CN109485553A - A kind of production equipment and process removing formic acid in DMMn product - Google Patents
A kind of production equipment and process removing formic acid in DMMn product Download PDFInfo
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- CN109485553A CN109485553A CN201910052952.0A CN201910052952A CN109485553A CN 109485553 A CN109485553 A CN 109485553A CN 201910052952 A CN201910052952 A CN 201910052952A CN 109485553 A CN109485553 A CN 109485553A
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- CN
- China
- Prior art keywords
- flash tank
- discharging
- formic acid
- flash
- caustic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 235000019253 formic acid Nutrition 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000003518 caustics Substances 0.000 claims abstract description 41
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000007599 discharging Methods 0.000 claims description 40
- 239000003513 alkali Substances 0.000 claims description 27
- 238000004140 cleaning Methods 0.000 claims description 16
- 238000007701 flash-distillation Methods 0.000 claims description 8
- 239000002699 waste material Substances 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 6
- 239000002585 base Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 33
- 239000000126 substance Substances 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000007787 solid Substances 0.000 abstract description 5
- 239000003245 coal Substances 0.000 abstract description 4
- 239000012847 fine chemical Substances 0.000 abstract description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 11
- 239000000047 product Substances 0.000 description 11
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 8
- 239000000446 fuel Substances 0.000 description 7
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 description 6
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical compound C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000012495 reaction gas Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical compound [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- COTNUBDHGSIOTA-UHFFFAOYSA-N meoh methanol Chemical compound OC.OC COTNUBDHGSIOTA-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/58—Separation; Purification; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of fine that coal chemical industry is converted to petrochemical industry, are related to a kind of production equipment and process for removing formic acid in DMMn product.Apparatus body includes primary flash system and caustic washing system.The invention belongs to the field of fine chemical that coal chemical industry is converted to petrochemical industry, traditional handicraft uses solid base in process of production, resistance drop in equipment is larger and cannot remove the formic acid, formaldehyde and water contained in material, apparatus of the present invention and method use liquid base that solid base is replaced to carry out production operation, it is verified through actual production, liquid alkaline can completely remove the formic acid in material, while can also remove a small amount of formaldehyde and water, while also ensure the stability of material and the continuous and steady operation of device.
Description
Technical field
The invention belongs to the technical field of fine that coal chemical industry is converted to petrochemical industry, are related to a kind of removing DMMn product
The production equipment and process of middle formic acid.
Background technique
The alcohol-ether fuel experimental rig of present invention applicant, mainly for the production of alcohol-ether fuel (DMMn) product, while
The byproducts such as dimethoxym ethane, metaformaldehyde can be produced, designed capacity is 50,000 tons/year, and operating flexibility is 70~110%.Present apparatus master
It to include 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 DMM2 and DMMn, wherein 20132 tons of DMM2 annual output, 29940 tons of DMMn annual output.Original technology utilization solid base,
Have the shortcomings that triviality and unreliability in operation.
Summary of the invention
The present invention is directed to the production for the problem of traditional handicraft proposing formic acid in the novel removing DMMn product of one kind
Equipment and technique.
In order to achieve the above object, the present invention is realized using following technical solutions:
A kind of production equipment removing formic acid in DMMn product, including apparatus body, the apparatus body include primary flash distillation system
System and caustic washing system；
The primary flash system includes flash tank, flash distillation discharging cooler, and the caustic washing system includes entry mixers and alkali
Cleaning of evaporator；The flash tank is set between the DMMn reactor of system ontology and caustic treater, between the flash tank and caustic treater
It is provided with discharging cooler；Entry mixers are provided between the flash tank discharging cooler and caustic treater, system ontology is also
Including alkali cleaning top by flow container, the caustic treater is set to flash tank and alkali cleaning top by between flow container.
Preferably, the system ontology further includes that benefit alkali line and salkali waste flow container, the entry mixers are gone out by flash tank
Material cooler outlet is connected with entry mixers, and the entry mixers branch mouth and the discharging of caustic treater bottom connect, the charging
Mixer branch mouth is connect with alkali line is mended, and the caustic treater bottom discharging is divided into two-way, is gone entry mixers all the way, is removed spent lye all the way
Tank, the caustic treater ejection material are connect with alkali cleaning top by flow container.
Preferably, the flash tank gas phase is connected with flash distillation the first cooler of tower top, the discharging of flash tank bottom and discharging are cold
But device connects, and discharging cooler outlet removes caustic washing system.
The production technology that formic acid in DMMn product is removed using above equipment, is included the following steps,
(1) carry out the material of autoreactor after flash tank flashes, top gas phase enters light component recycling, and bottom is through pump through cooling
Device is cooled to 40 DEG C, then send after mixer 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
Machine is pumped to salkali waste flow container, and top discharge to alkali cleaning top is by flow container.
