CN109516902A - A kind of production equipment and method of DMMn - Google Patents

A kind of production equipment and method of DMMn Download PDF

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Publication number
CN109516902A
CN109516902A CN201910052686.1A CN201910052686A CN109516902A CN 109516902 A CN109516902 A CN 109516902A CN 201910052686 A CN201910052686 A CN 201910052686A CN 109516902 A CN109516902 A CN 109516902A
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rectifying
tower
flow container
discharging
alkali cleaning
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CN109516902B (en
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侯福顺
马相亭
张永魁
乔天培
刘亚军
王文超
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CITIC National Chemical Co Ltd
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CITIC National Chemical Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C41/00Preparation of ethers; Preparation of compounds having groups, groups or groups
    • C07C41/48Preparation of compounds having groups
    • C07C41/58Separation; Purification; Stabilisation; Use of additives

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention relates to the field of fine chemical that coal chemical industry is converted to petrochemical industry, in particular to the production equipment and method of a kind of DMMn.The production equipment of the DMMn, including primary flash system, caustic washing system and thick DMMn distillation system, the primary flash system include flash tank, flash distillation discharging cooler;The caustic washing system includes entry mixers and caustic treater, alkali cleaning tank deck by flow container, coalescer and salkali waste flow container, and the distillation system includes 2 tower of 1 tower of rectifying and rectifying.The beneficial effects of the present invention are: effectively removing moisture, product quality, smooth operation, energy conservation and environmental protection are improved.

Description

A kind of production equipment and method of DMMn
(1) technical field
The present invention relates to the field of fine chemical that coal chemical industry is converted to petrochemical industry, in particular to the production equipment of a kind of DMMn and Method.
(2) background technique
The alcohol-ether fuel experimental rig of Chemical Co., Ltd., CITIC Guoan, mainly for the production of alcohol-ether fuel (DMMn) product, together When can also produce the byproducts such as dimethoxym ethane, metaformaldehyde, designed capacity is 50,000 tons/year, and operating flexibility is 70~110%.This dress Set mainly includes formaldehyde preparation unit, dimethoxym ethane preparation unit, metaformaldehyde synthesis unit and alcohol-ether fuel synthesis unit.
Formaldehyde preparation unit, as raw material, produces formaldehyde with methanol.Methanol and oxygen are under silver catalyst and 650 DEG C of high temperature Dehydrogenation occurs, oxidation reaction generates formaldehyde gaseous mixture and generates the formalin of high concentration using absorption.
Dimethoxym ethane unit, as raw material, under the action of solid acid catalyst, by addition, is dehydrated instead with methanol and formaldehyde Synthesizing dimethoxym ethane is answered, is then refining to obtain the dimethoxym ethane product of high concentration by processes such as flash distillation, rectifying again.
Metaformaldehyde synthesis unit is using the formaldehyde of formaldehyde unit processed production as raw material, in the effect of ionic-liquid catalyst Lower progress TOX synthetic reaction generates TOX reaction gas, and since synthetic reaction is balanced reaction, TOX is dense in the TOX reaction gas of generation Spend it is low, reaction gas need to by concentration, extraction, alkali cleaning, washing, a series of subtractive processes such as separate with extractant, finally obtain height The metaformaldehyde product of concentration.
Alcohol-ether fuel synthesis unit is using dimethoxym ethane and metaformaldehyde as raw material, using Chinese Academy of Sciences's Lanzhou Chemical Physics The Novel solid-catalyst of research institute's recent development reacts under certain temperature and pressure, generate alcohol-ether fuel, then using With reactants separate, the operation such as depickling, light component recycling obtains the alcohol-ether fuel product of high-purity.
Alcohol-ether fuel is the common name of a substance, and skeleton symbol can indicate are as follows: CH3O(CH2O)nCH3(n is more than or equal to 1 Integer), wherein with application value n value range are as follows: 1≤n≤8.There are two the alcohol ether products of alcohol ether Workshop Production, point It is not DMM2And DMMn, wherein DMM220132 tons of annual output, 29940 tons of DMMn annual output.
(3) summary of the invention
In order to compensate for the shortcomings of the prior art, the present invention provides a kind of raising product purities, the production of the DMMn of environmental protection and energy saving Device and method.
