the method and apparatus that supplement water realizes polymethoxy dimethyl ether separation and purification, can use six essences
Evaporate tower and a dewatering unit.
By taking 6 grades of rectifying as an example, technical solution is as follows:
(a) scheme 1 (as shown in Figure 1)
A kind of separator of polymethoxy dimethyl ether, including six rectifying columns and a dewatering unit, first rectifying column
The tower reactor outlet of 1-A connects the feed inlet of Second distillation column 1-B by pipeline, and the tower top outlet of first rectifying column 1-A passes through pipe
Line connects the feed inlet of third distillation column 1-C, and the tower top outlet of third distillation column 1-C connects the 4th rectifying column 1-D by pipeline
Feed inlet, the tower reactor discharge port of the 4th rectifying column 1-D connects the feed inlet of the 5th rectifying column 1-E, the 5th rectifying by pipeline
The tower reactor discharge port of tower 1-E connects the feed inlet of dewatering unit 1-F, the discharge port connection the 6th of dewatering unit 1-F by pipeline
The feed inlet of rectifying column 1-G.It supplements water and can discharge with the tower top of first rectifying column 1-A and enter third distillation column 1-C jointly, or
It is individually added into, if supplement water is individually added into, needs that supplement water feed inlet is additionally arranged on third distillation column 1-C.
PODEn raw material (1-1) enters first rectifying column (1-A), and first rectifying column (1-A) overhead extraction is essentially formic acid first
Ester, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (1-2)；First rectifying column (1-A) kettle material (1-
3) enter Second distillation column (1-B), Second distillation column (1-B) overhead extraction is essentially PODE3-5Material (1-4) and tower reactor base
This is PODE6-10Material (1-5)；First rectifying column (1-A) tower top material (1-2) enters third distillation column (1-C), while the
Three rectifying columns (1-C) introduce supplement water (1-6), and the extraction of third distillation column (1-C) tower reactor is essentially formalin and trimerization first
The material (1-8) of aldehyde；Third distillation column (1-C) tower top material (1-7) enters the 4th rectifying column (1-D), the 4th rectifying column (1-D)
Overhead extraction is essentially the material (1-9) of methyl formate；4th rectifying column (1-D) kettle material (1-10) enters the 5th rectifying column
(1-E), the 5th rectifying column (1-E) overhead extraction are essentially the material (1-11) of dimethoxym ethane and methanol；5th rectifying column (1-E) tower
Kettle material (1-12) enters dewatering unit (1-F), and moisture (1-13) is removed；Material (1-14) after removing water enters the 6th essence
It evaporates tower (1-G), overhead extraction is essentially the material (1-15) of methanol and tower reactor is essentially PODE2Material (1-16)；Wherein,
The operating pressure of one rectifying column (1-A) is 80-120KPa, and tower top operation temperature is 70-100 DEG C, the behaviour of Second distillation column (1-B)
Making pressure is 1-50KPa, and the operation temperature of tower top is 50-150 DEG C, and the operating pressure of third distillation column (1-C) is 80-
120KPa, tower top operation temperature are 70-120 DEG C, supplement mass ratio of water (1-6) content by weight with material (1-2) and are
0.2:1~1:1, the operating pressure of the 4th rectifying column (1-D) are 100-200KPa, and tower top operation temperature is 30-60 DEG C, the 5th essence
Evaporate tower (1-E) operating pressure be 100-200KPa, tower top operation temperature be 35-70 DEG C, dewatering unit (1-F) be film dehydration,
Molecular sieve dehydration, adsorption dewatering, the operating pressure of the 6th rectifying column (1-G) are 100-200KPa, and tower top operation temperature is 60-90
℃。
(b) scheme 2 (as shown in Figure 2)
A kind of separator of polymethoxy dimethyl ether, including six rectifying columns and a dewatering unit, first rectifying column
The tower reactor outlet of 2-A connects the feed inlet of Second distillation column 2-B by pipeline, and the tower top outlet of first rectifying column 2-A passes through pipe
Line connects the feed inlet of third distillation column 2-C, and the tower top outlet of third distillation column 2-C connects the 4th rectifying column 2-D by pipeline
Feed inlet, the tower top discharge port of the 4th rectifying column 2-D connects the feed inlet of the 5th rectifying column 2-E, the 4th rectifying by pipeline
The tower reactor discharge port of tower 2-D connects the feed inlet of dewatering unit 2-F, the discharge port connection the 6th of dewatering unit 2-F by pipeline
The feed inlet of rectifying column 2-G.It supplements water and can discharge with the tower top of first rectifying column 2-A and enter third distillation column 2-C jointly, or
It is individually added into, if supplement water is individually added into, needs that supplement water feed inlet is additionally arranged on third distillation column 2-C.
PODEn raw material (2-1) enters first rectifying column (2-A), and first rectifying column (2-A) overhead extraction is essentially formic acid first
Ester, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (2-2)；First rectifying column (2-A) kettle material (2-
3) enter Second distillation column (2-B), Second distillation column (2-B) overhead extraction is essentially PODE3-5Material (2-4) and tower reactor base
This is PODE6-10Material (2-5)；First rectifying column (2-A) tower top material (2-2) enters third distillation column (2-C), while the
Three rectifying columns (2-C) introduce supplement water (2-6), and the extraction of third distillation column (2-C) tower reactor is essentially formalin and trimerization first
The material (2-8) of aldehyde；Third distillation column (2-C) tower top material (2-7) enters the 4th rectifying column (2-D), the 4th rectifying column (2-D)
Overhead extraction is essentially the material (2-9) of methyl formate, dimethoxym ethane and methanol；4th rectifying column (2-D) tower top material (2-9) into
Enter the 5th rectifying column (2-E), the 5th rectifying column (2-E) overhead extraction be essentially methyl formate material (2-11) and tower reactor it is basic
For the material (2-12) of dimethoxym ethane and methanol；4th rectifying column (2-D) kettle material (2-10) enters dewatering unit (2-F), water
(13) are divided to be removed；Material (2-14) after removing water enters the 6th rectifying column (2-G), and overhead extraction is essentially the material of methanol
(2-15) and tower reactor are essentially PODE2Material (2-16)；Wherein, the operating pressure of first rectifying column (2-A) is 80-
120KPa, tower top operation temperature are 70-100 DEG C, and the operating pressure of Second distillation column (2-B) is 1-50KPa, the operation temperature of tower top
Degree is 50-150 DEG C, and the operating pressure of third distillation column (2-C) is 80-120KPa, and tower top operation temperature is 70-120 DEG C, supplement
Water (2-6) content is by weight 0.2:1~1:1, the operating pressure of the 4th rectifying column (2-D) with the mass ratio of material (2-2)
For 100-200KPa, tower top operation temperature is 35-70 DEG C, and the operating pressure of the 5th rectifying column (2-E) is 100-200KPa, tower top
Operation temperature be 30-60 DEG C, dewatering unit (2-F) be film dehydration, molecular sieve dehydration, adsorption dewatering, the 6th rectifying column (2-G)
Operating pressure is 100-200KPa, and tower top operation temperature is 60-90 DEG C.