Preferably, the liquidometer pressure of the flash tank, is no more than 100KPa, discharging cooler outlet temperature is not higher than
50℃；Liquid level is not less than 50% before caustic treater is fed, and opens lye circulation, lye is kept not less than molar fraction 15% after charging
Low concentration alkali is discharged in operating process in time for concentration of lye, supplements concentrated base.
Compared with prior art, the advantages and positive effects of the present invention are:
The invention belongs to the field of fine chemical that coal chemical industry is converted to petrochemical industry, traditional handicraft uses solid in process of production
Alkali, the resistance drop in equipment is larger and cannot remove the formic acid, formaldehyde and water contained in material, and apparatus of the present invention and method use
Liquid base replaces solid base to carry out production operation, verifies through actual production, liquid alkaline can completely remove the formic acid in material, simultaneously
Also a small amount of formaldehyde and water can be removed, while also ensuring the stability of material and the continuous and steady operation of device.
Detailed description of the invention
Fig. 1 is the flow path device schematic diagram of DMMn process units of the present invention.
Each appended drawing reference are as follows: 100 flash tanks, 101 flash tank discharging pumps, 102 flash tanks discharging cooler, 103 match
Alkali entry mixers, 200 caustic treaters, 201 caustic treaters recycle discharging pump, 202 spent lye surge tanks, 203 salkali waste liquid pumps.
Specific embodiment
To better understand the objects, features and advantages of the present invention, right combined with specific embodiments below
The present invention is described further.It should be noted that in the absence of conflict, the spy in embodiments herein and embodiment
Sign can be combined with each other.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, still, the present invention may be used also
To be implemented using other modes described herein are different from, therefore, the present invention is not limited to the specific of specification is described below
The limitation of embodiment.
Embodiment 1, as shown in Figure 1, the present embodiment provides DMMn process units specific structure and processing steps.Device includes
Primary flash system and caustic washing system.Primary flash system includes flash tank 100, flash distillation discharging cooler 102, flash tank 100
It is set between DMMn reactor and caustic treater 200, the flash tank discharging cooler 102 is set to flash tank 100 and alkali cleaning
Between tank 200, flash tank discharging pump 101 is set on flash tank discharging 102 entrance pipe of cooler；Caustic washing system include with alkali into
Expect mixer 103 and caustic treater 200, it is described to be set to flash tank discharging cooler 102 and caustic treater with alkali entry mixers 103
Between 200, the caustic treater 200 is set to flash tank 100 and alkali cleaning top by between flow container.Successively according to the structure in attached drawing 1
Primary flash system is connected with each device in caustic washing system.Entry mixers 103 are exported by flash tank discharging cooler 102
It is connected with entry mixers, entry mixers branch mouth and the discharging of 200 bottom of caustic treater connect, 103 mouths of entry mixers and benefit
The connection of alkali line, the discharging of 200 bottom of caustic treater are divided into two-way, go entry mixers 103 through caustic treater circulation discharging pump 201 all the way, and one
Spent lye (buffering) tank 202 is removed through salkali waste liquid pump 203 in road, and the ejection material of caustic treater 200 is connect with alkali cleaning top by flow container；Flash tank into
Material mouth and the discharging of DMMn reactor connect, and flash tank gas phase is connect with flash distillation the first cooler inlet of tower top.100 bottom of flash tank goes out
Material is connect with flash tank discharging cooler 102, and caustic washing system is removed in the outlet of flash tank discharging cooler 102.Flash tank feed inlet with
The discharging connection of DMMn reactor, flash tank gas phase are connect with flash distillation the first cooler inlet of tower top, the discharging of flash tank bottom and discharging
Cooler connection, cooler outlet remove caustic washing system.
The method for removing the production technology of formic acid in DMMn product using above-mentioned device, the specific steps are as follows:
(1) material (crude glycol ether: DMM2-10, formaldehyde, formic acid, water, DMM1) of autoreactor in future is after flash tank flashes, top
Portion's gas phase enters light component (thick DMM1: formic acid, water, DMM1) recycling, and bottom (crude glycol ether) is cooled to 40 through cooler through pump
DEG C, then give after mixer to caustic treater；
(2) it will uniformly be mixed according to a certain percentage with lye by mixer from flash tank bottom discharging (crude glycol ether), bottom is useless
Lye (low concentration) is pumped to salkali waste flow container by machine, and top discharge (crude glycol ether) to top is by flow container.
Above-mentioned steps need to meet following process conditions:
A. before driving, cooling equipment comes into operation cooling water；
B. when flash tank liquid level is up to 30%, starting pump feeds (crude glycol ether) to caustic treater；
C. add the lye of certain liquid level (50%) in caustic treater, and open self-loopa.
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
It imitates embodiment and is applied to other fields, but without departing from the technical solutions of the present invention, according to the technical essence of the invention
Any simple modification, equivalent variations and remodeling to the above embodiments, still fall within the protection scope of technical solution of the present invention.
