CN109776289A - A kind of method and apparatus of separation and purification polymethoxy dimethyl ether - Google Patents
A kind of method and apparatus of separation and purification polymethoxy dimethyl ether Download PDFInfo
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Abstract
It is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE in charging that the present invention relates to a kind of method and apparatus of separation and purification polymethoxy dimethyl ether using multistage rectification2Supplement water is introduced in the rectifying column of mixture, formalin and metaformaldehyde produce to realize the purpose of separating formaldehyde and metaformaldehyde from tower reactor.The process can use different separation sequences.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 dimethoxym ethane, methanol, water, formaldehyde, trimerization first
Aldehyde and PODE2The method and apparatus that supplement water realizes polymethoxy dimethyl ether separation and purification are introduced in the rectifying column of mixture.
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, US
20080221368, US 7671240, US 7700809), conversion per pass is low, and separation process is complicated, and material heats repeatedly to be divided
From energy consumption is high, 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 dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE that the purpose of the present invention is to provide one kind in charging2It is mixed
It closes and introduces the method and apparatus that supplement water realizes polymethoxy dimethyl ether separation and purification in the rectifying column of object.Using distillating method
Separation is refining to obtain the PODEn of suitable diesel component, together using methanol and formalin as the synthetic product of raw material PODEn
When recovery section raw material return to above-mentioned first stage and second stage reaction process respectively.
One kind of the invention is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE in charging2In the rectifying column of mixture
The method and apparatus that introducing supplement water realizes polymethoxy dimethyl ether separation and purification, including six rectifying columns and a dehydration list
Member.
Technical scheme is as follows:
A kind of method of separation and purification polymethoxy dimethyl ether, using multistage rectification, charging be dimethoxym ethane, methanol, water,
Formaldehyde, metaformaldehyde and PODE2Supplement water is introduced in the rectifying column of mixture, formalin and metaformaldehyde are produced from tower reactor
To realize the purpose of separating formaldehyde and metaformaldehyde.
Moreover, the additional amount of supplement water is by weight 0.2:1~0.8:1 with the mass ratio of charging.
It is added moreover, supplement water is added or separates from the same feed inlet with charging from two feed inlets.
The first scheme:
One kind is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE in charging2It introduces and mends in the rectifying column of mixture
Water-filling separates the device of PODEn, including six rectifying columns and a dewatering unit, and the tower reactor outlet of first rectifying column passes through pipeline
The feed inlet of Second distillation column is connected, the tower top outlet of Second distillation column connects the feed inlet of the 4th rectifying column by pipeline, the
The tower reactor outlet of two rectifying columns connects the feed inlet of third distillation column by pipeline, and the tower top discharge port of the 4th rectifying column passes through pipe
Line connects the feed inlet of the 5th rectifying column, and the tower reactor discharge port of the 5th rectifying column connects the feed inlet of dewatering unit by pipeline,
The discharge port of dewatering unit connects the feed inlet of the 6th rectifying column, introduces supplement water in the 4th rectifying column, and the supplement water is from the 4th
The feed inlet of rectifying column is added or the setting supplement water water inlet on the 4th rectifying column.
One kind is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE in charging2It introduces and mends in the rectifying column of mixture
The method that water-filling separates PODEn, process are as follows: PODEn raw material enters first rectifying column, and first rectifying column overhead extraction is formic acid
The material of methyl esters；First rectifying column kettle material enters Second distillation column, Second distillation column overhead extraction be dimethoxym ethane, methanol,
Water, formaldehyde, metaformaldehyde and PODE2Mixed material；Second distillation column kettle material enters third distillation column, third distillation column
Overhead extraction is PODE3-5Material, tower reactor PODE6-10Material；Second distillation column tower top material enters the 4th rectifying column,
The 4th rectifying column introduces supplement water simultaneously, 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, and the extraction of the 5th the top of the distillation column is the mixed material of dimethoxym ethane and methanol；
5th tower bottom of rectifying tower material enters dewatering unit, and moisture is removed；Material after removing water enters the 6th rectifying column, the 6th essence
Evaporate that column overhead extraction be the material of methanol, tower reactor produces is PODE2Material.The operating pressure of first rectifying column is 100-
200KPa, tower top operation temperature are 30-60 DEG C, and the operating pressure of Second distillation column is 80-120KPa, and tower top operation temperature is
70-100 DEG C, the operating pressure of third distillation column is 1-50KPa, and the operation temperature of tower top is 50-150 DEG C, the 4th rectifying column
Operating pressure is 80-120KPa, and tower top operation temperature is 70-120 DEG C, and the operating pressure of the 5th rectifying column is 100-200KPa,
Tower top operation temperature is 35-70 DEG C, and the operating pressure of the 6th rectifying column is 100-200KPa, and tower top operation temperature is 60-90 DEG C.
