CN109761766A - A kind of separating technology of the polymethoxy dimethyl ether system containing formaldehyde - Google Patents
A kind of separating technology of the polymethoxy dimethyl ether system containing formaldehyde Download PDFInfo
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Abstract
The present invention proposes a kind of separating technology of polymethoxy dimethyl ether system containing formaldehyde, using multistage rectification, introduces water comprising the rectifying column of formaldehyde in any level charging, formaldehyde is made to produce to realize the purpose of separating formaldehyde in form of an aqueous solutions 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 isolation technics of the synthetic product mixture of oxygroup dimethyl ether, point of especially a kind of polymethoxy dimethyl ether system containing formaldehyde
Separating process.
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.
The separating technology for the polymethoxy dimethyl ether system containing formaldehyde that the purpose of the present invention is to provide a kind of.Using distillation
Method is separated using methanol and formalin as the synthetic product of raw material PODEn, is refining to obtain suitable diesel component
PODEn, while recovery section raw material returns to above-mentioned first stage and second stage reaction process respectively.
A kind of separating technology of the polymethoxy dimethyl ether system containing formaldehyde is fed in any level and is wrapped using multistage rectification
Rectifying column containing formaldehyde introduces water, and formaldehyde is made to produce to realize the purpose of separating formaldehyde in form of an aqueous solutions from tower reactor.
It is added moreover, supplement water is added or separates from the same feed inlet with charging from two feed inlets.
Moreover, the additional amount of supplement water is by weight 0.2:1~1:1 with the mass ratio of charging.
A kind of multi-stage separation device of polymethoxy dimethyl ether, including Multistage rectifying tower include formaldehyde in any level charging
Rectifying column setting supplement water water inlet.
Moreover, the dewatering unit is film dehydration, molecular sieve dehydration, adsorption dewatering.
The separating technology of this polymethoxy dimethyl ether system containing formaldehyde, including six rectifying columns and a dewatering unit.
The program includes following 4 kinds of concomitant regimens:
Scheme one: supplement water (1-10) is introduced in the 5th rectifying column (1-E), the extraction of the 5th rectifying column (1-E) tower reactor is first
The material (1-12) of aldehyde aqueous solution and metaformaldehyde；5th rectifying column (1-E) tower top material (1-11) 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 methanol
Material (1-15) and tower reactor are PODE2Material (1-16)；
This programme includes following 3 separation process:
Process 1:PODEn raw material (1- (1) -1) enters first rectifying column (1- (1)-A), first rectifying column (1- (1)-A) tower
Top extraction is the material (1- (1) -2) of methyl formate；First rectifying column (1- (1)-A) kettle material (1- (1) -3) enters second
Rectifying column (1- (1)-B), Second distillation column (1- (1)-B) overhead extraction be dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and
PODE2Material (1- (1) -4)；Second distillation column (1- (1)-B) kettle material (1- (1) -5) enters third distillation column (1-
(1)-C), third distillation column (1- (1)-C) overhead extraction is PODE3-5Material (1- (1) -6) and tower reactor be PODE6-10Object
Expect (1- (1) -7)；Second distillation column (1- (1)-B) tower top material (1- (1) -4) enters the 4th rectifying column (1- (1)-D), and the 4th
Rectifying column (1- (1)-D) overhead extraction is the material (1- (1) -8) of dimethoxym ethane and methanol；4th rectifying column (1- (1)-D) tower reactor
Material (1- (1) -9) enters the 5th rectifying column (1-E)；
Process 2:PODEn raw material (1- (2) -1) enters first rectifying column (1- (2)-A), first rectifying column (1- (2)-A) tower
Top extraction is methyl formate, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (1- (2) -2)；First rectifying
Tower (1- (2)-A) kettle material (1- (2) -3) enters Second distillation column (1- (2)-B), and Second distillation column (1- (2)-B) tower top is adopted
It is out PODE3-5Material (1- (2) -4) and tower reactor be PODE6-10Material (1- (2) -5)；First rectifying column (1- (2)-A) tower
Push up material (1- (2) -2) enter third distillation column (1- (2)-C), third distillation column (1- (2)-C) overhead extraction be methyl formate,
The material (1- (2) -6) of dimethoxym ethane and methanol；Third distillation column (1- (2)-C) tower top material (1- (2) -6) enters the 4th rectifying
Tower (1- (2)-D), the 4th rectifying column (1- (2)-D) overhead extraction is the material (1- (2) -8) of methyl formate and tower reactor is first contracting
The material (1- (2) -9) of aldehyde and methanol；Third distillation column (1- (2)-C) kettle material (1- (2) -7) enters the 5th rectifying column (1-
E)；
Process 3:PODEn raw material (1- (3) -1) enters first rectifying column (1- (3)-A), first rectifying column (1- (3)-A) tower
Top extraction is methyl formate, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (1- (3) -2)；First rectifying
Tower (1- (3)-A) kettle material (1- (3) -3) enters Second distillation column (1- (3)-B), and Second distillation column (1- (3)-B) tower top is adopted