(c) scheme 3 (as shown in Figure 3)
A kind of separator of polymethoxy dimethyl ether, including six rectifying columns and a dewatering unit, first rectifying column
The tower reactor outlet of 3-A connects the feed inlet of Second distillation column 3-B by pipeline, and the tower top outlet of first rectifying column 3-A passes through pipe
Line connects the feed inlet of third distillation column 3-C, and the tower top outlet of third distillation column 3-C connects the 4th rectifying column 3-D by pipeline
Feed inlet, the tower reactor discharge port of third distillation column 3-C connects the feed inlet of the 5th rectifying column 3-E, the 5th rectifying by pipeline
The tower top discharge port of tower 3-E connects the feed inlet of dewatering unit 3-F, the discharge port connection the 6th of dewatering unit 3-F by pipeline
The feed inlet of rectifying column 3-G.It supplements water and can discharge with the tower top of first rectifying column 3-A and enter third distillation column 3-C jointly, or
It is individually added into, if supplement water is individually added into, needs that supplement water feed inlet is additionally arranged on third distillation column 3-C.
PODEn raw material (3-1) enters first rectifying column (3-A), and first rectifying column (3-A) overhead extraction is essentially formic acid first
Ester, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (3-2)；First rectifying column (3-A) kettle material (3-
3) enter Second distillation column (3-B), Second distillation column (3-B) overhead extraction is essentially PODE3-5Material (3-4) and tower reactor base
This is PODE6-10Material (3-5)；First rectifying column (3-A) tower top material (3-2) enters third distillation column (3-C), while the
Three rectifying columns (3-C) introduce supplement water (3-6), and third distillation column (3-C) overhead extraction is essentially methyl formate, dimethoxym ethane and first
The material (3-7) of alcohol；Third distillation column (3-C) tower top material (3-7) enters the 4th rectifying column (3-D), the 4th rectifying column (3-D)
Overhead extraction is essentially the material (3-9) of methyl formate and tower reactor is essentially the material (3-10) of dimethoxym ethane and methanol；Third essence
Tower (3-C) kettle material (3-8) is evaporated into the 5th rectifying column (3-E), and the extraction of the 5th rectifying column (3-E) tower reactor is essentially formalin
The material (3-12) of solution and metaformaldehyde；5th rectifying column (3-E) tower top material (3-11) enters dewatering unit (3-F), water
(3-13) is divided to be removed；Material (3-14) after removing water enters the 6th rectifying column (3-G), and overhead extraction is essentially the object of methanol
Material (3-15) and tower reactor are essentially PODE2Material (3-16)；Wherein, the operating pressure of first rectifying column (3-A) is 80-
120KPa, tower top operation temperature are 70-100 DEG C, and the operating pressure of Second distillation column (3-B) is 1-50KPa, the operation temperature of tower top
Degree is 50-150 DEG C, and the operating pressure of third distillation column (3-C) is 100-200KPa, and tower top operation temperature is 35-70 DEG C, supplement
Water (3-6) content is by weight 0.2:1~1:1, the operating pressure of the 4th rectifying column (3-D) with the mass ratio of material (3-2)
For 100-200KPa, tower top operation temperature is 30-60 DEG C, and the operating pressure of the 5th rectifying column (3-E) is 80-120KPa, tower top
Operation temperature is 70-120 DEG C, and dewatering unit (3-F) is film dehydration, molecular sieve dehydration, adsorption dewatering, the 6th rectifying column (3-G)
Operating pressure be 80-120KPa, tower top operation temperature be 60-90 DEG C.
(d) scheme 4 (as shown in Figure 4)
A kind of separator of polymethoxy dimethyl ether, including six rectifying columns and a dewatering unit, first rectifying column
The tower reactor outlet of 4-A connects the feed inlet of Second distillation column 4-B by pipeline, and the tower top outlet of first rectifying column 4-A passes through pipe
Line connects the feed inlet of third distillation column 4-C, and the tower reactor outlet of third distillation column 4-C connects the 4th rectifying column 4-D by pipeline
Feed inlet, the tower reactor discharge port of the 4th rectifying column 4-D connects the feed inlet of the 5th rectifying column 4-E, the 5th rectifying by pipeline
The tower top discharge port of tower 4-E connects the feed inlet of dewatering unit 4-F, the discharge port connection the 6th of dewatering unit 4-F by pipeline
The feed inlet of rectifying column 4-G.It supplements water and can discharge with the tower top of first rectifying column 4-A and enter third distillation column 4-C jointly, or
It is individually added into, if supplement water is individually added into, needs that supplement water feed inlet is additionally arranged on third distillation column 4-C.