Second scheme:
One kind is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE in charging2It introduces and mends in the rectifying column of mixture
Water-filling separates the device of PODEn, including six rectifying columns and a dewatering unit, and the tower reactor outlet of first rectifying column passes through pipeline
The feed inlet of Second distillation column is connected, the tower top outlet of Second distillation column connects the feed inlet of the 4th rectifying column by pipeline, the
The tower reactor outlet of two rectifying columns connects the feed inlet of third distillation column by pipeline, and the tower reactor discharge port of the 4th rectifying column passes through pipe
Line connects the feed inlet of the 5th rectifying column, and the tower top discharge port of the 5th rectifying column connects the feed inlet of dewatering unit by pipeline,
The discharge port of dewatering unit connects the feed inlet of the 6th rectifying column, introduces supplement water in the 4th rectifying column, and the supplement water is from the 4th
The feed inlet of rectifying column is added or the setting supplement water water inlet on the 4th rectifying column.
One kind is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE in charging2It introduces and mends in the rectifying column of mixture
The method that water-filling separates PODEn, process are as follows: PODEn raw material enters first rectifying column, and first rectifying column overhead extraction is formic acid
The material of methyl esters；First rectifying column kettle material enters Second distillation column, Second distillation column overhead extraction be dimethoxym ethane, methanol,
Water, formaldehyde, metaformaldehyde and PODE2Mixed material；Second distillation column kettle material enters third distillation column, third distillation column
Overhead extraction is PODE3-5Material, tower reactor extraction be PODE6-10Material；Second distillation column tower top material enters the 4th rectifying
Tower, while the 4th rectifying column introduces supplement water, the extraction of the 4th the top of the distillation column is the mixed material of dimethoxym ethane and methanol；4th essence
Tower kettle material is evaporated into the 5th rectifying column, and the extraction of the 5th tower bottom of rectifying tower is the mixture of formalin and metaformaldehyde
Material；5th the top of the distillation column material enters dewatering unit；Material after removing water enters the 6th rectifying column, the 6th the top of the distillation column
Extraction is the material of methanol, tower reactor extraction is PODE2Material.The operating pressure of first rectifying column is 100-200KPa, tower top
Operation temperature is 30-60 DEG C, and the operating pressure of Second distillation column is 80-120KPa, and tower top operation temperature is 70-100 DEG C, third
The operating pressure of rectifying column is 1-50KPa, and the operation temperature of tower top is 50-150 DEG C, and the operating pressure of the 4th rectifying column is 100-
200KPa, tower top operation temperature are 35-70 DEG C, and the operating pressure of the 5th rectifying column is 80-120KPa, and tower top operation temperature is
70-120 DEG C, the operating pressure of the 6th rectifying column is 100-200KPa, and tower top operation temperature is 60-90 DEG C.
Above-mentioned dewatering unit uses film dehydration, molecular sieve dehydration, adsorption dewatering.It is preferred that film is dehydrated.
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 dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2The rectifying column of mixture introduces supplement water and realizes polymethoxy two
The method and apparatus of methyl 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 dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE in charging2It is introduced in the rectifying column of mixture
Water is supplemented, more methanol are removed with dimethoxym ethane in tower top, reduce the energy consumption of subsequent dewatering unit and the 6th rectifying column.
Detailed description of the invention
Fig. 1 is the separating technology flow diagram of embodiment 1,2；
Fig. 2 is the separating technology flow diagram of embodiment 3.
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, Second distillation column 1- by pipeline
The tower top outlet of B connects the feed inlet of the 4th rectifying column 1-D by pipeline, and the tower reactor outlet of Second distillation column 1-B passes through pipeline
The feed inlet of third distillation column 1-C is connected, the tower top 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 Second distillation column 1-B and enter the 4th rectifying column 1-D jointly, or be individually added into,
If supplement water is individually added into, need that supplement water feed inlet is additionally arranged on the 4th rectifying column 1-D.