It is out PODE3-5Material (1- (3) -4) and tower reactor be PODE6-10Material (1- (3) -5)；First rectifying column (1- (3)-A) tower
It pushes up material (1- (3) -2) and enters third distillation column (1- (3)-C), third distillation column (1- (3)-C) overhead extraction is methyl formate
Material (1- (3) -6)；Third distillation column (1- (3)-C) kettle material (1- (3) -7) enters the 4th rectifying column (1- (3)-D),
4th rectifying column (1- (3)-D) overhead extraction is the material (1- (3) -8) of dimethoxym ethane and methanol；4th rectifying column (1- (3)-D)
Kettle material (1- (3) -9) enters the 5th rectifying column (1-E)；
Two: PODEn raw material of scheme (2-1) enters first rectifying column (2-A), and first rectifying column (2-A) overhead extraction is first
The material (2-2) of sour methyl esters；First rectifying column (2-A) kettle material (2-3) enters Second distillation column (2-B), Second distillation column
(2-B) overhead 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 is PODE6-10Material (2-7)；Second distillation column (2-B) tower top material (2-4) enters the 4th rectifying column, while the 4th
Rectifying column introduces supplement water (2-8)；5th rectifying tower top or tower bottoms enter film dewatering unit (2-F), and moisture (2-13) is taken off
It removes；Material (2-14) after removing water enters the 6th rectifying column (2-G), and overhead extraction is the material (2-15) of methanol and tower reactor is
PODE2Material (2-16)；
This programme includes following 2 separation process:
The extraction of 1: the four rectifying column of process (2- (1)-D) tower reactor is the material (2- (1)-of formalin and metaformaldehyde
10)；4th rectifying column (2- (1)-D) tower top material (2- (1) -9) enters the 5th rectifying column (2- (1)-E), the 5th rectifying column (2-
(1)-E) overhead extraction be dimethoxym ethane and methanol material (2- (1) -11), the 5th rectifying tower kettle liquid (2- (1) -12) enters de-
Water unit (2-F)；
2: the four rectifying column of process (2- (2)-D) overhead extraction is the material (2- (2) -9) of dimethoxym ethane and methanol；4th essence
Tower (2- (2)-D) kettle material (2- (2) -10) is evaporated into the 5th rectifying column (2- (2)-E), the 5th rectifying column (2- (2)-E) tower
Kettle extraction is the material (2- (2) -12) of formalin and metaformaldehyde；5th rectifying column (2- (2)-E) tower top material (2-
(2) -11) enter dewatering unit (2-F)；
Three: PODEn raw material of scheme (3-1) enters first rectifying column (3-A), and first rectifying column (3-A) overhead extraction is first
Sour methyl esters, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (3-2)；First rectifying column (3-A) kettle material
(3-3) enters Second distillation column (3-B), and Second distillation column (3-B) overhead extraction is 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, while third distillation column
Introduce supplement water (3-6)；5th rectifying tower top or tower bottoms enter film dewatering unit (3-F), and moisture (3-13) is removed；Removing
Material (3-14) after water enters the 6th rectifying column (3-G), and overhead extraction is the material (3-15) of methanol and tower reactor is PODE2's
Material (3-16)；
This programme includes following 5 separation process:
Process 1: the extraction of third distillation column (3- (1)-C) tower reactor is the material (3- (1)-of formalin and metaformaldehyde
8)；Third distillation column (3- (1)-C) tower top material (3- (1) -7) enters the 4th rectifying column (3- (1)-D), the 4th rectifying column (3-
(1)-D) overhead extraction be methyl formate material (3- (1) -9)；4th rectifying column (3- (1)-D) kettle material (3- (1) -10)
Into the 5th rectifying column (3- (1)-E), the 5th rectifying column (3- (1)-E) overhead extraction is the material (3- of dimethoxym ethane and methanol
(1)-11)；5th rectifying column (3- (1)-E) kettle material (3- (1) -12) enters dewatering unit (3-F)；
Process 2: the extraction of third distillation column (3- (2)-C) tower reactor is the material (3- (2)-of formalin and metaformaldehyde
8)；Third distillation column (3- (2)-C) tower top material (3- (2) -7) enters the 4th rectifying column (3- (2)-D), the 4th rectifying column (3-
(2)-D) overhead extraction be methyl formate, dimethoxym ethane and methanol material (3- (2) -9)；4th rectifying column (3- (2)-D) tower top
Material (3- (2) -9) enters the 5th rectifying column (3- (2)-E), and the 5th rectifying column (3- (2)-E) overhead extraction is methyl formate
Material (3- (2) -11) and tower reactor are the material (3- (2) -12) of dimethoxym ethane and methanol；4th rectifying column (3- (2)-D) tower reactor object
Expect that (3- (2) -10) enters dewatering unit (3-F)；
Process 3: third distillation column (3- (3)-C) overhead extraction is the material (3- (3)-of methyl formate, dimethoxym ethane and methanol
7)；Third distillation column (3- (3)-C) tower top material (3- (3) -7) enters the 4th rectifying column (3- (3)-D), the 4th rectifying column (3-
(3)-D) overhead extraction be methyl formate material (3- (3) -9) and tower reactor be dimethoxym ethane and methanol material (3- (3) -10)；
Third distillation column (3- (3)-C) kettle material (3- (3) -8) enters the 5th rectifying column (3- (3)-E), the 5th rectifying column (3- (3) -
E) tower reactor extraction is the material (3- (3) -12) of formalin and metaformaldehyde；5th rectifying column (3- (3)-E) tower top material
(3- (3) -11) enters dewatering unit (3-F)；
Process 4: third distillation column (3- (4)-C) overhead extraction is the material (3- (4) -7) of methyl formate；Third distillation column