PODEn raw material (4-1) enters first rectifying column (4-A), and first rectifying column (4-A) overhead extraction is essentially formic acid first
Ester, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (4-2)；First rectifying column (4-A) kettle material (4-
3) enter Second distillation column (4-B), Second distillation column (4-B) overhead extraction is essentially PODE3-5Material (4-4) and tower reactor base
This is PODE6-10Material (4-5)；First rectifying column (4-A) tower top material (4-2) enters third distillation column (4-C), while the
Three rectifying columns (4-C) introduce supplement water (4-6), the material (4-7) of third distillation column (4-C) overhead extraction methyl formate；Third
Rectifying column (4-C) kettle material (4-8) enters the 4th rectifying column (4-D), the 4th rectifying column (4-D) overhead extraction dimethoxym ethane and first
The material (4-9) of alcohol；4th rectifying column (4-D) kettle material (4-10) enters the 5th rectifying column (4-E), the 5th rectifying column (4-
E) the material (4-12) of tower reactor extraction formalin and metaformaldehyde；5th rectifying column (4-E) tower top material (4-11) enters
Dewatering unit (4-F), moisture (4-13) are removed；Material (4-14) after removing water enters the 6th rectifying column (4-G), and tower top is adopted
The material (4-15) of methanol and tower reactor are PODE out2Material (4-16)；Wherein, the operating pressure of first rectifying column (4-A) is
80-120KPa, tower top operation temperature are 70-100 DEG C, and the operating pressure of Second distillation column (4-B) is 1-50KPa, the behaviour of tower top
Making temperature is 50-150 DEG C, and the operating pressure of third distillation column (4-C) is 100-200KPa, and tower top operation temperature is 30-60 DEG C,
Supplementing water (4-6) content is by weight 0.2:1~1:1, the operation of the 4th rectifying column (4-D) with the mass ratio of material (4-2)
Pressure is 100-200KPa, and tower top operation temperature is 35-70 DEG C, and the operating pressure of the 5th rectifying column (4-E) is 80-120KPa,
Tower top operation temperature is 70-120 DEG C, and dewatering unit (4-F) is film dehydration, molecular sieve dehydration, adsorption dewatering, the 6th rectifying column
The operating pressure of (4-G) is 80-120KPa, and tower top operation temperature is 60-90 DEG C.
(f) scheme 5 (as shown in Figure 5)
A kind of separator of polymethoxy dimethyl ether, including six rectifying columns and a dewatering unit, first rectifying column
The tower reactor outlet of 5-A connects the feed inlet of Second distillation column 5-B by pipeline, and the tower top outlet of first rectifying column 5-A passes through pipe
Line connects the feed inlet of third distillation column 5-C, and the tower reactor outlet of third distillation column 5-C connects the 4th rectifying column 5-D by pipeline
Feed inlet, the tower top discharge port of the 4th rectifying column 5-D connects the feed inlet of the 5th rectifying column 5-E, the 5th rectifying by pipeline
The tower reactor discharge port of tower 5-E connects the feed inlet of dewatering unit 5-F, the discharge port connection the 6th of dewatering unit 5-F by pipeline
The feed inlet of rectifying column 5-G.It supplements water and can discharge with the tower top of first rectifying column 5-A and enter third distillation column 5-C jointly, or
It is individually added into, if supplement water is individually added into, needs that supplement water feed inlet is additionally arranged on third distillation column 5-C.
PODEn raw material (5-1) enters first rectifying column (5-A), and first rectifying column (5-A) overhead extraction is essentially formic acid first
Ester, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (5-2)；First rectifying column (5-A) kettle material (5-
3) enter Second distillation column (5-B), Second distillation column (5-B) overhead extraction PODE3-5Material (5-4) and tower reactor be PODE6-10
Material (5-5)；First rectifying column (5-A) tower top material (5-2) enters third distillation column (5-C), while third distillation column (5-
C supplement water (5-6), the material (5-7) of third distillation column (5-C) overhead extraction methyl formate) are introduced；Third distillation column (5-C)
Kettle material (5-8) enters the 4th rectifying column (5-D), and the 4th rectifying column (5-D) tower reactor produces formalin and metaformaldehyde
Material (5-10)；4th rectifying column (5-D) tower top material (5-9) enters the 5th rectifying column (5-E), the 5th rectifying column (5-E)
The material (5-11) of overhead extraction dimethoxym ethane and methanol；5th rectifying column (5-E) kettle material (5-12) enters dewatering unit (5-
F), moisture (5-13) is removed；Material (5-14) after removing water enters the 6th rectifying column (5-G), the object of overhead extraction methanol
Expect (5-15) and tower reactor is PODE2Material (5-16)；Wherein, the operating pressure of first rectifying column (5-A) is 80-120KPa,
Tower top operation temperature is 70-100 DEG C, and the operating pressure of Second distillation column (5-B) is 1-50KPa, and the operation temperature of tower top is 50-
150 DEG C, the operating pressure of third distillation column (5-C) is 100-200KPa, and tower top operation temperature is 30-60 DEG C, is supplemented water (5-6)
Content is 0.2:1~1:1 with the mass ratio of material (5-2) by weight, and the operating pressure of the 4th rectifying column (5-D) is 80-
120KPa, tower top operation temperature are 70-120 DEG C, and the operating pressure of the 5th rectifying column (5-E) is 100-200KPa, tower top operation
Temperature is 35-70 DEG C, and dewatering unit (5-F) is film dehydration, molecular sieve dehydration, adsorption dewatering, the operation of the 6th rectifying column (5-G)
Pressure is 100-200KPa, and tower top operation temperature is 60-90 DEG C.
The invention has the benefit that
The present invention is directed to using methanol and synthesizes polymethoxy dimethyl ether (PODEn) product as catalytic material with formalin
Complicated component, formaldehyde easily polymerize in rectifying separation process, the state of the art that unreacting material need to be separately recovered, propose it is a kind of into
Material is methyl formate, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Mixed material rectifying column introduce supplement water
The method and apparatus for realizing polymethoxy dimethyl ether separation and purification, the unique distinction of method are as follows:
1. other intermediate species such as dimethoxym ethane discharge jointly with formaldehyde, reduce the easy oligomer concentrations such as hemiacetal, methylene glycol,
Its polymerization blocking pipeline is prevented, equipment is improved and uses continuity.
2. tower reactor produces the aqueous solution containing formaldehyde by introducing supplement water, oxymethylene polymerization blocking condenser and pipeline are prevented,
It improves equipment and uses continuity, while the aqueous solution containing formaldehyde recycled may return to formaldehyde and methanol oxidation synthesizing dimethoxym ethane
Reaction unit rationally recycles unreacting material, improves raw material availability.
3. by being methyl formate, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE in charging2Mixed material
Rectifying column introduce supplement water, more methanol are removed with dimethoxym ethane in tower top, reduce subsequent dewatering unit and afterbody essence
Evaporate the energy consumption of tower.
Detailed description of the invention
Fig. 1 is the separating technology flow diagram of embodiment 1；
Fig. 2 is the separating technology flow diagram of embodiment 2；
Fig. 3 is the separating technology flow diagram of embodiment 3；
Fig. 4 is the separating technology flow diagram of embodiment 4；
Fig. 5 is the separating technology flow diagram of embodiment 5；
Specific embodiment
The invention will be further described with reference to the accompanying drawing and by specific embodiment, and following embodiment is descriptive
, it is not restrictive, this does not limit the scope of protection of the present invention.