The present invention is achieved through the following technical solutions:
A kind of production equipment of DMMn, including primary flash system, caustic washing system and thick DMMn distillation system, the primary flash distillation System includes flash tank, flash distillation discharging cooler;The caustic washing system includes entry mixers and caustic treater, alkali cleaning tank deck by liquid Tank, coalescer and salkali waste flow container, the distillation system include 2 tower of 1 tower of rectifying and rectifying.
Entry mixers are set to before caustic treater in the caustic washing system, the caustic treater be set to entry mixers with Alkali cleaning tank deck is by between flow container, and the alkali cleaning tank deck is set to caustic treater between salkali waste flow container by flow container, and the coalescer is set Caustic treater and alkali cleaning tank deck are placed in by between flow container, salkali waste flow container is set to alkali cleaning tank deck after by flow container.
The caustic treater bottom discharging is divided into two-way, and the branch mouth of alkali entry mixers is matched in connection all the way, and another way connects salkali waste Flow container is connect with alkali entry mixers branch mouth with alkali line is mended, and caustic treater ejection material is connected with coalescer, the coalescer and alkali Cleaning of evaporator top is connected by flow container.
The alkali cleaning top is divided water packet to connect with salkali waste flow container by flow container, and the alkali cleaning top is discharged and rectifying column phase by flow container bottom Connection is equipped with caustic treater and recycles discharging pump between the caustic treater and salkali waste flow container, alkali cleaning tank deck is by connection alkali cleaning below flow container Tank deck is by flow container discharging pump.
1 tower of rectifying is in alkali cleaning tank deck by between 2 tower of flow container and rectifying, and the charging of 1 tower of rectifying is with alkali cleaning tank deck by flow container Discharging is connected, and 1 top gaseous phase of rectifying is connected with 1 overhead condenser import of rectifying, 1 overhead condenser of rectifying outlet with 1 tower top of rectifying is connected by flow container, and the discharging of 1 tower bottom of rectifying is connected with 2 tower of rectifying, and 1 tower top of rectifying is by flow container discharging and raw material Recycling is connected, and 1 tower top of rectifying is equipped with 1 tower top of rectifying by flow container discharging pump by flow container lower section.
The 2 tower feed inlet of rectifying discharges with 1 tower tower reactor of rectifying to be connected by 1 tower bottom discharging pump of rectifying, 2 tower top of rectifying Gas phase is connected with 2 overhead condenser import of rectifying, and the outlet of 2 overhead condenser of rectifying is connected with 2 tower top of rectifying by flow container, essence It evaporates 2 tower tops and is discharged by flow container and is connected with raw materials recovery, 2 tower of rectifying is connected with the charging of product tower, and essence is equipped with below 2 tower of rectifying Evaporate 2 tower tower reactor discharging pumps, above 2 tower of rectifying and 2 tower top of rectifying is by being equipped with 2 tower reflux pump of rectifying between flow container, 2 tower top of rectifying by 2 tower top discharging pump of rectifying is equipped with below flow container.
The flash tank is set to after reaction discharging, and the flash distillation discharging cooler setting is mixed in flash tank with charging Between device, flash tank charging is connected with flash tank discharging cooler inlet by flash tank discharging pump, the flash tank discharging Cooler outlet is connected with caustic treater entry mixers.
A kind of production method of DMMn, which comprises the following steps:
(1) for the material of autoreactor after flash tank flashes, top gas phase enters light component recycling, and bottoms material goes out through flash tank 40 DEG C are cooled to through flash tank discharging cooler after material pump, then is sent after entry mixers to caustic treater;
(2) it will uniformly be mixed according to a certain percentage with lye by mixer from the discharging of flash tank bottom, bottom spent lye passes through Spent lye circulation discharging is pumped to salkali waste flow container, and top discharge is dehydrated to alkali cleaning tank deck through coalescer by flow container;
(3) alkali cleaning tank deck by material in flow container after settlement, by dividing water packet that moisture is drained into salkali waste flow container, further remove water Point, the material of finished off water point is sent to rectifying column;
(4) passed through 1 tower rectifying of rectifying, top DMM by the material of flow container from alkali cleaning tank deck1Dimethoxym ethane is gone to recycle, bottom is thick DMMn removes 2 tower of rectifying, and column bottom temperature is controlled at 100 DEG C;
(5) enter 2 tower of rectifying, top DMM from the discharging of 1 tower tower reactor of rectifying1Dimethoxym ethane is gone to recycle, bottom crude glycol ether removes rear portion product Tower continues separating-purifying, and column bottom temperature is controlled at 120 DEG C.