Material 1-1 is that PODEn waits for refined material, and 1-2 is methyl formate, and 1-3 is without methyl formate to refined material,
1-4 is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material, 1-5 PODE3-10Material, 1-6 PODE3-5
Product material, 1-7 PODE6-10Material, 1-8 be pure water material, 1-9 be dimethoxym ethane, methanol, water, PODE2Material, 1-
10 be formalin and metaformaldehyde material, and 1-11 is the material of dimethoxym ethane and methanol, 1-12 PODE2, water and methanol object
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), and first rectifying column (1-A) overhead extraction is methyl formate
Material (1-2)；First rectifying column (1-A) kettle material (1-3) enters Second distillation column (1-B), Second distillation column (1-B) tower top
Extraction is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (1-4)；Second distillation column (1-B) kettle material
(1-5) enters third distillation column (1-C), and third distillation column (1-C) overhead extraction is PODE3-5Material (1-6) and tower reactor be
PODE6-10Material (1-7)；Second distillation column (1-B) tower top material (1-4) enters the 4th rectifying column (1-D), while the 4th essence
It evaporates tower (1-D) and introduces supplement water (1-8), the extraction of the 4th rectifying column (1-D) tower reactor is the material of formalin and metaformaldehyde
(1-10)；4th rectifying column (1-D) tower top material (1-9) enters the 5th rectifying column (1-E), and the 5th rectifying column (1-E) tower top is adopted
It is out the material (1-11) of dimethoxym ethane and methanol；5th rectifying column (1-E) kettle material (1-12) enters dewatering unit (1-F),
Moisture (1-13) is removed；Material (1-14) after removing water enters the 6th rectifying column (1-G), and overhead extraction is the material of methanol
(1-15) and tower reactor are 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, 32 DEG C of tower top operation temperature, the
Two rectifying columns (1-B) operating pressure 80KPa, 86 DEG C of tower top operation temperature, third distillation column (1-C) operating pressure 1KPa, tower top
52 DEG C of operation temperature, the 4th rectifying column (1-D) operating pressure 80KPa, water (1-8) and material (1-4) mass ratio 0.2:1 are supplemented,
76 DEG C of tower top operation temperature, the 5th rectifying column (1-E) operating pressure 100KPa, 80 DEG C of tower top operation temperature, dewatering unit (1-F)
Using molecular sieve dehydration, the 6th rectifying column (1-G) operating pressure 100KPa, 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 389t/h mass fraction 42% or so.
Embodiment 2
The synthetic product mixture of 2400t/h PODEn forms as follows:
It is separated using the method and apparatus of embodiment 1, first rectifying column (1-A) operating pressure 200KPa, tower top operation temperature
52 DEG C, Second distillation column (1-B) operating pressure 120KPa of degree, 98 DEG C DEG C of tower top operation temperature, third distillation column (1-C) operation pressure
Power 50KPa, supplements water (1-8) and material (1- by 144 DEG C of tower top operation temperature, the 4th rectifying column (1-D) operating pressure 120KPa
4) mass ratio 0.8:1,96 DEG C of tower top operation temperature, the 5th rectifying column (1-E) operating pressure 200KPa, tower top operation temperature 61
DEG C, dewatering unit (1-F) is dehydrated using film, the 6th rectifying column (1-G) operating pressure 200KPa, and 82 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, 80t/h's
PODE3-5Qualified products, and recycled the formalin of 1089t/h mass fraction 20% or so.
Embodiment 3:
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, Second distillation column 2- by pipeline
The tower top outlet of B connects the feed inlet of the 4th rectifying column 2-D by pipeline, and the tower reactor outlet of Second distillation column 2-B passes through pipeline
The feed inlet of third distillation column 2-C is connected, the tower reactor discharge port of the 4th rectifying column 2-D connects the 5th rectifying column 2-E by pipeline
Feed inlet, the tower top discharge port of the 5th rectifying column 2-E 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 Second distillation column 2-B and enter the 4th rectifying column 2-D jointly, or be individually added into,
If supplement water is individually added into, need that supplement water feed inlet is additionally arranged on the 4th rectifying column 2-D.