Embodiment 1
1-A is first rectifying column in Fig. 1, and 1-B is Second distillation column, and 1-C is third distillation column, and 1-D is the 4th rectifying column,
1-E is the 5th rectifying column, and 1-F is dewatering unit, the 6th rectifying column of 1-G.
The tower reactor outlet of first rectifying column 1-A connects the feed inlet of Second distillation column 1-B, first rectifying column 1- by pipeline
The tower top outlet of A connects the feed inlet of third distillation column 1-C by pipeline, and the tower top outlet of third distillation column 1-C passes through pipeline
The feed inlet of the 4th rectifying column 1-D is connected, the tower reactor discharge port of the 4th rectifying column 1-D connects the 5th rectifying column 1-E by pipeline
Feed inlet, the tower reactor discharge port of the 5th rectifying column 1-E connects the feed inlet of dewatering unit 1-F, dewatering unit 1-F by pipeline
Discharge port connect the 6th rectifying column 1-G feed inlet.
It supplements water and can discharge with the tower top of first rectifying column 1-A and enter third distillation column 1-C jointly, or be individually added into,
If supplement water is individually added into, need that supplement water feed inlet is additionally arranged on third distillation column 1-C.
Material 1-1 is that PODEn waits for that refined material, 1-2 are without PODE3-10To refined material, 1-3 PODE3-10Object
Material, 1-4 PODE3-5Product material, 1-5 PODE6-10Material, 1-6 be pure water material, 1-7 be methyl formate, first contract
Aldehyde, methanol, water and PODE2Material, 1-8 be formalin and metaformaldehyde material, 1-9 be methyl formate material, 1-10
For dimethoxym ethane, methanol, water and PODE2Material, 1-11 be dimethoxym ethane and methanol material, 1-12 PODE2, water and methanol
Material, 1-13 are water material, and 1-14 is methanol and PODE2Material, 1-15 are methanol charge, 1-16 PODE2Material.
PODEn raw material (1-1) enters first rectifying column (1-A), first rectifying column (1-A) overhead extraction methyl formate, first
Acetal, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (1-2)；First rectifying column (1-A) kettle material (1-3) enters
Second distillation column (1-B), Second distillation column (1-B) overhead extraction PODE3-5Material (1-4) and tower reactor be PODE6-10Material
(1-5)；First rectifying column (1-A) tower top material (1-2) enters third distillation column (1-C), while third distillation column (1-C) introduces
It supplements water (1-6), third distillation column (1-C) tower reactor produces the material (1-8) of formalin and metaformaldehyde；Third distillation column
(1-C) tower top material (1-7) enters the 4th rectifying column (1-D), the material of the 4th rectifying column (1-D) overhead extraction methyl formate
(1-9)；4th rectifying column (1-D) kettle material (1-10) enters the 5th rectifying column (1-E), and the 5th rectifying column (1-E) tower top is adopted
The material (1-11) of dimethoxym ethane and methanol out；5th rectifying column (1-E) kettle material (1-12) enters dewatering unit (1-F), water
(1-13) is divided to be removed；Material (1-14) after removing water enters the 6th rectifying column (1-G), the material (1- of overhead extraction methanol
15) and tower reactor is PODE2Material (1-16).
The synthetic product mixture of 1800t/h PODEn forms as follows:
| Number | Component | Content % |
| 1 | Methyl formate | 1.80 |
| 2 | Dimethoxym ethane | 36.66 |
| 3 | Methanol | 5.19 |
| 4 | Formaldehyde | 9.08 |
| 5 | Water | 1.17 |
| 6 | Metaformaldehyde | 2.50 |
| 7 | PODE2 | 20.96 |
| 8 | PODE3-5 | 20.03 |
| 9 | PODE6-10 | 2.41 |
It is separated using this method scheme 1, first rectifying column (1-A) operating pressure 100KPa, 90 DEG C of tower top operation temperature, the
Two rectifying columns (1-B) operating pressure 1KPa, 52 DEG C of tower top operation temperature, third distillation column (1-C) operating pressure 100KPa, supplement
Water (1-6) amount and material (1-2) mass ratio 0.4:1,80 DEG C of tower top operation temperature, the 4th rectifying column (1-D) operating pressure
100KPa, 32 DEG C of tower top operation temperature, the 5th rectifying column (1-E) operating pressure 100KPa, 40 DEG C of tower top operation temperature, dehydration is single
First (1-F) is dehydrated using film, the 6th rectifying column (1-G) operating pressure 100KPa, and 64 DEG C of tower top operation temperature.
The methyl formate of isolated 32t/h, the PODE of dimethoxym ethane and methanol charge 670t/h, 377t/h2, 360t/h's
PODE3-5Qualified products, and recycled the formalin of 466t/h mass fraction 35% or so.
Embodiment 2
2-A is first rectifying column in Fig. 2, and 2-B is Second distillation column, and 2-C is third distillation column, and 2-D is the 4th rectifying column,
2-E is the 5th rectifying column, and 2-F is dewatering unit, the 6th rectifying column of 2-G.
The tower reactor outlet of first rectifying column 2-A connects the feed inlet of Second distillation column 2-B, first rectifying column 2- by pipeline
The tower top outlet of A connects the feed inlet of third distillation column 2-C by pipeline, and the tower top outlet of third distillation column 2-C passes through pipeline
The feed inlet of the 4th rectifying column 2-D is connected, the tower top discharge port of the 4th rectifying column 2-D connects the 5th rectifying column 2-E by pipeline
Feed inlet, the tower reactor discharge port of the 4th rectifying column 2-D connects the feed inlet of dewatering unit 2-F, dewatering unit 2-F by pipeline
Discharge port connect the 6th rectifying column 2-G feed inlet.
It supplements water and can discharge with the tower top of first rectifying column 2-A and enter third distillation column 2-C jointly, or be individually added into,
If supplement water is individually added into, need that supplement water feed inlet is additionally arranged on third distillation column 2-C.
Material 2-1 is that PODEn waits for that refined material, 2-2 are without PODE3-10To refined material, 2-3 PODE3-10Object
Material, 2-4 PODE3-5Product material, 2-5 PODE6-10Material, 2-6 be pure water material, 2-7 be methyl formate, first contract
Aldehyde, methanol, water, formaldehyde, metaformaldehyde and PODE2Material, 2-8 be formalin and metaformaldehyde material, 2-9 is formic acid
The material of methyl esters, dimethoxym ethane and methanol, 2-10 PODE2, water and methanol material, 2-11 is methyl formate, and 2-12 is first contracting
The material of aldehyde and methanol, 2-13 are water material, and 2-14 is methanol and PODE2Material, 2-15 are methanol charge, 2-16 PODE2Object
Material.
