CN106146266A - A kind of concentrated formaldehyde prepares process and the device of polymethoxy dimethyl ether - Google Patents
A kind of concentrated formaldehyde prepares process and the device of polymethoxy dimethyl ether Download PDFInfo
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- CN106146266A CN106146266A CN201610522668.1A CN201610522668A CN106146266A CN 106146266 A CN106146266 A CN 106146266A CN 201610522668 A CN201610522668 A CN 201610522668A CN 106146266 A CN106146266 A CN 106146266A
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- 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
- C07C41/50—Preparation of compounds having groups by reactions producing groups
- C07C41/56—Preparation of compounds having groups by reactions producing groups by condensation of aldehydes, paraformaldehyde, or ketones
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Abstract
The invention discloses a kind of concentrated formaldehyde and prepare process and the device of polymethoxy dimethyl ether, it is with dimethoxym ethane and formalin that concentration is 50%～88% as raw material, reacts and obtain containing polymethoxy dimethyl ether and unreacted formalin and the reactant liquor of dimethoxym ethane；Described reactant liquor sends into extraction tower after dehydrogenation from tower top, and carry out counter current contacting reaction with the extractant entered from tower bottom, polymethoxy dimethyl ether in reactant liquor is dissolved in extractant and obtains organic facies, formalin is layered with organic facies, and extraction organic facies is sent in extractant recovery tower；Described organic facies is sent into and is carried out air-distillation separation in extractant recovery tower, and recovery obtains the extractant of tower top and the polymethoxy dimethyl ether of the degree of polymerization 2～8 of tower reactor extraction.Present invention reduces cost, and improve Synthesis conversion and yield is low, and the present invention has and well moves thermal effect, can be efficiently promoting reaction and carry out, transforming degree achieves controllability.
Description
Technical field
The invention belongs to chemical production technology and equipment technical field, relate generally to formaldehyde and prepare polymethoxy dimethyl ether
Technology.
Background technology
The feature of China's energy resource structure is: rich coal, gas oil-poor, few, economical maintains sustained and rapid growth more to carry out energy demand
The biggest, the contradiction of society, expanding economy and oil supply.Since 2009, crude oil in China external dependence degree is even
Continue and within 6 years, exceed warning line (50%), have a strong impact on the energy strategy safety of China.From China's energy strategy safety, in conjunction with
China's primary energy structure feature, Development of Coal base liquid fuel synthetic technology has strategic significance undoubtedly.It addition, China's methanol
Production capacity is superfluous, exploitation Downstream Products of Methanol, extension Chemical Industry chain, all has realistic meaning.
Along with science and technology and economic progress, incity, city automobile quantity showed increased, and motor vehicle exhaust emission thing becomes
One of major reason of city haze.Compared to gasoline, diesel oil has higher boiling point, and H/C mass ratio is low, therefore diesel combustion
During the waste gas CO of discharge, oxynitride, particulate matter etc. more, the damage ratio gasoline caused is more serious.Therefore, bavin is improved
Oil firing efficiency, reduces disposal of pollutants, and improving urban air-quality is the most important environmental protection task.
Polymethoxy dimethyl ether is a kind of universally acknowledged cleaning diesel oil component, its Cetane number >=70, not sulfur-bearing, no
Containing aromatic hydrocarbons.Add in diesel oil in 5%-20% ratio, it is possible to increase diesel cetane-number, promote burning, it will be apparent that reduce vapour
The discharge of the harmful gas such as PM2.5, PM10, NOx, CO in tail gas.Due to the excellent properties of polymethoxy dimethyl ether, its synthesis
Technique has become the heat subject of research both at home and abroad.
At present, polymethoxy dimethyl ether is with one or more in methanol or dimethoxym ethane and formalin/tri-mostly
Polyformaldehyde/paraformaldehyde reacts generation under the catalytic action of acidic catalyst.Use metaformaldehyde or paraformaldehyde, technique
Long flow path and complexity, construction costs increases considerably, and production cost remains high.And use formalin relatively inexpensive, one
Kind first refine as formaldehyde gas for formalin, participate in synthetic reaction with gas phase；One first concentrates as dense for formalin
Formaldehyde, participates in synthetic reaction with concentrated formaldehyde.The preparation of gaseous formaldehyde need to be through extracting, be dehydrated, resolve three technical processs, and formaldehyde is
Becoming gas phase eventually, energy consumption is relatively big, and relates to another extractant, and extractant has certain loss.The preparation of concentrated formaldehyde only needs
The lower evaporation of decompression just can complete, and operates relatively easy, and concentrated formaldehyde is that raw material carries out synthetic reaction, for full liquid phase reactor, reacts bar
Part is gentle, and yield is higher.By adjusting the charging proportioning of concentrated formaldehyde and dimethoxym ethane, product degree of polymerization distribution can be optimized, obtain
More DMM3-5.Test proves that DMMn3-5 is the DMMn product being best suitable for doing diesel fuel additives.