(3- (4)-C) kettle material (3- (4) -8) enters the 4th rectifying column (3- (4)-D), the 4th rectifying column (3- (4)-D) overhead extraction
For the material (3- (4) -9) of dimethoxym ethane and methanol；4th rectifying column (3- (4)-D) kettle material (3- (4) -8) enters the 5th essence
It evaporates tower (3- (4)-E), the extraction of the 5th rectifying column (3- (4)-E) tower reactor is the material (3- (4)-of formalin and metaformaldehyde
12)；5th rectifying column (3- (4)-E) tower top material (3- (4) -11) enters dewatering unit (3-F)；
Process 5: third distillation column (3- (5)-C) overhead extraction is the material (3- (5) -7) of methyl formate；Third distillation column
(3- (5)-C) kettle material (3- (5) -8) enters the 4th rectifying column (3- (5)-D), the extraction of the 4th rectifying column (3- (5)-D) tower reactor
For the material (3- (5) -10) of formalin and metaformaldehyde；4th rectifying column (3- (5)-D) tower top material (3- (5) -9) into
Enter the 5th rectifying column (3- (5)-E), the 5th rectifying column (3- (5)-E) overhead extraction is the material (3- (5)-of dimethoxym ethane and methanol
11)；5th rectifying column (3- (5)-E) kettle material (3- (5) -12) enters dewatering unit (3-F)；
Four: PODEn raw material of scheme (4-1) enters first rectifying column (4-A), while first rectifying column (4-A) introduces supplement
Water (4-2), first rectifying column (4-A) overhead extraction are methyl formate, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2
Material (4-3)；First rectifying column (4-A) kettle material (4-4) enters Second distillation column (4-B), Second distillation column (4-B) tower
Top extraction is PODE3-5Material (4-5) and tower reactor be PODE6-10Material (4-6)；First rectifying column (4-A) tower top material
(4-3) enters third distillation column；5th rectifying tower top or tower bottoms enter film dewatering unit (4-F), and moisture (4-13) is removed；
Material (4-14) after removing water enters the 6th rectifying column (4-G), and overhead extraction is the material (4-15) of methanol and tower reactor is
PODE2Material (4-16)；
This programme includes following 5 separation process:
Process 1: the extraction of third distillation column (4- (1)-C) tower reactor is the material (4- (1)-of formalin and metaformaldehyde
8)；Third distillation column (4- (1)-C) tower top material (4- (1) -7) enters the 4th rectifying column (4- (1)-D), the 4th rectifying column (4-
(1)-D) overhead extraction be methyl formate material (4- (1) -9)；4th rectifying column (4- (1)-D) kettle material (4- (1) -10)
Into the 5th rectifying column (4- (1)-E), the 5th rectifying column (4- (1)-E) overhead extraction is the material (4- of dimethoxym ethane and methanol
(1)-11)；5th rectifying column (4- (1)-E) kettle material (4- (1) -12) enters dewatering unit (4-F)；
Process 2: the extraction of third distillation column (4- (2)-C) tower reactor is the material (4- (2)-of formalin and metaformaldehyde
8)；Third distillation column (4- (2)-C) tower top material (4- (2) -7) enters the 4th rectifying column (4- (2)-D), the 4th rectifying column (4-
(2)-D) overhead extraction be methyl formate, dimethoxym ethane and methanol material (4- (2) -9)；4th rectifying column (4- (2)-D) tower top
Material (4- (2) -9) enters the 5th rectifying column (4- (2)-E), and the 5th rectifying column (4- (2)-E) overhead extraction is methyl formate
Material (4- (2) -11) and tower reactor are the material (4- (2) -12) of dimethoxym ethane and methanol；4th rectifying column (4- (2)-D) tower reactor object
Expect that (4- (2) -10) enters dewatering unit (4-F)；
Process 3: third distillation column (4- (3)-C) overhead extraction is the material (4- (3)-of methyl formate, dimethoxym ethane and methanol
7)；Third distillation column (4- (3)-C) tower top material (4- (3) -7) enters the 4th rectifying column (4- (3)-D), the 4th rectifying column (4-
(3)-D) overhead extraction be methyl formate material (4- (3) -9) and tower reactor be dimethoxym ethane and methanol material (4- (3) -10)；
Third distillation column (4- (3)-C) kettle material (4- (3) -8) enters the 5th rectifying column (4- (3)-E), the 5th rectifying column (4- (3) -
E) tower reactor extraction is the material (4- (3) -12) of formalin and metaformaldehyde；5th rectifying column (4- (3)-E) tower top material
(4- (3) -11) enters dewatering unit (4-F)；
Process 4: third distillation column (4- (4)-C) overhead extraction is the material (4- (4) -7) of methyl formate；Third distillation column
(4- (4)-C) kettle material (4- (4) -8) enters the 4th rectifying column (4- (4)-D), the 4th rectifying column (4- (4)-D) overhead extraction
For the material (4- (4) -9) of dimethoxym ethane and methanol；4th rectifying column (4- (4)-D) kettle material (4- (4) -10) enters the 5th essence
It evaporates tower (4- (4)-E), the extraction of the 5th rectifying column (4- (4)-E) tower reactor is the material (4- (4)-of formalin and metaformaldehyde
12)；5th rectifying column (4- (4)-E) tower top material (4- (4) -11) enters dewatering unit (4-F)；
Process 5: third distillation column (4- (5)-C) overhead extraction is the material (4- (5) -7) of methyl formate；Third distillation column
(4- (5)-C) kettle material (4- (5) -8) enters the 4th rectifying column (4- (5)-D), the extraction of the 4th rectifying column (4- (5)-D) tower reactor
For the material (4- (5) -10) of formalin and metaformaldehyde；4th rectifying column (4- (5)-D) tower top material (4- (5) -9) into