PODEn raw material (2-1) enters first rectifying column (2-A), first rectifying column (2-A) overhead extraction methyl formate, first
Acetal, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (2-2)；First rectifying column (2-A) kettle material (2-3) enters
Second distillation column (2-B), Second distillation column (2-B) overhead extraction PODE3-5Material (2-4) and tower reactor be PODE6-10Material
(2-5)；First rectifying column (2-A) tower top material (2-2) enters third distillation column (2-C), while third distillation column (2-C) introduces
It supplements water (2-6), third distillation column (2-C) tower reactor produces the material (2-8) of formalin and metaformaldehyde；Third distillation column
(2-C) tower top material (2-7) enters the 4th rectifying column (2-D), the 4th rectifying column (2-D) overhead extraction methyl formate, dimethoxym ethane
With the material (2-9) of methanol；4th rectifying column (2-D) tower top material (2-9) enters the 5th rectifying column (2-E), the 5th rectifying column
The material (2-11) and tower reactor of (2-E) overhead extraction methyl formate are the material (2-12) of dimethoxym ethane and methanol；4th rectifying column
(2-D) kettle material (2-10) enters dewatering unit (2-F), and moisture (13) is removed；Material (2-14) after removing water enters
6th rectifying column (2-G), the material (2-15) and tower reactor of overhead extraction methanol are PODE2Material (2-16).
The synthetic product mixture of 2400t/h PODEn forms as follows:
| Number | Component | Content % |
| 1 | Methyl formate | 1.80 |
| 2 | Dimethoxym ethane | 36.66 |
| 3 | Methanol | 5.19 |
| 4 | Formaldehyde | 9.08 |
| 5 | Water | 1.17 |
| 6 | Metaformaldehyde | 2.50 |
| 7 | PODE2 | 20.96 |
| 8 | PODE3-5 | 20.03 |
| 9 | PODE6-10 | 2.41 |
It is separated using this method scheme 2, first rectifying column (2-A) operating pressure 100KPa, 90 DEG C of tower top operation temperature, the
Two rectifying columns (2-B) operating pressure 1KPa, 52 DEG C of tower top operation temperature, third distillation column (2-C) operating pressure 100KPa, supplement
Water (2-6) content and material (2-2) mass ratio 0.3:1,80 DEG C of tower top operation temperature, the 4th rectifying column (2-D) operating pressure
100KPa, 40 DEG C of tower top operation temperature, the 5th rectifying column (2-E) operating pressure 100KPa, 32 DEG C of tower top operation temperature, dehydration is single
First (2-F) uses molecular sieve dehydration, the 6th rectifying column (2-G) operating pressure 100KPa, and 64 DEG C of tower top operation temperature.
The methyl formate of isolated 42t/h, the PODE of dimethoxym ethane and methanol charge 893t/h, 503t/h2, 480t/h's
PODE3-5Qualified products, and recycled the formalin of 660t/h mass fraction 33% or so.
Embodiment 3
3-A is first rectifying column in Fig. 3, and 3-B is Second distillation column, and 3-C is third distillation column, and 3-D is the 4th rectifying column,
3-E is the 5th rectifying column, and 3-F is dewatering unit, the 6th rectifying column of 3-G.
The tower reactor outlet of first rectifying column 3-A connects the feed inlet of Second distillation column 3-B, first rectifying column 3- by pipeline
The tower top outlet of A connects the feed inlet of third distillation column 3-C by pipeline, and the tower top outlet of third distillation column 3-C passes through pipeline
The feed inlet of the 4th rectifying column 3-D is connected, the tower reactor discharge port of third distillation column 3-C connects the 5th rectifying column 3-E by pipeline
Feed inlet, the tower top discharge port of the 5th rectifying column 3-E connects the feed inlet of dewatering unit 3-F, dewatering unit 3-F by pipeline
Discharge port connect the 6th rectifying column 3-G feed inlet.
It supplements water and can discharge with the tower top of first rectifying column 3-A and enter third distillation column 3-C jointly, or be individually added into,
If supplement water is individually added into, need that supplement water feed inlet is additionally arranged on third distillation column 3-C.
Material 3-1 is that PODEn waits for that refined material, 3-2 are without PODE3-10To refined material, 3-3 PODE3-10Object
Material, 3-4 PODE3-5Product material, 3-5 PODE6-10Material, 3-6 be pure water material, 3-7 be methyl formate, first contract
The material of aldehyde and methanol, 3-8 are methanol, formaldehyde, water, metaformaldehyde and PODE2Material, 3-9 is methyl formate, and 3-10 is first
The material of acetal and methanol, 3-11 are water, PODE2With the material of methanol, 3-12 is the material of formalin and metaformaldehyde,
3-13 is water material, and 3-14 is methanol and PODE2Material, 3-15 are methanol charge, 3-16 PODE2Material.
PODEn raw material (3-1) enters first rectifying column (3-A), first rectifying column (3-A) overhead extraction methyl formate, first
Acetal, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (3-2)；First rectifying column (3-A) kettle material (3-3) enters
Second distillation column (3-B), Second distillation column (3-B) overhead extraction PODE3-5Material (3-4) and tower reactor be PODE6-10Material
(3-5)；First rectifying column (3-A) tower top material (3-2) enters third distillation column (3-C), while third distillation column (3-C) introduces
It supplements water (3-6), the material (3-7) of third distillation column (3-C) overhead extraction methyl formate, dimethoxym ethane and methanol；Third rectifying
Tower (3-C) tower top material (3-7) enters the 4th rectifying column (3-D), the material of the 4th rectifying column (3-D) overhead extraction methyl formate
(3-9) and tower reactor are the material (3-10) of dimethoxym ethane and methanol；Third distillation column (3-C) kettle material (3-8) enters the 5th essence
It evaporates tower (3-E), the 5th rectifying column (3-E) tower reactor produces the material (3-12) of formalin and metaformaldehyde；5th rectifying column
(3-E) tower top material (3-11) enters dewatering unit (3-F), and moisture (3-13) is removed；Remove water after material (3-14) into
Enter the 6th rectifying column (3-G), the material (3-15) and tower reactor of overhead extraction methanol are PODE2Material (3-16).