Summary of the invention
Goal of the invention: for problem and the defect of above-mentioned existence, the invention provides a kind of concentrated formaldehyde and prepares polymethoxy
The process of dimethyl ether and device, solve and turn with cost height, the synthesis brought in paraformaldehyde/trimerization production process at present
Rate and the low problem of yield, and the present invention has and well moves thermal effect, can be efficiently promoting reaction and carry out, transforming degree realizes
Controllability.
Technical scheme: for achieving the above object, the present invention by the following technical solutions: a kind of concentrated formaldehyde prepares poly-first
The process of epoxide dimethyl ether, with dimethoxym ethane and formalin that concentration is 50%～88% as raw material, exists in the reactor
React under the catalysis of solid acid resin and obtain containing polymethoxy dimethyl ether and unreacted formalin and dimethoxym ethane
Reactant liquor；Described reactant liquor after dehydrogenation from tower top send into extraction tower, and with the extraction entered from extraction tower tower bottom
Agent carries out counter current contacting and fully reacts, and the polymethoxy dimethyl ether in reactant liquor is dissolved in extractant and obtains organic facies, formalin
Solution is layered with organic facies, and extraction organic facies is sent in extractant recovery tower, and formalin is from the tower reactor of extraction tower
Extraction；Described organic facies is sent into and is carried out air-distillation separation in extractant recovery tower, reclaims extractant and the tower reactor obtaining tower top
The polymethoxy dimethyl ether of the degree of polymerization 2～8 of extraction；The polymethoxy dimethyl ether of the described degree of polymerization 2～8 refined point further
From.
As preferably, described extractant is benzene, hexamethylene, normal hexane or diisopropyl ether.
As preferably, described extractant is, normal hexane or diisopropyl ether.
As preferably, the reaction temperature under solid acid resin catalysis of described dimethoxym ethane and formalin is 50～150
DEG C, reaction pressure is 0.1～1.5MPa.
As preferably, the polymethoxy dimethyl ether of the described degree of polymerization 2～8 sends into one-level treating column, and in normal pressure, tower top temperature
Degree is 100～105 DEG C, and reflux ratio is to refine under conditions of 0.5～2, obtains, at tower top, the polymethoxy two that the degree of polymerization is 2
Methyl ether.
As preferably, the tower bottoms that described one-level treating column obtains sends into two grades for the treatment of columns, 2～20KPa, tower top temperature
Being 110～140 DEG C, column bottom temperature is 160～200 DEG C, and reflux ratio is that to carry out backflow under conditions of 0.5～2 refined, obtains at tower top
To the polymethoxy dimethyl ether that the degree of polymerization is 3～5.
Present invention also offers a kind of concentrated formaldehyde based on above-mentioned process and prepare the technique dress of polymethoxy dimethyl ether
Put, including the reactor being sequentially connected with, lightness-removing column, extraction tower, extractant recovery tower, one-level treating column and two grades for the treatment of columns, institute
Stating the top of reactor and be provided with mixing material inlet, described mixing material inlet connects mixed liquor distributor, described instead
The stage casing answering device is filled with solid acid resin catalyst, and described reactor bottom is provided with reactant liquor outlet and is connected with lightness-removing column.
As preferably, described reactor is fluid bed.
As preferably, described extraction tower is packed tower.
Beneficial effect: compared with prior art, the invention have the advantages that and solve at present with paraformaldehyde/trimerization
The cost that brings in production process is high, Synthesis conversion and the low problem of yield, and the present invention has and well moves thermal effect, can be high
The promotion reaction of effect is carried out, and transforming degree achieves controllability.
The reaction of the fluidized-bed reactor in the present invention has more more preferable heat transfer property than fixed bed reactors, whether footpath
The most visibly homogeneous to still axial temperature Temperature Distribution, due to the strenuous exercise of bed, eliminate the laminar flow side near heat-transfer area
Interlayer so that it moves the thermal efficiency far above the other types reactor such as fixed bed and blank pipe.