Enter the 5th rectifying column (4- (5)-E), the 5th rectifying column (4- (5)-E) overhead extraction is the material (4- (5)-of dimethoxym ethane and methanol
11)；5th rectifying column (4- (5)-E) kettle material (4- (5) -12) enters dewatering unit (4-F)；
The operating pressure of the 5th rectifying column (1-E) is 80-120KPa in scheme one, and tower top operation temperature is 70-120 DEG C,
Supplementing water (1-10) content is by weight 0.3:1~1:1, dewatering unit (1- with the mass ratio of the 5th rectifying column (1-E) charging
F film dehydration, molecular sieve dehydration, adsorption dewatering) be can be, the operating pressure of the 6th rectifying column (1-G) is 100-200KPa, tower top
Operation temperature is 60-90 DEG C；
The operating pressure of first rectifying column (1- (1)-A) is 100-200KPa in process 1, and tower top operation temperature is 30-60
DEG C, the operating pressure of Second distillation column (1- (1)-B) is 80-120KPa, and tower top operation temperature is 70-100 DEG C, third distillation column
The operating pressure of (1- (1)-C) is 1-50KPa, and the operation temperature of tower top is 50-150 DEG C, the behaviour of the 4th rectifying column (1- (1)-D)
Making pressure is 100-200KPa, and tower top operation temperature is 35-70 DEG C；
The operating pressure of first rectifying column (1- (2)-A) is 80-120KPa in process 2, and tower top operation temperature is 70-100
DEG C, the operating pressure of Second distillation column (1- (2)-B) is 1-50KPa, and the operation temperature of tower top is 50-150 DEG C, third distillation column
The operating pressure of (1- (2)-C) is 100-200KPa, and tower top operation temperature is 35-70 DEG C, the behaviour of the 4th rectifying column (1- (2)-D)
Making pressure is 100-200KPa, and tower top operation temperature is 30-60 DEG C；
The operating pressure of first rectifying column (1- (3)-A) is 80-120KPa in process 3, and tower top operation temperature is 70-100
DEG C, the operating pressure of Second distillation column (1- (3)-B) is 1-50KPa, and the operation temperature of tower top is 50-150 DEG C, third distillation column
The operating pressure of (1- (3)-C) is 100-200KPa, and tower top operation temperature is 30-60 DEG C, the behaviour of the 4th rectifying column (1- (3)-D)
Making pressure is 100-200KPa, and tower top operation temperature is 35-70 DEG C；
The operating pressure of first rectifying column (2-A) is 100-200KPa in scheme two, and tower top operation temperature is 30-60 DEG C,
The operating pressure of Second distillation column (2-B) is 80-120KPa, and tower top operation temperature is 70-100 DEG C, third distillation column (2-C)
Operating pressure is 1-50KPa, and the operation temperature of tower top is 50-150 DEG C, supplement water (2-8) content by weight with material (2-4)
Mass ratio be 0.2:1~0.8:1, dewatering unit (2-F) can be film dehydration, molecular sieve dehydration, adsorption dewatering, the 6th rectifying
The operating pressure of tower (2-G) is 100-200KPa, and tower top operation temperature is 60-90 DEG C；
The operating pressure of the 4th rectifying column (2- (1)-D) is 80-120KPa in process 1, and tower top operation temperature is 70-120
DEG C, the operating pressure of the 5th rectifying column (2- (1)-E) is 100-200KPa, and tower top operation temperature is 35-70 DEG C；
The operating pressure of the 4th rectifying column (2- (2)-D) is 100-200KPa in process 2, and tower top operation temperature is 35-70
DEG C, the operating pressure of the 5th rectifying column (2- (2)-E) is 80-120KPa, and tower top operation temperature is 70-120 DEG C；
The operating pressure of first rectifying column (3-A) is 80-120KPa in scheme three, and tower top operation temperature is 70-100 DEG C,
The operating pressure of Second distillation column (3-B) is 1-50KPa, and the operation temperature of tower top is 50-150 DEG C, supplement water (3-6) content with
The mass ratio of poidometer and material (3-2) are 0.2:1~1:1, and dewatering unit (3-F) can be film dehydration, molecular sieve dehydration, suction
Attached dehydration, the operating pressure of the 6th rectifying column (3-G) are 100-200KPa, and tower top operation temperature is 60-90 DEG C；
The operating pressure of third distillation column (3- (1)-C) is 80-120KPa in process 1, and tower top operation temperature is 70-120
DEG C, the operating pressure of the 4th rectifying column (3- (1)-D) is 100-200KPa, and tower top operation temperature is 30-60 DEG C, the 5th rectifying column
The operating pressure of (3- (1)-E) is 100-200KPa, and tower top operation temperature is 35-70 DEG C；
The operating pressure of third distillation column (3- (2)-C) is 80-120KPa in process 2, and tower top operation temperature is 70-120
DEG C, the operating pressure of the 4th rectifying column (3- (2)-D) is 100-200KPa, and tower top operation temperature is 35-70 DEG C, the 5th rectifying column
The operating pressure of (3- (2)-E) is 100-200KPa, and tower top operation temperature is 30-60 DEG C；
The operating pressure of third distillation column (3- (3)-C) is 100-200KPa in process 3, and tower top operation temperature is 35-70
DEG C, the operating pressure of the 4th rectifying column (3- (3)-D) is 100-200KPa, and tower top operation temperature is 30-60 DEG C, the 5th rectifying column
The operating pressure of (3- (3)-E) is 80-120KPa, and tower top operation temperature is 70-120 DEG C；
The operating pressure of third distillation column (3- (4)-C) is 100-200KPa in process 4, and tower top operation temperature is 30-60