The beneficial effects of the present invention are: reaction mass can be had by 2% or so the moisture contained after alkali cleaning, sedimentation Effect removal, further improves product quality, hydrolytic spoilage occurs during preventing water-containing materials in subsequent distillation system While extend follow-up system adsorbent service life, realize it is energy-saving;Reactor discharges by adding alkali neutralization, sinks simultaneously Drop dehydration.Lye is reacted with formaldehyde during this generates formic acid and water, reduces and inhibit the generation of formaldehyde.The method both reduced Formaldehyde generates the risk of blocking pipeline, while reducing the triviality of solid caustic soda used, so that production operation is more steady, produces Product purity is higher, and property is more stable, more environmentally-friendly close friend.
(4) Detailed description of the invention
The present invention will be further described below with reference to the drawings.
Attached drawing 1 is process unit structural schematic diagram of the invention;
In figure, 100 flash tanks, 101 flash tank discharging pumps, 102 flash tanks discharging cooler, 200 entry mixers, 201 alkali cleanings Tank, 202 spent lyes recycle discharging pump, and 203 coalescers, 204 alkali cleaning tank decks are by flow container, 205 salkali waste flow containers, 206 alkali cleaning tank decks by Flow container discharging pump, 207 salkali waste liquid pumps, 300 rectifying, 1 tower, 301 rectifying, 1 tower bottom discharging pump, 302 rectifying, 1 overhead condenser, 303 essences 1 tower top is evaporated by flow container, and 304 rectifying, 1 tower top is by flow container discharging pump, 401 rectifying, 2 tower, 402 rectifying, 2 tower tower reactor discharging pump, 403 essences 2 overhead condensers are evaporated, 404 rectifying, 2 tower top is by flow container, 405 rectifying, 2 tower reflux pump, 406 rectifying, 2 tower top discharging pump.
(5) specific embodiment
Attached drawing is a kind of specific embodiment of the invention.The production equipment of DMMn in the embodiment, including primary flash system, alkali System and thick DMMn distillation system are washed, primary flash system includes flash tank 100, flash distillation discharging cooler 102;Caustic washing system packet Entry mixers 200, caustic treater 201, alkali cleaning tank deck are included by flow container 204, coalescer 203 and salkali waste flow container 205, distillation system packet Include 2 tower 401 of 1 tower 300 of rectifying and rectifying.
Entry mixers 200 are set to before caustic treater 201 in caustic washing system, and caustic treater 201 is set to entry mixers 200 and alkali cleaning tank deck by between flow container 204, alkali cleaning tank deck is set between caustic treater 201 and salkali waste flow container 205 by flow container 204, The coalescer 203 is set to caustic treater 201 and alkali cleaning tank deck by between flow container 204, and salkali waste flow container 205 is set to alkali cleaning tank deck After by flow container 204.The discharging of 201 bottom of caustic treater is divided into two-way, connects the branch mouth of entry mixers 200, another way connection all the way Salkali waste flow container 205,200 mouths of entry mixers are connect with alkali line is mended, and the ejection material of caustic treater 201 is connected with coalescer 203, are gathered Knot device 203 is connect with alkali cleaning tank deck by flow container 204.Alkali cleaning top is divided water packet to connect with salkali waste flow container 205 by flow container 204, the alkali Cleaning of evaporator top is discharged by 204 bottom of flow container to be connected with rectifying column, and spent lye is equipped between the caustic treater 201 and salkali waste flow container 205 Discharging pump 202 is recycled, alkali cleaning tank deck is by connection alkali cleaning tank deck below flow container 204 by flow container discharging pump 206.