Material 2-1 is that PODEn waits for refined material, and 2-2 is methyl formate, and 2-3 is without methyl formate to refined material,
2-4 is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material, 2-5 PODE3-10Material, 2-6 PODE3-5
Product material, 2-7 PODE6-10Material, 2-8 be pure water material, 2-9 be dimethoxym ethane and methanol material, 2-10 is first
Alcohol, formaldehyde, water, metaformaldehyde and PODE2Material, 2-11 PODE2, water and methanol material, 2-12 be formalin and
Micro metaformaldehyde material, 2-13 are water material, and 2-14 is methanol and PODE2Material, 2-15 are methanol charge, 2-16 PODE2
Material.
PODEn raw material (2-1) enters first rectifying column (2-A), and first rectifying column (2-A) overhead extraction is methyl formate
Material (2-2)；First rectifying column (2-A) kettle material (2-3) enters Second distillation column (2-B), Second distillation column (2-B) tower top
Extraction is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (2-4)；Second distillation column (2-B) kettle material
(2-5) enters third distillation column (2-C), and third distillation column (2-C) overhead extraction is PODE3-5Material (2-6) and tower reactor be
PODE6-10Material (2-7)；Second distillation column (2-B) tower top material (2-4) enters the 4th rectifying column (2-D), while the 4th essence
It evaporates tower (2-D) and introduces supplement water (2-8), the 4th rectifying column (2-D) overhead extraction is the material (2-9) of dimethoxym ethane and methanol；The
Four rectifying columns (2-D) kettle material (2-10) enters the 5th rectifying column (2-E), and the extraction of the 5th rectifying column (2-E) tower reactor is formaldehyde
The material (2-12) of aqueous solution and metaformaldehyde；5th rectifying column (2-E) tower top material (2-11) enters dewatering unit (2-F),
Moisture (2-13) is removed；Material (2-14) after removing water enters the 6th rectifying column (2-G), and overhead extraction is the material of methanol
(2-15) and tower reactor are PODE2Material (2-16).
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, first rectifying column (2-A) operating pressure 100KPa, 32 DEG C of tower top operation temperature, the second essence
Tower (2-B) operating pressure 100KPa is evaporated, 90 DEG C of tower top operation temperature, third distillation column (2-C) operating pressure 1KPa, tower top operates
52 DEG C of temperature, the 4th rectifying column (2-D) operating pressure 100KPa, supplement water (2-8) and material (2-4) mass ratio 0.5:1, tower top
40 DEG C of operation temperature, the 5th rectifying column (2-E) operating pressure 100KPa, 80 DEG C of tower top operation temperature, dewatering unit (2-F) uses
Adsorption dewatering, the 6th rectifying column (2-G) operating pressure 100KPa, 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 700t/h mass fraction 35% or so.
One kind proposed by the present invention is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE in charging2The essence of mixture
It evaporates and introduces the method and apparatus that supplement water realizes polymethoxy dimethyl ether separation and purification in tower, passed through preferred embodiment
Son is described, related technical personnel obviously can not depart from the content of present invention, in spirit and scope to knot as described herein
Structure and equipment are modified or appropriate changes and combinations, Lai Shixian the technology of the present invention.In particular, it should be pointed out that all similar
Replacement and change it is apparent to those skilled in the art, they are considered as being included in spirit of that invention, model
Enclose in content.
Claims (10)
1. a kind of method of separation and purification polymethoxy dimethyl ether, using multistage rectification, it is characterised in that: contract in charging for first
Aldehyde, methanol, water, formaldehyde, metaformaldehyde and PODE2Supplement water, formalin and trimerization first are introduced in the rectifying column of mixture
Aldehyde produces to realize the purpose of separating formaldehyde and metaformaldehyde from tower reactor.
2. the method for separation and purification polymethoxy dimethyl ether according to claim 1, it is characterised in that: supplement the addition of water
Amount is by weight 0.2:1~0.8:1 with the mass ratio of charging.
3. the method for separation and purification polymethoxy dimethyl ether according to claim 1, it is characterised in that: supplement water and charging
It is added or separates from the same feed inlet and be added from two feed inlets.