The synthetic product mixture of 2700t/h PODEn forms as follows:
| Number | Component | Content % |
| 1 | Methyl formate | 1.80 |
| 2 | Dimethoxym ethane | 36.66 |
| 3 | Methanol | 5.19 |
| 4 | Formaldehyde | 9.08 |
| 5 | Water | 1.17 |
| 6 | Metaformaldehyde | 2.50 |
| 7 | PODE2 | 20.96 |
| 8 | PODE3-5 | 20.03 |
| 9 | PODE6-10 | 2.41 |
It is separated using this method scheme 3, first rectifying column (3-A) operating pressure 100KPa, 90 DEG C of tower top operation temperature, the
Two rectifying columns (3-B) operating pressure 50KPa, is mended by 144 DEG C of tower top operation temperature, third distillation column (3-C) operating pressure 100KPa
Water-filling (3-6) amount and material (3-2) mass ratio 0.5:1,80 DEG C of tower top operation temperature, the 4th rectifying column (3-D) operating pressure
200KPa, 51 DEG C of tower top operation temperature, the 5th rectifying column (3-E) operating pressure 100KPa, 80 DEG C of tower top operation temperature, dehydration is single
First (3-F) uses adsorption dewatering, the 6th rectifying column (3-G) operating pressure 100KPa, and 64 DEG C of tower top operation temperature.
The methyl formate of isolated 48t/h, the PODE of dimethoxym ethane and methanol charge 1004t/h, 566t/h2, 540t/h
PODE3-5Qualified products, and recycled the formalin of 875t/h mass fraction 28% or so.
Embodiment 4
4-A is first rectifying column in Fig. 4, and 4-B is Second distillation column, and 4-C is third distillation column, and 4-D is the 4th rectifying column,
4-E is the 5th rectifying column, and 4-F is dewatering unit, the 6th rectifying column of 4-G.
The tower reactor outlet of first rectifying column 4-A connects the feed inlet of Second distillation column 4-B, first rectifying column 4- by pipeline
The tower top outlet of A connects the feed inlet of third distillation column 4-C by pipeline, and the tower reactor outlet of third distillation column 4-C passes through pipeline
The feed inlet of the 4th rectifying column 4-D is connected, the tower reactor discharge port of the 4th rectifying column 4-D connects the 5th rectifying column 4-E by pipeline
Feed inlet, the tower top discharge port of the 5th rectifying column 4-E connects the feed inlet of dewatering unit 4-F, dewatering unit 4-F by pipeline
Discharge port connect the 6th rectifying column 4-G feed inlet.
It supplements water and can discharge with the tower top of first rectifying column 4-A and enter third distillation column 4-C jointly, or be individually added into,
If supplement water is individually added into, need that supplement water feed inlet is additionally arranged on third distillation column 4-C.
Material 4-1 is that PODEn waits for that refined material, 4-2 are without PODE3-10To refined material, 4-3 PODE3-10Object
Material, 4-4 PODE3-5Product material, 4-5 PODE6-10Material, 4-6 be pure water material, 4-7 be methyl formate material,
4-8 is dimethoxym ethane, methanol, formaldehyde, water, metaformaldehyde and PODE2Material, 4-9 is the material of dimethoxym ethane and methanol, and 4-10 is
Methanol, water, formaldehyde, metaformaldehyde and PODE2Material, 4-11 be water, PODE2With the material of methanol, 4-12 is formalin
With the material of metaformaldehyde, 4-13 is water material, and 4-14 is methanol and PODE2Material, 4-15 are methanol charge, 4-16 PODE2
Material.
PODEn raw material (4-1) enters first rectifying column (4-A), first rectifying column (4-A) overhead extraction methyl formate, first
Acetal, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (4-2)；First rectifying column (4-A) kettle material (4-3) enters
Second distillation column (4-B), Second distillation column (4-B) overhead extraction PODE3-5Material (4-4) and tower reactor be PODE6-10Material
(4-5)；First rectifying column (4-A) tower top material (4-2) enters third distillation column (4-C), while third distillation column (4-C) introduces
It supplements water (4-6), the material (4-7) of third distillation column (4-C) overhead extraction methyl formate；Third distillation column (4-C) tower reactor object
Expect that (4-8) enters the 4th rectifying column (4-D), the material (4-9) of the 4th rectifying column (4-D) overhead extraction dimethoxym ethane and methanol；The
Four rectifying columns (4-D) kettle material (4-10) enters the 5th rectifying column (4-E), and the extraction of the 5th rectifying column (4-E) tower reactor is essentially
The material (4-12) of formalin and metaformaldehyde；5th rectifying column (4-E) tower top material (4-11) enters dewatering unit (4-
F), moisture (4-13) is removed；Material (4-14) after removing water enters the 6th rectifying column (4-G), the object of overhead extraction methanol
Expect (4-15) and tower reactor is PODE2Material (4-16).
The synthetic product mixture of 2400t/h PODEn forms as follows:
| Number | Component | Content % |
| 1 | Methyl formate | 1.80 |
| 2 | Dimethoxym ethane | 36.66 |
| 3 | Methanol | 5.19 |
| 4 | Formaldehyde | 9.08 |
| 5 | Water | 1.17 |
| 6 | Metaformaldehyde | 2.50 |
| 7 | PODE2 | 20.96 |
| 8 | PODE3-5 | 20.03 |
| 9 | PODE6-10 | 2.41 |
It is separated using this method scheme 4, first rectifying column (4-A) operating pressure 100KPa, 90 DEG C of tower top operation temperature, the
Two rectifying columns (4-B) operating pressure 1KPa, 52 DEG C of tower top operation temperature, third distillation column (4-C) operating pressure 100KPa, supplement
Water (4-6) content and material (4-2) mass ratio 0.3:1,32 DEG C of tower top operation temperature, the 4th rectifying column (4-D) operating pressure
100KPa, 40 DEG C of tower top operation temperature, the 5th rectifying column (4-E) operating pressure 100KPa, 80 DEG C of tower top operation temperature, dehydration is single
First (4-F) uses molecular sieve dehydration, the 6th rectifying column (4-G) operating pressure 100KPa, and 64 DEG C of tower top operation temperature.