DEG C, the operating pressure of the 4th rectifying column (3- (4)-D) is 100-200KPa, and tower top operation temperature is 35-70 DEG C, the 5th rectifying column
The operating pressure of (3- (4)-E) is 80-120KPa, and tower top operation temperature is 70-120 DEG C；
Process 5: the operating pressure of third distillation column (3- (5)-C) is 100-200KPa, and tower top operation temperature is 30-60
DEG C, the operating pressure of the 4th rectifying column (3- (5)-D) is 80-120KPa, and tower top operation temperature is 70-120 DEG C, the 5th rectifying column
The operating pressure of (3- (5)-E) is 100-200KPa, and tower top operation temperature is 35-70 DEG C；
The operating pressure of first rectifying column (4-A) is 80-120KPa in scheme four, and supplement water (4-2) content is by weight
Mass ratio with material (4-1) is 0.2:1~1:1, and tower top operation temperature is 70-100 DEG C, the operation of Second distillation column (4-B)
Pressure is 1-50KPa, and the operation temperature of tower top is 50-150 DEG C；Dewatering unit (4-F) can be film dehydration, molecular sieve dehydration,
Adsorption dewatering, the operating pressure of the 6th rectifying column (4-G) are 100-200KPa, and tower top operation temperature is 60-90 DEG C；
The operating pressure of third distillation column (4- (1)-C) is 80-120KPa in process 1, and tower top operation temperature is 70-120
DEG C, the operating pressure of the 4th rectifying column (4- (1)-D) is 100-200KPa, and tower top operation temperature is 30-60 DEG C, the 5th rectifying column
The operating pressure of (4- (1)-E) is 100-200KPa, and tower top operation temperature is 35-70 DEG C；
The operating pressure of third distillation column (4- (2)-C) is 80-120KPa in process 2, and tower top operation temperature is 70-120
DEG C, the operating pressure of the 4th rectifying column (4- (2)-D) is 100-200KPa, and tower top operation temperature is 35-70 DEG C, the 5th rectifying column
The operating pressure of (4- (2)-E) is 100-200KPa, and tower top operation temperature is 30-60 DEG C；
The operating pressure of third distillation column (4- (3)-C) is 100-200KPa in process 3, and tower top operation temperature is 35-70
DEG C, the operating pressure of the 4th rectifying column (4- (3)-D) is 100-200KPa, and tower top operation temperature is 30-60 DEG C, the 5th rectifying column
The operating pressure of (4- (3)-E) is 80-120KPa, and tower top operation temperature is 70-120 DEG C；
The operating pressure of third distillation column (4- (4)-C) is 100-200KPa in process 4, and tower top operation temperature is 30-60
DEG C, the operating pressure of the 4th rectifying column (4- (4)-D) is 100-200KPa, and tower top operation temperature is 35-70 DEG C, the 5th rectifying column
The operating pressure of (4- (4)-E) is 80-120KPa, and tower top operation temperature is 70-120 DEG C；
The operating pressure of third distillation column (4- (5)-C) is 100-200KPa in process 5, and tower top operation temperature is 30-60
DEG C, the operating pressure of the 4th rectifying column (4- (5)-D) is 80-120KPa, and tower top operation temperature is 70-120 DEG C, the 5th rectifying column
The operating pressure of (4- (5)-E) is 100-200KPa, and tower top operation temperature is 35-70 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, and proposes a kind of containing first
The separating technology of the polymethoxy dimethyl ether system of aldehyde, the unique distinction of method are as follows:
1. although can reduce methyl formate after purified separation methyl formate is few as side reaction product amount and produce
Accumulation in object.
2. 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.
3. the reaction unit that unreacted dimethoxym ethane is back to dimethoxym ethane and formaldehyde catalyzes and synthesizes PODEn can be recycled, rationally
Unreacting material is recycled, raw material availability is improved.
4. 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.
5. material PODE2, first alcohol and water by dewatering unit and the 6th rectifying column PODE can be obtained2By-product product, mentions
High economic benefit.
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.
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- (1)-A is first rectifying column in Fig. 1, and 1- (1)-B is Second distillation column, and 1- (1)-C is third distillation column, 1-
(1)-D is the 4th rectifying column, and 1-E is the 5th rectifying column, and 1-F is dewatering unit, the 6th rectifying column of 1-G.
First rectifying column 1- (1)-A tower reactor outlet by pipeline connection Second distillation column 1- (1)-B feed inlet, second
The tower top outlet of rectifying column 1- (1)-B connects the feed inlet of the 4th rectifying column 1- (1)-D, Second distillation column 1- (1)-by pipeline
The tower reactor outlet of B connects the feed inlet of third distillation column 1- (1)-C, the tower reactor discharging of the 4th rectifying column 1- (1)-D by pipeline
The feed inlet of the 5th rectifying column 1-E of mouth connection, the tower top discharge port of the 5th rectifying column 1-E pass through pipeline and connect dewatering unit 1-F
Feed inlet, the discharge port of dewatering unit 1-F connects the feed inlet of the 6th rectifying column 1-G.
Supplement water can discharge with the tower reactor of the 4th rectifying column 1- (1)-D enters the 5th rectifying column 1-E jointly, or individually adds
Enter, if supplement water is individually added into, needs that supplement water feed inlet is additionally arranged on the 5th rectifying column 1-E.