The present invention uses the formalin of higher concentration to replace with paraformaldehyde or the solid materials such as formaldehyde of living scattered simultaneously,
Combined coefficient and yield are high；The formalin simultaneously utilizing high concentration can promote the forward reaction of polyreaction to balance.
Accompanying drawing explanation
Fig. 1 is the structural representation that concentrated formaldehyde of the present invention prepares the process unit of polymethoxy dimethyl ether.
Wherein, reactor 1, lightness-removing column 2, extraction tower 3, extractant recovery tower 4,5, two grades for the treatment of columns 6 of one-level treating column.
Detailed description of the invention
Below in conjunction with the accompanying drawings and specific embodiment, it is further elucidated with the present invention, it should be understood that these embodiments are merely to illustrate
The present invention rather than limit the scope of the present invention, after having read the present invention, each to the present invention of those skilled in the art
The amendment planting the equivalent form of value all falls within the application claims limited range.
As it is shown in figure 1, polymethoxy dimethyl ether of the present invention synthesis and separating-purifying device, including reactor, lightness-removing column, extraction
Take tower, extractant recovery tower, DMM2 product tower, DMM3～5 product towers.Wherein:
Its version of described reactor is not limited to fluid bed or fixed bed, for full liquid phase reactor, relative to solid-liquid reaction,
Reactant contact surface is bigger, and reaction efficiency is high, yield is high.Reactor head arranges concentrated formaldehyde-dimethoxym ethane mixed solution charging aperture,
And carry out feeding mixed liquor distribution by liquid distribution trough；Reactor stage casing loads solid acid resin catalyst, reactor bottom
It is provided with reactant liquor outlet, and is connected with lightness-removing column.
Described reactor feedstocks uses concentrated formaldehyde and liquid dimethoxym ethane.Concentrated formaldehyde and liquid dimethoxym ethane are in static mixer
Add from reactor head after uniformly mixing in proportion, through solid acid resin catalyst, arrive reactor bottom reactant liquor and go out
Mouthful.The outer circulation cooling of the hot facility of shifting such as employing can be set in reactor reaction section or increase cooling tube, but this is not necessarily, excellent
Choosing is not provided with moving hot facility.
Reactant liquor discharging opening bottom described lightness-removing column charging aperture coupled reaction device, reactant liquor removes first contracting in lightness-removing column
Aldehyde.This tower top atmospheric operation, tower top arranges condenser and return tank, reflux ratio preferably 1～2.Tower top obtains pure component dimethoxym ethane.
Tower reactor obtains the reactant liquor without dimethoxym ethane.
Then the reactant liquor without dimethoxym ethane is sent in extraction tower and carry out extractive reaction.Described extraction tower use filler or
Person's plank frame, preferred filler tower.Reactant liquor is added by extraction tower top, and extractant diisopropyl ether adds from extraction tower bottom,
Reactant liquor and diisopropyl ether counter current contacting, owing to the density of diisopropyl ether is gently the most upwards turned with density contrast from top to down by bottom
The reactant liquor moved carries out uninterrupted counter current contacting, and during being somebody's turn to do, DMMn constantly extracts and is transferred to organic facies, and formalin
Aqueous phase the most constantly sinks, it is achieved the uninterrupted separation of the extraction of constantly extraction and the upper layer of extraction liquid under full liquid status, effect in tower
Rate is higher.During Gai, diisopropyl ether be light materials, can effectively DMMn in extractive reaction liquid, and do not occur chemistry anti-with DMMn
Answer, and follow-up dehydrogenation separates and is easier to.
The Organic substance based on DMMn in reactant liquor is dissolved in extractant, and water and formaldehyde in reactant liquor cannot be dissolved in
In extractant, owing to there is obvious density contrast between them, therefore in tower, produce noted phase separation phenomena, by boundary height control
Extraction upper liquid processed and subnatant.Subnatant is the aqueous solution mainly containing formaldehyde；Upper liquid is mainly to contain DMM2～8 components and extraction
Taking the organic facies of agent component, upper liquid discharging opening is connected with extractant recovery tower charging aperture.