The methyl formate of isolated 42t/h, the PODE of dimethoxym ethane and methanol charge 893t/h, 503t/h2, 480t/h's
PODE3-5Qualified products, and recycled the formalin of 660t/h mass fraction 33% or so.
Embodiment 5
5-A is first rectifying column in Fig. 5, and 5-B is Second distillation column, and 5-C is that third distillation column 5-D is the 4th rectifying column,
5-E is the 5th rectifying column, and 5-F is dewatering unit, the 6th rectifying column of 5-G；
The tower reactor outlet of first rectifying column 5-A connects the feed inlet of Second distillation column 5-B, first rectifying column 5- by pipeline
The tower top outlet of A connects the feed inlet of third distillation column 5-C by pipeline, and the tower reactor outlet of third distillation column 5-C passes through pipeline
The feed inlet of the 4th rectifying column 5-D is connected, the tower top discharge port of the 4th rectifying column 5-D connects the 5th rectifying column 5-E by pipeline
Feed inlet, the tower reactor discharge port of the 5th rectifying column 5-E connects the feed inlet of dewatering unit 5-F, dewatering unit 5-F by pipeline
Discharge port connect the 6th rectifying column 5-G feed inlet.
It supplements water and can discharge with the tower top of first rectifying column 5-A and enter third distillation column 5-C jointly, or be individually added into,
If supplement water is individually added into, need that supplement water feed inlet is additionally arranged on third distillation column 5-C.
Material 5-1 is that PODEn waits for that refined material, 5-2 are without PODE3-10To refined material, 5-3 PODE3-10Object
Material, 5-4 PODE3-5Product material, 5-5 PODE6-10Material, 5-6 be pure water material, 5-7 be methyl formate material,
5-8 is dimethoxym ethane, methanol, formaldehyde, water, metaformaldehyde and PODE2Material, 5-9 be dimethoxym ethane, methanol, water and PODE2Object
Material, 5-10 be formalin and metaformaldehyde material, 5-11 be dimethoxym ethane and methanol material, 5-12 be methanol, water and
PODE2Material, 5-13 be water material, 5-14 be methanol and PODE2Material, 5-15 are methanol charge, 5-16 PODE2Material.
PODEn raw material (5-1) enters first rectifying column (5-A), first rectifying column (5-A) overhead extraction methyl formate, first
Acetal, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (5-2)；First rectifying column (5-A) kettle material (5-3) enters
Second distillation column (5-B), Second distillation column (5-B) overhead extraction PODE3-5Material (5-4) and tower reactor be PODE6-10Material
(5-5)；First rectifying column (5-A) tower top material (5-2) enters third distillation column (5-C), while third distillation column (5-C) introduces
It supplements water (5-6), the material (5-7) of third distillation column (5-C) overhead extraction methyl formate；Third distillation column (5-C) tower reactor object
Expect that (5-8) enters the 4th rectifying column (5-D), the 4th rectifying column (5-D) tower reactor produces the material of formalin and metaformaldehyde
(5-10)；4th rectifying column (5-D) tower top material (5-9) enters the 5th rectifying column (5-E), and the 5th rectifying column (5-E) tower top is adopted
The material (5-11) of dimethoxym ethane and methanol out；5th rectifying column (5-E) kettle material (5-12) enters dewatering unit (5-F), water
(5-13) is divided to be removed；Material (5-14) after removing water enters the 6th rectifying column (5-G), the material (5- of overhead extraction methanol
15) and tower reactor is PODE2Material (5-16).
The synthetic product mixture of 1800t/h PODEn forms as follows:
| Number | Component | Content % |
| 1 | Methyl formate | 1.80 |
| 2 | Dimethoxym ethane | 36.66 |
| 3 | Methanol | 5.19 |
| 4 | Formaldehyde | 9.08 |
| 5 | Water | 1.17 |
| 6 | Metaformaldehyde | 2.50 |
| 7 | PODE2 | 20.96 |
| 8 | PODE3-5 | 20.03 |
| 9 | PODE6-10 | 2.41 |
It is separated using this method scheme 5, first rectifying column (5-A) operating pressure 100KPa, 90 DEG C of tower top operation temperature, the
Two rectifying columns (5-B) operating pressure 1KPa, 52 DEG C of tower top operation temperature, third distillation column (5-C) operating pressure 100KPa, supplement
Water (5-6) amount and material (5-2) mass ratio 0.4:1,32 DEG C of tower top operation temperature, the 4th rectifying column (5-D) operating pressure
100KPa, 80 DEG C of tower top operation temperature, the 5th rectifying column (5-E) operating pressure 100KPa, 40 DEG C of tower top operation temperature, dehydration is single
First (5-F) is dehydrated using film, the 6th rectifying column (5-G) operating pressure 100KPa, and 64 DEG C of tower top operation temperature.
The methyl formate of isolated 32t/h, the PODE of dimethoxym ethane and methanol charge 670t/h, 377t/h2, 360t/h's
PODE3-5Qualified products, and recycled the formalin of 466t/h mass fraction 35% or so.
One kind proposed by the present invention is methyl formate, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE in charging2
Mixed material rectifying column introduce supplement water realize polymethoxy dimethyl ether separation and purification method and apparatus, passed through
Preferred embodiment is described, related technical personnel obviously can not depart from the content of present invention, in spirit and scope it is right
Structure and equipment as described herein are modified or appropriate changes and combinations, Lai Shixian the technology of the present invention.In particular
It is that all similar replacements and change are apparent to those skilled in the art, they are considered as being included in
In spirit of that invention, range and content.
Claims (10)
1. a kind of separation method of polymethoxy dimethyl ether, using multistage rectification, it is characterised in that: charging be methyl formate,
Dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Mixed material rectifying column in introduce supplement water, formalin
And metaformaldehyde produces to realize the purpose of separating formaldehyde and metaformaldehyde from tower reactor.
2. the separation method of polymethoxy dimethyl ether according to claim 1, it is characterised in that: supplement the additional amount of water with
Poidometer and the mass ratio of charging are 0.2:1~1:1.
3. the separation method of polymethoxy dimethyl ether according to claim 1, it is characterised in that: supplement water and feed from same
One feed inlet is added or separates to be added from two feed inlets.