1 tower 300 of rectifying is in alkali cleaning tank deck by between 2 tower 401 of flow container 204 and rectifying, and 1 tower 300 of rectifying is fed and caustic treater Top is connected by the discharging of flow container 204, and 1 tower of rectifying, the 300 top gas phase is connected with 1 overhead condenser of rectifying, 302 import, rectifying The outlet of 1 overhead condenser 302 is connected with 1 tower top of rectifying by flow container 303, and the discharging of 1 tower of rectifying, 300 bottom is connected with 2 tower 401 of rectifying Connect, 1 tower top of rectifying is discharged by flow container 303 to be connected with raw materials recovery, 1 tower top of rectifying by below flow container 303 equipped with 1 tower top of rectifying By flow container discharging pump 304.2 tower of rectifying, 401 feed inlet passes through 1 tower bottom discharging pump of rectifying, 301 phase with the discharging of 1 tower of rectifying, 300 tower reactor Connection, 2 tower of rectifying, 401 top gas phase is connected with 2 overhead condenser of rectifying, 403 import, the outlet of 2 overhead condenser 403 of rectifying and 2 tower top of rectifying is connected by flow container 404, and 2 tower top of rectifying is discharged by flow container 404 to be connected with raw materials recovery, 2 tower 401 of rectifying and The charging of product tower is connected, and 2 tower tower reactor discharging pump 402 of rectifying, 2 tower of rectifying, 401 top and rectifying 2 are equipped with below 2 tower 401 of rectifying By 2 tower reflux pump 405 of rectifying is equipped between flow container 404,2 tower top of rectifying is discharged tower top by 2 tower top of rectifying is equipped with below flow container 404 Pump 406.
Flash tank 100 is set to after reaction discharging, and flash tank discharges the setting of cooler 102 in flash tank 100 and charging Between mixer 200, the charging of flash tank 100 is connected with flash tank discharging 102 import of cooler by flash tank discharging pump 101 It connects, the outlet of flash tank discharging cooler 102 is connected with caustic treater entry mixers 200.
The production method of DMMn in the embodiment, comprising the following steps:
(1) material (the crude glycol ether: DMM of autoreactor2-10, formaldehyde, formic acid, water, DMM1And TOX) after the flash distillation of flash tank 100, Top gas phase (thick DMM1) enter light component recycling, bottoms material (crude glycol ether: DMM2-10, formaldehyde, formic acid, water, DMM1And TOX) 40 DEG C are cooled to through flash tank discharging cooler 102 after flash tank discharging pump 101, then is sent after entry mixers 200 to alkali Cleaning of evaporator 201;
(2) will discharge (crude glycol ether: DMM from 100 bottom of flash tank2-10, formaldehyde, formic acid, water, DMM1And TOX) pass through with lye Mixer uniformly mixes according to a certain percentage, and bottom spent lye recycles discharging pump 202 by spent lye and send to salkali waste flow container 205, Top discharge (crude glycol ether: DMM2-10, water, DMM1And TOX) be dehydrated to alkali cleaning tank deck through coalescer 203 by flow container 204;
(3) alkali cleaning tank deck is by material (crude glycol ether: DMM in flow container 2042-10, water, DMM1And TOX) after settlement, by dividing water packet Moisture is drained into salkali waste flow container 205, further removes moisture, material (the crude glycol ether: DMM of finished off water point2-10, water, DMM1With TOX it) send to rectifying column;
(4) from alkali cleaning tank deck by material (the crude glycol ether: DMM of flow container 2042-10, water, DMM1And TOX) pass through 1 tower 300 of rectifying Rectifying, top DMM1Dimethoxym ethane is gone to recycle, the thick DMMn in bottom removes 2 tower 401 of rectifying, and column bottom temperature is controlled at 100 DEG C;
(5) from 1 tower of rectifying, 300 tower reactor discharging (crude glycol ether: DMM2-10, water, DMM1And TOX) enter 2 tower 401 of rectifying, top DMM1 Dimethoxym ethane is gone to recycle, bottom crude glycol ether (DMM2-10And TOX) rear portion product tower is gone to continue separating-purifying, column bottom temperature control exists 120℃。
When work, keep a close eye on flash tank 100 liquidometer pressure, must not superpressure, and discharge cooler outlet temperature not Preferably it is higher than 50 DEG C, 201 feeding temperature of caustic treater should not be higher than 50 DEG C, and caustic treater 201 should first establish certain liquid level before feeding, and open Lye circulation is opened, lye keeps concentration of lye in a certain range after charging, and low concentration alkali is discharged in time, supplements concentrated base, coalescer When 203 filter core pressure differences are greater than 0.1MPa, cut-in stand-by coalescer, Fen Shuibao circle are not higher than 50%, must guarantee 1 tower 300 of rectifying Separating effect controls 100 DEG C of 1 tower of rectifying, 300 bottom temperature, guarantees DMM in 2 tower 401 of rectifying1Separating effect, control rectifying 2 120 DEG C of the bottom temperature of tower 401.