Material 1- (1) -1 is that PODEn waits for that refined material, 1- (1) -2 are methyl formate, and 1- (1) -3 is without methyl formate
To refined material, 1- (1) -4 is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material, 1- (1) -5 is
PODE3-10Material, 1- (1) -6 be PODE3-5Product material, 1- (1) -7 be PODE6-10Material, 1- (1) -8 be dimethoxym ethane
With the material of methanol, 1- (1) -9 is methanol, formaldehyde, water, metaformaldehyde and PODE2Material, 1-10 be pure water material, 1-11
For PODE2, water and methanol charge, 1-12 is containing formalin and metaformaldehyde, and 1-13 is water material, 1-14 be methanol and
PODE2Material, 1-15 are methanol charge, 1-16 PODE2Material.
Process 1:PODEn raw material (1- (1) -1) enters first rectifying column (1- (1)-A), first rectifying column (1- (1)-A) tower
Top extraction is the material (1- (1) -2) of methyl formate；First rectifying column (1- (1)-A) kettle material (1- (1) -3) enters second
Rectifying column (1- (1)-B), Second distillation column (1- (1)-B) overhead extraction be dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and
PODE2Material (1- (1) -4)；Second distillation column (1- (1)-B) kettle material (1- (1) -5) enters third distillation column (1-
(1)-C), third distillation column (1- (1)-C) overhead extraction is PODE3-5Material (1- (1) -6) and tower reactor be PODE6-10Object
Expect (1- (1) -7)；Second distillation column (1- (1)-B) tower top material (1- (1) -4) enters the 4th rectifying column (1- (1)-D), and the 4th
Rectifying column (1- (1)-D) overhead extraction is the material (1- (1) -8) of dimethoxym ethane and methanol；4th rectifying column (1- (1)-D) tower reactor
Material (1- (1) -9) enters the 5th rectifying column (1-E).Supplement water (1-10), the 5th rectifying column are introduced in the 5th rectifying column (1-E)
The extraction of (1-E) tower reactor is the material (1-12) of formalin and metaformaldehyde；5th rectifying column (1-E) tower top material (1-11)
Into dewatering unit (1-F), moisture (1-13) is removed；Material (1-14) after removing water enters the 6th rectifying column (1-G), tower
The material (1-15) and tower reactor that top extraction is methanol 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 one process 1 of this method scheme, first rectifying column (1- (1)-A) operating pressure 100KPa, tower top operation
32 DEG C of temperature, Second distillation column (1- (1)-B) operating pressure 80KPa, 86 DEG C of tower top operation temperature, third distillation column (1- (1)-
C) operating pressure 1KPa, 52 DEG C of tower top operation temperature, the 4th rectifying column (1- (1)-D) operating pressure 100KPa, tower top operation temperature
40 DEG C, the 5th rectifying column (1-E) operating pressure 80KPa of degree, supplement water (1-10) amount and material (1- (1) -9) mass ratio 0.3:1,
80 DEG C of tower top operation temperature, dewatering unit (1-F) uses molecular sieve dehydration, the 6th rectifying column (1-G) operating pressure 100KPa, tower
64 DEG C of operation temperature of top.
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 327t/h mass fraction 50% 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- (1)-D is the 4th essence
Tower is evaporated, 2- (1)-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- (1)-D by pipeline, and the tower reactor outlet of Second distillation column 2-B passes through
Pipeline connects the feed inlet of third distillation column 2-C, and the tower top discharge port of the 4th rectifying column 2- (1)-D passes through the 5th essence of pipeline connection
Evaporate the feed inlet of tower 2- (1)-E, the tower reactor discharge port of the 5th rectifying column 2- (1)-E by pipeline connect dewatering unit 2-F into
Material mouth, the discharge port of dewatering unit 2-F connect the feed inlet of the 6th rectifying column 2-G.
Supplement water can discharge with the tower top of Second distillation column 2-B enters the 4th rectifying column 2- (1)-D jointly, or individually adds
Enter, if supplement water is individually added into, needs in the upper additional setting supplement water feed inlet of the 4th rectifying column 2- (1)-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- (1) -9 be dimethoxym ethane, methanol, formaldehyde, water, trimerization
Formaldehyde and PODE2Material, 2- (1) -10 is formalin and metaformaldehyde material, and 2- (1) -11 is dimethoxym ethane and methanol
Material, 2- (1) -12 are PODE2, water and methanol charge, 2-13 is water material, and 2-14 is methanol and PODE2Material, 2-15 are first
Alcohol material, 2-16 PODE2Material.
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, while the 4th rectifying column
Introduce supplement water (2-8)；The extraction of 4th rectifying column (2- (1)-D) tower reactor is the material (2- of formalin and metaformaldehyde
(1)-10)；4th rectifying column (2- (1)-D) tower top material (2- (1) -9) enters the 5th rectifying column (2- (1)-E), the 5th rectifying
Tower (2- (1)-E) overhead extraction is the material (2- (1) -11) of dimethoxym ethane and methanol, the 5th rectifying tower kettle liquid (2- (1) -12)
Into dewatering unit (2-F)；Moisture (2-13) is removed；Material (2-14) after removing water enters the 6th rectifying column (2-G), tower
The material (2-15) and tower reactor that top extraction is methanol are PODE2Material (2-16).