4. the separation method of polymethoxy dimethyl ether according to claim 1, it is characterised in that: six grades of rectifying are used,
PODEn raw material enters first rectifying column, and first rectifying column overhead extraction is methyl formate, dimethoxym ethane, methanol, water, formaldehyde, trimerization
Formaldehyde and PODE2Mixed material；First rectifying column kettle material enters Second distillation column, and Second distillation column overhead extraction is
PODE3-5Material, tower reactor PODE6-10Material；First rectifying column tower top material enters third distillation column, while third essence
It evaporates tower and introduces supplement water, the additional amount for supplementing water is by weight 0.2:1~1:1, third distillation column tower with the mass ratio of charging
Kettle extraction is the mixed material of formalin and metaformaldehyde；Third distillation column tower top material enter the 4th rectifying column, the 4th
The top of the distillation column extraction is the material of methyl formate；4th tower bottom of rectifying tower material enters the 5th rectifying column, the 5th rectifying tower
Top extraction is the mixed material of dimethoxym ethane and methanol；5th tower bottom of rectifying tower material enters dewatering unit, the material after removing water
Into the 6th rectifying column, the extraction of the 6th the top of the distillation column is the material of methanol, tower reactor extraction is PODE2Material.
5. the separation method of polymethoxy dimethyl ether according to claim 1, it is characterised in that: six grades of rectifying are used,
PODEn raw material enters first rectifying column, and first rectifying column overhead extraction is methyl formate, dimethoxym ethane, methanol, water, formaldehyde, trimerization
Formaldehyde and PODE2Mixed material；First rectifying column kettle material enters Second distillation column, and Second distillation column overhead extraction is
PODE3-5Material, tower reactor PODE6-10Material；First rectifying column tower top material enters third distillation column, while third essence
It evaporates tower and introduces supplement water, the additional amount for supplementing water is by weight 0.2:1~1:1, third distillation column tower with the mass ratio of charging
Kettle extraction is the mixed material of formalin and metaformaldehyde；Third distillation column tower top material enter the 4th rectifying column, the 4th
The top of the distillation column extraction is the mixed material of methyl formate, dimethoxym ethane and methanol；4th the top of the distillation column material enters the 5th essence
Tower is evaporated, the extraction of the 5th the top of the distillation column is the material of methyl formate, the mixed material that tower reactor is dimethoxym ethane and methanol；4th rectifying
Tower kettle material enters dewatering unit；Material after removing water enters the 6th rectifying column, and the extraction of the 6th the top of the distillation column is methanol
Material, tower reactor PODE2Material.
6. the separation method of polymethoxy dimethyl ether according to claim 1, it is characterised in that: six grades of rectifying are used,
PODEn raw material enters first rectifying column, and first rectifying column overhead extraction is methyl formate, dimethoxym ethane, methanol, water, formaldehyde, trimerization
Formaldehyde and PODE2Mixed material；First rectifying column kettle material enters Second distillation column, and Second distillation column overhead extraction is
PODE3-5Material, tower reactor PODE6-10Material；First rectifying column tower top material enters third distillation column, while third essence
It evaporates tower and introduces supplement water, the additional amount for supplementing water is by weight 0.2:1~1:1, third distillation column tower with the mass ratio of charging
Top extraction is the mixed material of methyl formate, dimethoxym ethane and methanol；Third distillation column tower top material enter the 4th rectifying column, the 4th
The top of the distillation column extraction is the material of methyl formate, the mixed material that tower reactor is dimethoxym ethane and methanol；Third distillation column tower reactor object
Material enters the 5th rectifying column, and the extraction of the 5th tower bottom of rectifying tower is the material of formalin and metaformaldehyde；5th rectifying tower
Top material enters dewatering unit, and the material after removing water enters the 6th rectifying column, and the extraction of the 6th the top of the distillation column is the object of methanol
Material, tower reactor PODE2Material.
7. the separation method of polymethoxy dimethyl ether according to claim 1, it is characterised in that: six grades of rectifying are used,
PODEn raw material enters first rectifying column, and first rectifying column overhead extraction is methyl formate, dimethoxym ethane, methanol, water, formaldehyde, trimerization
Formaldehyde and PODE2Mixed material；First rectifying column kettle material enters Second distillation column, and Second distillation column overhead extraction is
PODE3-5Material, tower reactor PODE6-10Material；First rectifying column tower top material enters third distillation column, while third essence
It evaporates tower and introduces supplement water, the additional amount for supplementing water is by weight 0.2:1~1:1, third distillation column tower with the mass ratio of charging
Top extraction is the material of methyl formate；Third distillation column kettle material enters the 4th rectifying column, and the extraction of the 4th the top of the distillation column is
The mixed material of dimethoxym ethane and methanol；4th tower bottom of rectifying tower material enters the 5th rectifying column, and the extraction of the 5th tower bottom of rectifying tower is
The mixed material of formalin and metaformaldehyde；5th the top of the distillation column material enters dewatering unit, the material after removing water
Into the 6th rectifying column, the extraction of the 6th the top of the distillation column is material, the tower reactor PODE of methanol2Material.
8. the separation method of polymethoxy dimethyl ether according to claim 1, it is characterised in that: six grades of rectifying are used,
PODEn raw material enters first rectifying column, and first rectifying column overhead extraction is methyl formate, dimethoxym ethane, methanol, water, formaldehyde, trimerization
Formaldehyde and PODE2Mixed material；First rectifying column kettle material enters Second distillation column, and Second distillation column overhead extraction is
PODE3-5Material, tower reactor PODE6-10Material；First rectifying column tower top material enters third distillation column, while third essence
It evaporates tower and introduces supplement water, the additional amount for supplementing water is by weight 0.2:1~1:1, third distillation column tower with the mass ratio of charging
Top extraction is the material of methyl formate；Third distillation column kettle material enters the 4th rectifying column, and the extraction of the 4th tower bottom of rectifying tower is
The mixed material of formalin and metaformaldehyde；4th the top of the distillation column material enters the 5th rectifying column, the 5th rectifying tower
Top extraction is the mixed material of dimethoxym ethane and methanol；5th tower bottom of rectifying tower material enters dewatering unit, the material after removing water
Into the 6th rectifying column, the extraction of six the top of the distillation column is material, the tower reactor PODE of methanol2Material.
9. according to the separation method of polymethoxy dimethyl ether described in claim 4~8 any claim, it is characterised in that:
The dewatering unit is film dehydration, molecular sieve dehydration, adsorption dewatering.
10. a kind of separator of polymethoxy dimethyl ether, using multistage rectification, it is characterised in that: charging be methyl formate,
Dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Mixed material rectifying column setting supplement water water inlet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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