4. the method for separation and purification polymethoxy dimethyl ether according to claim 1, it is characterised in that: use six grades of essences
It evaporates, PODEn raw material enters first rectifying column, and first rectifying column overhead extraction is the material of methyl formate；First rectifying column tower reactor
Material enters Second distillation column, and Second distillation column overhead extraction is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2's
Mixed material；Second distillation column kettle material enters third distillation column, and third distillation column overhead extraction is PODE3-5Material, tower
Kettle is PODE6-10Material；Second distillation column tower top material enters the 4th rectifying column, while the 4th rectifying column introduces supplement water,
The additional amount for supplementing water is 0.2:1~0.8:1 with the mass ratio of charging by weight, and the extraction of the 4th tower bottom of rectifying tower is formalin
The mixed material of solution and metaformaldehyde；4th the top of the distillation column material enters the 5th rectifying column, the extraction of the 5th the top of the distillation column
For the mixed material of dimethoxym ethane and methanol；5th tower bottom of rectifying tower material enters dewatering unit, and moisture is removed；After removing water
Material enters the 6th rectifying column, and the extraction of the 6th the top of the distillation column is the material of methanol, tower reactor extraction is PODE2Material.
5. the method for separation and purification polymethoxy dimethyl ether according to claim 1, it is characterised in that: use six grades of essences
It evaporates, PODEn raw material enters first rectifying column, and first rectifying column overhead extraction is the material of methyl formate；First rectifying column tower reactor
Material enters Second distillation column, and Second distillation column overhead extraction is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2's
Mixed material；Second distillation column kettle material enters third distillation column, and third distillation column overhead extraction is PODE3-5Material, tower
Kettle extraction is PODE6-10Material；Second distillation column tower top material enters the 4th rectifying column, while the 4th rectifying column introduces supplement
Water, the additional amount for supplementing water is 0.2:1~0.8:1 with the mass ratio of charging by weight, and the extraction of the 4th the top of the distillation column is first
The mixed material of acetal 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 first
The mixed material of aldehyde aqueous solution and metaformaldehyde；5th the top of the distillation column material enters dewatering unit；Remove water after material into
Enter 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.
6. the method for separation and purification polymethoxy dimethyl ether according to claim 4 or 5, it is characterised in that: described is de-
Water unit uses film dehydration, molecular sieve dehydration, adsorption dewatering.
7. a kind of device of separation and purification polymethoxy dimethyl ether, including Multistage rectifying tower, it is characterised in that: contract in charging for first
Aldehyde, methanol, water, formaldehyde, metaformaldehyde and PODE2Setting supplement water water inlet in the rectifying column of mixture.
8. the device of separation and purification polymethoxy dimethyl ether according to claim 7, it is characterised in that: including six rectifying
Tower and a dewatering unit, the tower reactor outlet of first rectifying column connect the feed inlet of Second distillation column, the second rectifying by pipeline
The tower top outlet of tower connects the feed inlet of the 4th rectifying column by pipeline, and the tower reactor outlet of Second distillation column connects the by pipeline
The feed inlet of three rectifying columns, the tower top discharge port of the 4th rectifying column connect the feed inlet of the 5th rectifying column, the 5th essence by pipeline
The tower reactor discharge port for evaporating tower connects the feed inlet of dewatering unit by pipeline, and the discharge port of dewatering unit connects the 6th rectifying column
Feed inlet introduces supplement water in the 4th rectifying column, which is added from the feed inlet of the 4th rectifying column or in the 4th rectifying
Setting supplement water water inlet on tower.
9. the device of separation and purification polymethoxy dimethyl ether according to claim 7, it is characterised in that: including six rectifying
Tower and a dewatering unit, the tower reactor outlet of first rectifying column connect the feed inlet of Second distillation column, the second rectifying by pipeline
The tower top outlet of tower connects the feed inlet of the 4th rectifying column by pipeline, and the tower reactor outlet of Second distillation column connects the by pipeline
The feed inlet of three rectifying columns, the tower reactor discharge port of the 4th rectifying column connect the feed inlet of the 5th rectifying column, the 5th essence by pipeline
The tower top discharge port for evaporating tower connects the feed inlet of dewatering unit by pipeline, and the discharge port of dewatering unit connects the 6th rectifying column
Feed inlet introduces supplement water in the 4th rectifying column, which is added from the feed inlet of the 4th rectifying column or in the 4th rectifying
Setting supplement water water inlet on tower.
10. the device of separation and purification polymethoxy dimethyl ether according to claim 8 or claim 9, it is characterised in that: described is de-
Water unit is film dewatering unit, Molecular sieve dehydration units, adsorption dewatering unit.
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