The charging of described extractant recovery tower connects extraction tower upper liquid discharging.It should be noted that the separation time that extractant reclaims
Sequence is not fixing, and it is relevant with the extractant kind used, and can be reclaimed by extractant for high boiling extractant and put
After product tower.Preferably extractant recovery tower is after extraction tower.Extractant recovery tower uses filler or plate column, normal pressure
Operation, tower top uses condenser and return tank, preferably reflux ratio 1～4. overhead extraction extractant material, and still liquid obtains product thing
Material DMM2～8.
According to described, still liquid product sends into DMM2 product.This tower uses filler or plate column, atmospheric operation, and tower top is adopted
With condenser and return tank, by controlling reflux ratio 0.5～2, the DMM2 product that extraction conforms to quality requirements.For not meeting matter
The product that amount requires will be fed into the charging of this tower and again refines, it is also possible to increases reflux ratio and improves product quality.
According to described, DMM2 product tower bottoms is DMM3～8 products.This still liquid sends into DMM3～5 product towers.This tower uses
Filler or plate column, decompression operation, preferred operations pressure 2～20kPa (absolute pressure), tower top uses condenser and backflow
Tank, preferably reflux ratio are that 0.5～2. tower tops obtain DMM3～5 products.It should be noted that overhead product not necessarily,
Different regions can control the product that extraction quality is different, such as, in the area that south winter temperature is higher, the lowest temperature is the most remote
Higher than the condensation point of DMM6, can suitably extraction part DMM6, more preferable blended diesel component.For northern area, the most on the contrary, need
Containing the fewest DMM6 in product to be controlled, it is to avoid wherein contain high condensation point blend component.
Preferably, extractant can also use and normal hexane.Most preferably use normal hexane, due to relative density
The counter current contacting of minimum, extractant and reactant liquor is more violent, and the DMMn therefrom extracted is the most thorough, has more preferably separating effect.
Claims (9)
1. a concentrated formaldehyde prepares the process of polymethoxy dimethyl ether, it is characterised in that: with dimethoxym ethane and concentration for 50%
～the formalin of 88% is raw material, reacting under the catalysis of solid acid resin in the reactor obtains containing polymethoxy
Dimethyl ether and unreacted formalin and the reactant liquor of dimethoxym ethane；Described reactant liquor sends into extraction after dehydrogenation from tower top
Take tower, and carry out counter current contacting with the extractant entered from extraction tower tower bottom and fully react, the polymethoxy two in reactant liquor
Methyl ether is dissolved in extractant and obtains organic facies, and formalin is layered with organic facies, and extraction organic facies sends into extractant
In recovery tower, formalin is from the tower reactor extraction of extraction tower；Described organic facies is sent in extractant recovery tower and is carried out normal pressure steaming
Fraction from, reclaim the polymethoxy dimethyl ether of the degree of polymerization 2～8 obtaining the extractant of tower top and tower reactor extraction；The described degree of polymerization 2
～the further refining spearation of polymethoxy dimethyl ether of 8.
The most according to claim 1, concentrated formaldehyde prepares the process of polymethoxy dimethyl ether, it is characterised in that: described extraction
Agent is benzene, hexamethylene, normal hexane or diisopropyl ether.
The most according to claim 1, concentrated formaldehyde prepares the process of polymethoxy dimethyl ether, it is characterised in that: described extraction
Agent is normal hexane or diisopropyl ether.
The most according to claim 1, concentrated formaldehyde prepares the process of polymethoxy dimethyl ether, it is characterised in that: described first contracts
The reaction temperature under solid acid resin catalysis of aldehyde and formalin is 50～150 DEG C, and reaction pressure is 0.1～1.5MPa.
The most according to claim 1, concentrated formaldehyde prepares the process of polymethoxy dimethyl ether, it is characterised in that: described polymerization
The polymethoxy dimethyl ether of degree 2～8 sends into one-level treating column, and is 100～105 DEG C in normal pressure, tower top temperature, and reflux ratio is
Refine under conditions of 0.5～2, obtain, at tower top, the polymethoxy dimethyl ether that the degree of polymerization is 2.
The most according to claim 5, concentrated formaldehyde prepares the process of polymethoxy dimethyl ether, it is characterised in that: described one-level
Two grades for the treatment of columns sent into by the tower bottoms that treating column obtains, and 2～20KPa, tower top temperature is 110～140 DEG C, and column bottom temperature is
160～200 DEG C, reflux ratio is that to carry out backflow under conditions of 0.5～2 refined, obtains, at tower top, the poly-methoxy that the degree of polymerization is 3～5
Base dimethyl ether.