Claims (5)
1. a kind of production equipment for removing formic acid in DMMn product, including apparatus body, it is characterised in that: the apparatus body packet
Include primary flash system and caustic washing system；
The primary flash system includes flash tank, flash distillation discharging cooler, and the caustic washing system includes entry mixers and alkali
Cleaning of evaporator；The flash tank is set between the DMMn reactor of system ontology and caustic treater, between the flash tank and caustic treater
It is provided with discharging cooler；Entry mixers are provided between the flash tank discharging cooler and caustic treater, system ontology is also
Including alkali cleaning top by flow container, the caustic treater is set to flash tank and alkali cleaning top by between flow container.
2. removing the production equipment of formic acid in DMMn product according to claim 1, it is characterised in that: the system ontology
It further include mending alkali line and salkali waste flow container, the entry mixers are connected by flash tank discharging cooler outlet with entry mixers
It connects, the entry mixers branch mouth and the discharging of caustic treater bottom connect, and the entry mixers branch mouth is connect with alkali line is mended, the alkali
The discharging of cleaning of evaporator bottom is divided into two-way, goes entry mixers all the way, goes to salkali waste flow container, the caustic treater ejection material and alkali cleaning top all the way
It is connected by flow container.
3. removing the production equipment of formic acid in DMMn product according to claim 1, it is characterised in that: the flash tank gas
It is connected and is connected to the first cooler of flash column top, the discharging of flash tank bottom is connect with discharging cooler, and discharging cooler outlet goes alkali cleaning
System.
4. removing the production technology of formic acid in DMMn product using equipment described in claim 1-3 any one, it is characterised in that:
Include the following steps,
(1) carry out the material of autoreactor after flash tank flashes, top gas phase enters light component recycling, and bottom is through pump through cooling
Device is cooled to 40 DEG C, then send after mixer 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
Machine is pumped to salkali waste flow container, and top discharge to alkali cleaning top is by flow container.
5. removing the production technology of formic acid in DMMn product according to claim 4, it is characterised in that: the liquid of the flash tank
Position meter pressure, is no more than 100KPa, and discharging cooler outlet temperature is not higher than 50 DEG C；Liquid level is not less than 50% before caustic treater is fed,
Lye circulation is opened, lye keeps the concentration of lye for being not less than molar fraction 15% after charging, is discharged in time in operating process low dense
Alkali is spent, concentrated base is supplemented.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910052952.0A CN109485553A (en) | 2019-01-21 | 2019-01-21 | A kind of production equipment and process removing formic acid in DMMn product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910052952.0A CN109485553A (en) | 2019-01-21 | 2019-01-21 | A kind of production equipment and process removing formic acid in DMMn product |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109485553A true CN109485553A (en) | 2019-03-19 |
Family
ID=65714819
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910052952.0A Pending CN109485553A (en) | 2019-01-21 | 2019-01-21 | A kind of production equipment and process removing formic acid in DMMn product |
Country Status (1)
| Country | Link |
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| CN (1) | CN109485553A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201157769Y (en) * | 2008-02-22 | 2008-12-03 | 山东华安新材料有限公司 | Liquefied gas water caustic wash apparatus system |
| 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 |
| CN103626640A (en) * | 2013-12-13 | 2014-03-12 | 江苏凯茂石化科技有限公司 | Process unit and method for preparing polymethoxy dimethyl ether |
| CN106957221A (en) * | 2017-05-05 | 2017-07-18 | 凯瑞环保科技股份有限公司 | The device and method of polymethoxy dimethyl ether is produced in a kind of methanol oxidation |
| CN107875990A (en) * | 2017-10-30 | 2018-04-06 | 烟台国邦化工机械科技有限公司 | A kind of continuous alkaline cleaner and technique |
| CN108164400A (en) * | 2018-02-02 | 2018-06-15 | 北京东方红升新能源应用技术研究院有限公司 | Synthesize the process of polymethoxy dimethyl ether reaction product separation |
-
2019
- 2019-01-21 CN CN201910052952.0A patent/CN109485553A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201157769Y (en) * | 2008-02-22 | 2008-12-03 | 山东华安新材料有限公司 | Liquefied gas water caustic wash apparatus system |
| 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 |
| CN103626640A (en) * | 2013-12-13 | 2014-03-12 | 江苏凯茂石化科技有限公司 | Process unit and method for preparing polymethoxy dimethyl ether |
| CN106957221A (en) * | 2017-05-05 | 2017-07-18 | 凯瑞环保科技股份有限公司 | The device and method of polymethoxy dimethyl ether is produced in a kind of methanol oxidation |
| CN107875990A (en) * | 2017-10-30 | 2018-04-06 | 烟台国邦化工机械科技有限公司 | A kind of continuous alkaline cleaner and technique |
| CN108164400A (en) * | 2018-02-02 | 2018-06-15 | 北京东方红升新能源应用技术研究院有限公司 | Synthesize the process of polymethoxy dimethyl ether reaction product separation |
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Application publication date: 20190319 |