The synthetic product mixture of 2400t/h PODEn forms as follows:
It is separated using two process 1 of this method scheme, first rectifying column (2-A) operating pressure 200KPa, tower top operation temperature
52 DEG C, Second distillation column (2-B) operating pressure 120KPa, 98 DEG C of tower top operation temperature, third distillation column (2-C) operating pressure
50KPa, 144 DEG C of tower top operation temperature, the 4th rectifying column (2- (1)-D) operating pressure 120KPa, supplement water (2-8) is measured and material
(2-4) mass ratio 0.8:1,96 DEG C of tower top operation temperature, the 5th rectifying column (2- (1)-E) operating pressure 200KPa, tower top operation
61 DEG C of temperature, dewatering unit (2-F) uses adsorption dewatering, the 6th rectifying column (2-G) operating pressure 200KPa, tower top operation temperature
82℃。
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 622t/h mass fraction 35% or so.
Embodiment 3
3-A is first rectifying column in Fig. 3, and 3-B is Second distillation column, and 3- (1)-C is third distillation column, and 3- (1)-D is the
Four rectifying columns, 3- (1)-E are 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- (1)-C, the tower top outlet of third distillation column 3- (1)-C by pipeline
The feed inlet of the 4th rectifying column 3- (1)-D is connected by pipeline, the tower reactor discharge port of the 4th rectifying column 3- (1)-D is connected by pipeline
The feed inlet of the 5th rectifying column 3- (1)-E is connect, the tower reactor discharge port of the 5th rectifying column 3- (1)-E connects dewatering unit by pipeline
The feed inlet of 3-F, the discharge port of dewatering unit 3-F connect the feed inlet of the 6th rectifying column 3-G.
Supplement water can discharge with the tower top of first rectifying column 3-A enters third distillation column 3- (1)-C jointly, or individually adds
Enter, if supplement water is individually added into, needs in the upper additional setting supplement water feed inlet of third distillation column 3- (1)-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- (1) -7 be methyl formate,
Dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material, 3- (1) -8 be formalin and metaformaldehyde material,
3- (1) -9 is methyl formate material, and 3- (1) -10 is dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material, 3-
(1) -11 is the material of dimethoxym ethane and methanol, and 3- (1) -12 is PODE2, water and methanol material, 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) enter first rectifying column (3-A), first rectifying column (3-A) overhead extraction be methyl formate,
Dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material (3-2)；First rectifying column (3-A) kettle material (3-3) into
Enter Second distillation column (3-B), Second distillation column (3-B) overhead extraction is PODE3-5Material (3-4) and tower reactor be PODE6-10's
Material (3-5)；First rectifying column (3-A) tower top material (3-2) enters third distillation column, while third distillation column introduces supplement water
(3-6)；The extraction of third distillation column (3- (1)-C) tower reactor is the material (3- (1) -8) of formalin and metaformaldehyde；Third essence
Tower (3- (1)-C) tower top material (3- (1) -7) is evaporated into the 4th rectifying column (3- (1)-D), the 4th rectifying column (3- (1)-D) tower top
Extraction is the material (3- (1) -9) of methyl formate；4th rectifying column (3- (1)-D) kettle material (3- (1) -10) enters the 5th essence
It evaporates tower (3- (1)-E), the 5th rectifying column (3- (1)-E) overhead extraction is the material (3- (1) -11) of dimethoxym ethane and methanol；5th
Rectifying column (3- (1)-E) kettle material (3- (1) -12) enters dewatering unit (3-F), and moisture (3-13) is removed；After removing water
Material (3-14) enter the 6th rectifying column (3-G), overhead extraction is the material (3-15) of methanol and tower reactor is 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 three process 1 of this method scheme, first rectifying column (3-A) operating pressure 100KPa, tower top operation temperature
90 DEG C, Second distillation column (3-B) operating pressure 1KPa, 52 DEG C of tower top operation temperature, third distillation column (3- (1)-C) operating pressure
100KPa, supplement water (3-6) amount and material (3-2) mass ratio 0.4:1,80 DEG C of tower top operation temperature, the 4th rectifying column (3- (1)-
D) operating pressure 100KPa, 32 DEG C of tower top operation temperature, the 5th rectifying column (3- (1)-E) operating pressure 100KPa, tower top operation
40 DEG C of temperature, dewatering unit (3-F) uses molecular sieve dehydration, the 6th rectifying column (3-G) operating pressure 100KPa, tower top operation temperature
64 DEG C of degree.
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 1225t/h mass fraction 20% or so.
Embodiment 4
4-A is first rectifying column in Fig. 4, and 4-B is Second distillation column, and 4- (1)-C is third distillation column, and 4- (1)-D is the
Four rectifying columns, 4- (1)-E are 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- (1)-C, the tower top outlet of third distillation column 4- (1)-C by pipeline
The feed inlet of the 4th rectifying column 4- (1)-D is connected by pipeline, the tower reactor discharge port of the 4th rectifying column 4- (1)-D is connected by pipeline
The feed inlet of the 5th rectifying column 4- (1)-E is connect, the tower reactor discharge port of the 5th rectifying column 4- (1)-E connects dewatering unit by pipeline
The feed inlet of 4-F, the discharge port of dewatering unit 4-F connect the feed inlet of the 6th rectifying column 4-G.
Supplement water can wait for that refined material enters first rectifying column 4-A jointly with PODEn, or be individually added into, if supplement
Water is individually added into, and needs that supplement water feed inlet is additionally arranged on first rectifying column 4-A.