7. prepare a process unit for polymethoxy dimethyl ether based on the concentrated formaldehyde of process described in claim 1～7, its
It is characterised by: include that the reactor, lightness-removing column, extraction tower, extractant recovery tower, one-level treating column and two grades that are sequentially connected with are refined
Tower, the top of described reactor is provided with mixing material inlet, and described mixing material inlet connects mixed liquor distributor, institute
The stage casing stating reactor is filled with solid acid resin catalyst, described reactor bottom be provided with reactant liquor outlet and with lightness-removing column phase
Even.
The most according to claim 8, concentrated formaldehyde prepares the process unit of polymethoxy dimethyl ether, it is characterised in that: described reaction
Device is fluid bed.
The most according to claim 8, concentrated formaldehyde prepares the process unit of polymethoxy dimethyl ether, it is characterised in that: described extraction
Tower is packed tower.
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| CN201610522668.1A CN106146266A (en) | 2016-07-05 | 2016-07-05 | A kind of concentrated formaldehyde prepares process and the device of polymethoxy dimethyl ether |
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Cited By (8)
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| CN107556171A (en) * | 2017-06-27 | 2018-01-09 | 河南中鸿集团煤化有限公司 | A kind of polymethoxy dimethyl ether process units |
| CN107721831A (en) * | 2017-11-08 | 2018-02-23 | 江苏道尔顿石化科技有限公司 | A kind of polymethoxy dimethyl ether synthesizes the plug-in reaction system of bubble type and synthetic method |
| CN107739301A (en) * | 2017-11-08 | 2018-02-27 | 江苏道尔顿石化科技有限公司 | A kind of polymethoxy dimethyl ether synthesis system and technique |
| CN110054550A (en) * | 2019-04-09 | 2019-07-26 | 天津大学 | A kind of process system and method for gaseous formaldehyde method production polymethoxy dimethyl ether |
| CN110372479A (en) * | 2018-04-13 | 2019-10-25 | 中国科学院大连化学物理研究所 | A kind of continuous catalysis extracting process preparing more polymethoxy dimethyl ethers |
| CN110372477A (en) * | 2018-04-13 | 2019-10-25 | 中国科学院大连化学物理研究所 | A kind of continuous catalysis extracting process preparing polymethoxy dimethyl ether |
| CN111517926A (en) * | 2020-04-27 | 2020-08-11 | 陈华 | System and method for synthesizing polymethoxy dimethyl ether from methylal |
| CN112299963A (en) * | 2020-11-20 | 2021-02-02 | 清华大学 | Method for continuously producing polymethoxy dimethyl ether |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110372479A (en) * | 2018-04-13 | 2019-10-25 | 中国科学院大连化学物理研究所 | A kind of continuous catalysis extracting process preparing more polymethoxy dimethyl ethers |
| CN110372477A (en) * | 2018-04-13 | 2019-10-25 | 中国科学院大连化学物理研究所 | A kind of continuous catalysis extracting process preparing polymethoxy dimethyl ether |
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| CN110054550A (en) * | 2019-04-09 | 2019-07-26 | 天津大学 | A kind of process system and method for gaseous formaldehyde method production polymethoxy dimethyl ether |
| CN111517926B (en) * | 2020-04-27 | 2023-05-02 | 陈华 | System and method for synthesizing polymethoxy dimethyl ether by methylal |
| CN111517926A (en) * | 2020-04-27 | 2020-08-11 | 陈华 | System and method for synthesizing polymethoxy dimethyl ether from methylal |
| CN112299963B (en) * | 2020-11-20 | 2022-01-07 | 清华大学 | Method for continuously producing polymethoxy dimethyl ether |
| CN112299963A (en) * | 2020-11-20 | 2021-02-02 | 清华大学 | Method for continuously producing polymethoxy dimethyl ether |
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Effective date of registration: 20180118 Address after: 214000 K-PARK Service Center No. 3, No. 50, No. 50, embroidery Creek Road, Binhu District, Jiangsu Province, Southeast of 4 Applicant after: Jiangsu Dalton Petrochemical Technology Co., Ltd. Address before: Jinxi road Binhu District 214000 Jiangsu city of Wuxi province No. 100 Applicant before: WUXI ZHIGUI TECHNOLOGY CO., LTD. |
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