It, can be by reaction mass by containing after alkali cleaning, sedimentation using the production equipment and method of DMMn of the invention 2% or so water effective removal, further improve product quality, prevent water-containing materials in subsequent distillation system process The middle service life for occurring to extend follow-up system adsorbent while hydrolytic spoilage, is realized energy-saving;Reactor discharging passes through Add alkali neutralization, while deposition dehydrating.Lye is reacted with formaldehyde during this generates formic acid and water, reduces and inhibit the production of formaldehyde It is raw.The method had both reduced formaldehyde and has generated the risk of blocking pipeline, while reducing the triviality of solid caustic soda used, so that production Operation is more steady, and product purity is higher, and property is more stable, more environmentally-friendly close friend.

Claims (8)

1. a kind of production equipment of DMMn, including including primary flash system, caustic washing system and thick DMMn distillation system, it is described first Grade flash system includes flash tank (100), flash distillation discharging cooler (102);The caustic washing system includes entry mixers (200), caustic treater (201), alkali cleaning tank deck are by flow container (204), coalescer (203) and salkali waste flow container (205), the distillation system Including 1 tower of rectifying (300) and 2 tower of rectifying (401).
2. the production equipment of DMMn according to claim 1, it is characterized in that: entry mixers in the caustic washing system (200) it is set to before caustic treater (201), the caustic treater (201) is set to entry mixers (200) and alkali cleaning tank deck by liquid Between tank (204), the alkali cleaning tank deck is set between caustic treater (201) and salkali waste flow container (205) by flow container (204), described Coalescer (203) is set to caustic treater (201) and alkali cleaning tank deck by between flow container (204), and salkali waste flow container (205) is set to alkali cleaning Tank deck is after by flow container (204).
3. the production equipment of DMMn according to claim 2, it is characterized in that: the discharging of the caustic treater (201) bottom is divided into two Road connects the branch mouth of entry mixers (200) all the way, and another way connects salkali waste flow container (205), entry mixers (200) branch mouth Connect with alkali line is mended, caustic treater (201) ejection material is connected with coalescer (203), the coalescer (203) and alkali cleaning tank deck by Flow container (204) connection.
4. the production equipment of DMMn according to claim 2, it is characterized in that: the alkali cleaning top is by flow container (204) Fen Shuibao It is connect with salkali waste flow container (205), the alkali cleaning tank deck is discharged by flow container (204) bottom to be connected with rectifying column, the caustic treater (201) spent lye circulation discharging pump (202) is equipped between salkali waste flow container (205), alkali cleaning tank deck is connected by below flow container (204) Alkali cleaning tank deck is by flow container discharging pump (206).
5. the production equipment of DMMn according to claim 1, it is characterized in that: 1 tower of the rectifying (300) alkali cleaning tank deck by Between flow container (204) and 2 tower of rectifying (401), 1 tower of rectifying (300) charging is connected with alkali cleaning tank deck by flow container (204) discharging, 1 tower of rectifying (300) the top gas phase is connected with 1 overhead condenser of rectifying (302) import, and 1 overhead condenser of rectifying (302) goes out Mouth is connected with 1 tower top of rectifying by flow container (303), and the discharging of 1 tower of rectifying (300) bottom is connected with 2 tower of rectifying (401), 1 tower of rectifying Top is discharged by flow container (303) to be connected with raw materials recovery, and 1 tower top of rectifying is equipped with 1 tower top of rectifying by flow container by flow container (303) lower section Discharging pump (304).