Material 4-1 is that PODEn waits for that refined material, 4-2 are pure water material, and 4-3 is without PODE3-10To refined material,
4-4 is PODE3-10Material, 4-5 PODE3-5Product material, 4-6 PODE6-10Material, 4- (1) -7 be methyl formate,
Dimethoxym ethane, methanol, water and PODE2Material, 4- (1) -8 be formalin and metaformaldehyde material, 4- (1) -9 be formic acid
Methyl esters, 4- (1) -10 are dimethoxym ethane, methanol, water and PODE2Material, 4- (1) -11 be dimethoxym ethane and methanol material, 4-
(1) -12 is PODE2, water and methanol material, 4-13 be water material, 4-14 be methanol and PODE2Material, 4-15 are methanol object
Material, 4-16 PODE2Material.
PODEn raw material (4-1) enters first rectifying column (4-A), while first rectifying column (4-A) introduces supplement water (4-2),
First rectifying column (4-A) overhead extraction is methyl formate, dimethoxym ethane, methanol, water, formaldehyde, metaformaldehyde and PODE2Material
(4-3)；First rectifying column (4-A) kettle material (4-4) enters Second distillation column (4-B), Second distillation column (4-B) overhead extraction
For PODE3-5Material (4-5) and tower reactor be PODE6-10Material (4-6)；First rectifying column (4-A) tower top material (4-3) into
Enter third distillation column (4- (1)-C)；The extraction of third distillation column (4- (1)-C) tower reactor is the material of formalin and metaformaldehyde
(4-(1)-8)；Third distillation column (4- (1)-C) tower top material (4- (1) -7) enters the 4th rectifying column (4- (1)-D), the 4th essence
Evaporate the material (4- (1) -9) that tower (4- (1)-D) overhead extraction is methyl formate；4th rectifying column (4- (1)-D) kettle material (4-
(1) -10) enter the 5th rectifying column (4- (1)-E), the 5th rectifying column (4- (1)-E) overhead extraction is the object of dimethoxym ethane and methanol
Expect (4- (1) -11)；5th rectifying column (4- (1)-E) kettle material (4- (1) -12) enters dewatering unit (4-F)；Moisture (4-
13) it is removed；Material (4-14) after removing water enters the 6th rectifying column (4-G), and overhead extraction is the material (4-15) of methanol
It is PODE with tower reactor2Material (4-16).
The synthetic product mixture of 2400t/h PODEn forms as follows:
It is separated using four process 1 of this method scheme, first rectifying column (4-A) operating pressure 100KPa, supplement water (4-2) amount
With material (4-1) mass ratio 0.8:1,90 DEG C of tower top operation temperature, Second distillation column (4-B) operating pressure 1KPa, tower top is operated
52 DEG C of temperature, third distillation column (4- (1)-C) operating pressure 100KPa, 80 DEG C of tower top operation temperature, the 4th rectifying column (4- (1)-
D) operating pressure 100KPa, 32 DEG C of tower top operation temperature, the 5th rectifying column (4- (1)-E) operating pressure 100KPa, tower top operation
40 DEG C of temperature, dewatering unit (4-F) uses adsorption dewatering, the 6th rectifying column (4-G) operating pressure 100KPa, tower top operation temperature
64℃。
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 622t/h mass fraction 35% or so.
A kind of separating technology of polymethoxy dimethyl ether system containing formaldehyde proposed by the present invention has passed through preferably real
Example is applied to be described, related technical personnel obviously can not depart from the content of present invention, in spirit and scope to described herein
Structure and equipment is modified or appropriate changes and combinations, Lai Shixian the technology of the present invention.In particular, it should be pointed out that Suo Youxiang
Similar replacement and change is apparent to those skilled in the art, they are considered as being included in essence of the invention
In mind, range and content.
Claims (8)
1. a kind of separating technology of the polymethoxy dimethyl ether system containing formaldehyde, using multistage rectification, it is characterised in that: any
Grade charging introduces water comprising the rectifying column of formaldehyde, and formaldehyde is made to produce to realize separating formaldehyde in form of an aqueous solutions from tower reactor
Purpose.
2. the separating technology of the polymethoxy dimethyl ether system according to claim 1 containing formaldehyde, it is characterised in that: supplement
Water is added or separates from the same feed inlet with charging and is added from two feed inlets.
3. the separating technology of the polymethoxy dimethyl ether system according to claim 1 containing formaldehyde, it is characterised in that: use
Six grades of rectifying.
4. the separating technology of the polymethoxy dimethyl ether system according to claim 1 containing formaldehyde, it is characterised in that: supplement
The additional amount of water is by weight 0.2:1~1:1 with the mass ratio of charging.
5. a kind of separator of the polymethoxy dimethyl ether system containing formaldehyde, including Multistage rectifying tower, it is characterised in that: in office
Rectifying column setting supplement water water inlet of the level-one charging comprising formaldehyde.
6. the separator of the polymethoxy dimethyl ether system according to claim 5 containing formaldehyde, it is characterised in that: including
Six grades of rectifying columns.
7. the separator of the polymethoxy dimethyl ether system according to claim 6 containing formaldehyde, it is characterised in that:
Dewatering unit is connected between Pyatyi, the 6th grade of rectifying column.
8. the separator of the polymethoxy dimethyl ether system according to claim 7 containing formaldehyde, it is characterised in that: described
Dewatering unit be film dehydration, molecular sieve dehydration, adsorption dewatering.
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| CN109776288A (en) * | 2019-01-31 | 2019-05-21 | 天津大学 | A kind of separation method and device of polymethoxy dimethyl ether |
| CN109776288B (en) * | 2019-01-31 | 2022-07-08 | 天津大学 | Method and device for separating polymethoxy dimethyl ether |
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