6. the production equipment of DMMn according to claim 1, it is characterized in that: 2 tower of the rectifying (401) feed inlet and rectifying The discharging of 1 tower (300) tower reactor is connected by 1 tower bottom discharging pump (301) of rectifying, 2 tower of rectifying (401) top gas phase and 2 tower top of rectifying Condenser (403) import is connected, and 2 overhead condenser of rectifying (403) outlet is connected with 2 tower top of rectifying by flow container (404), essence It evaporates 2 tower tops and is discharged by flow container (404) and is connected with raw materials recovery, 2 tower of rectifying (401) is connected with the charging of product tower, 2 tower of rectifying (401) lower section is equipped with 2 tower tower reactor discharging pump (402) of rectifying, above 2 tower of rectifying (401) with 2 tower top of rectifying by flow container (404) it Between be equipped with 2 tower reflux pump (405) of rectifying, 2 tower top of rectifying is by being equipped with 2 tower top discharging pump (406) of rectifying below flow container (404).
7. the production equipment of DMMn according to claim 1, it is characterized in that: the flash tank (100) is set to and reflects After material, flash tank discharging cooler (102) is arranged between flash tank (100) and entry mixers (200), flash tank (100) charging is connected with flash tank discharging cooler (102) import by flash tank discharging pump (101), and the flash tank goes out Material cooler (102) outlet is connected with caustic treater entry mixers (200).
8. a kind of production method of DMMn described in claim 1, it is characterized in that: the following steps are included:
(1) material of autoreactor is after flash tank (100) flash distillation, and top gas phase enters light component recycling, and bottoms material is through dodging Steaming pot discharging pump (101) is cooled to 40 DEG C by flash tank discharging cooler (102), then send after entry mixers (200) to Caustic treater (201);
(2) it will uniformly be mixed according to a certain percentage with lye by mixer from the discharging of flash tank (100) bottom, bottom spent lye It is sent by spent lye circulation discharging pump (202) to salkali waste flow container (205), top discharge is dehydrated through coalescer (203) to caustic treater Top is by flow container (204);
(3) alkali cleaning tank deck by flow container (204) interior material after settlement, by dividing water packet that moisture is drained into salkali waste flow container (205), into The material of one-step removal moisture, finished off water point is sent to rectifying column;
(4) passed through 1 tower of rectifying (300) rectifying, top DMM by the material of flow container (204) from alkali cleaning tank deck1Dimethoxym ethane is gone to recycle, The thick DMMn in bottom removes 2 tower of rectifying (401), and column bottom temperature is controlled at 100 DEG C;
(5) enter 2 tower of rectifying (401), top DMM from the discharging of rectifying 1 tower (300) tower reactor1Dimethoxym ethane is gone to recycle, bottom crude glycol ether Rear portion product tower is gone to continue separating-purifying, column bottom temperature is controlled at 120 DEG C.
CN201910052686.1A 2019-01-21 2019-01-21 DMMn production equipment and method Active CN109516902B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102701923A (en) * 2012-06-11 2012-10-03 北京科尔帝美工程技术有限公司 System device and process for preparing polymethoxy dimethyl ether
CN202808649U (en) * 2012-06-11 2013-03-20 北京科尔帝美工程技术有限公司 Systemic device for preparing polyoxymethylene dimethyl ether
CN204644230U (en) * 2015-05-14 2015-09-16 江苏凯茂石化科技有限公司 Formaldehyde absorption process unit in a kind of polymethoxy dimethyl ether synthesis
CN107118083A (en) * 2017-06-03 2017-09-01 天津大学 A kind of apparatus and method for the refining spearation of polymethoxy dimethyl ether containing formaldehyde

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102701923A (en) * 2012-06-11 2012-10-03 北京科尔帝美工程技术有限公司 System device and process for preparing polymethoxy dimethyl ether
CN202808649U (en) * 2012-06-11 2013-03-20 北京科尔帝美工程技术有限公司 Systemic device for preparing polyoxymethylene dimethyl ether
CN204644230U (en) * 2015-05-14 2015-09-16 江苏凯茂石化科技有限公司 Formaldehyde absorption process unit in a kind of polymethoxy dimethyl ether synthesis
CN107118083A (en) * 2017-06-03 2017-09-01 天津大学 A kind of apparatus and method for the refining spearation of polymethoxy dimethyl ether containing formaldehyde

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