CN107011130A - The device and operating method of a kind of synthesizing polymethoxy methylal - Google Patents
The device and operating method of a kind of synthesizing polymethoxy methylal Download PDFInfo
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- CN107011130A CN107011130A CN201710257636.8A CN201710257636A CN107011130A CN 107011130 A CN107011130 A CN 107011130A CN 201710257636 A CN201710257636 A CN 201710257636A CN 107011130 A CN107011130 A CN 107011130A
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- 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 device and operating method of a kind of synthesizing polymethoxy methylal of the present invention.Including the reactor with catalyst filtration film and the water filter with water filtration film；The water filter that series connection one carries water filtration film between two reactors with catalyst filtration film；Raw material dimethoxym ethane and metaformaldehyde enter reactor of the First with catalyst filtration film by pipeline after blender is preheated and reacted, the water filter with water filtration film is entered by pipeline after reaction, then reacted through piping into next reactor with catalyst filtration film；Last reactor with catalyst filtration film is connected by pipeline with first rectifying column, and first rectifying column bottom is connected by pipeline with Second distillation column, and final product is obtained from Second distillation column top.The present invention improves production efficiency, while using the method for rectifying by n<3 and n>8 DMMnSeparation, is sent in reactor by pipeline, recycled.
Description
Technical field
The invention belongs to field of chemical technology, it is related to device and the operation side of a kind of synthesizing polymethoxy methylal
Method.
Background technology
With expanding economy, people are more and more using the quantity of automobile, and a large amount of harmful substances in vehicle exhaust are just
It can be discharged into air, seriously endanger the healthy of people.Nowadays, petroleum-based energy is in short supply, and people are directed to improving now
Oil quality, improves performance to alleviate the pressure of oil shortage.
In the application of internal combustion engine, the thermal efficiency relative to gasoline engine diesel engine is high, and has broader practice scope.
And diesel engine primary discharge NOXAnd particulate matter, pollution can be produced to air, seemed so finding a kind of suitable diesel fuel additives
It is particularly important.
Polymethoxy methylal also known as polymethoxy dimethyl ether (abbreviation DMMnOr PODE) it is a kind of oil dope, it is put down
Equal Cetane number (CN) value is 76, and oxygen content is high.DMMnThe calorific value of diesel oil can be improved and the discharge of tail gas is reduced.Therefore, DMMn
The concern for enjoying scientists.Suitably it is the polymethoxy methylal (DMM of oil dopen) n=3~8 are generally,
Because it has very high Cetane number (being more than 76) and oxygen content, the discharge of carbon monoxide and oxynitrides is reduced, and
And improve the thermal efficiency.
From 1948, E.I.Du Pont Company reported synthesizing polymethoxy methylal first, and research of the scientist to this respect does not just have
Have and stopped.US2449469 discloses one kind and prepares polymethoxy methylal, catalyst using dimethoxym ethane and paraformaldehyde as raw material
For sulfuric acid, but the problem of there is etching apparatus, and used reactor can not in time be excluded in course of reaction and generated
Water, water as reaction product appearance, if discharging reaction system not in time, then the polymethoxy generated can be hydrolyzed
Dimethoxym ethane, so as to generate unstable hemiacetal.BASF Aktiengellschaft reports in the A of patent CN 101048537
A kind of method for preparing polymethoxy methylal, is characterised by introducing reaction mixing by dimethoxym ethane, trioxanes and/or catalyst
Water is set to be less than the 1% of reactant mixture weight in thing, but its reactor used is stirring reactor or pipe reaction
Device, this reactor can not discharge the water that reaction is produced in time.A kind of synthesis is reported in the special B of CN 103664550 poly-
The tank reactor of methoxy methyl acetal, is characterized as paste state bed reactor, during the course of the reaction respectively in control different reactor
Temperature reached good reaction effect.But, the method for this series multistage reactor can not be excluded in time reacted
The water generated in journey.
The content of the invention
The purpose of the present invention is to overcome to produce influence of the water to reaction in existing building-up process, it is proposed that the poly- first of one kind synthesis
The device and operating method of epoxide dimethoxym ethane, concrete technical scheme are as follows：
A kind of device of synthesizing polymethoxy methylal of the present invention；Including reactor and band with catalyst filtration film
There is the water filter of water filtration film；It is characterized in that series connection one carries water filtration between two reactors with catalyst filtration film
The water filter of film, first reactor with catalyst filtration film is provided with charging aperture, and last carries catalyst filtration
The reactor connection first rectifying column of film；The reactor of catalyst filtration film is at least 2；Water filter with water filtration film is extremely
It is 1 less.
The catalyst filtration film is various tubulose stainless steel filter membranes.
The water filtration film is the collector tube that stainless steel filter membrane is connected with permeable membrane.
The catalyst is cationic catalysts reactive resin.
The reactor of the catalyst filtration film is 2~8.Preferably 3~5.
The water filter with water filtration film is 1~7.Preferably 2~4.
The reactor air speed is 0.2~1.5h-1.It is preferred that air speed is 0.4~0.5h-1。
80~150 DEG C of the reactor reaction temperature.Preferable reaction temperature is 115~125 DEG C.
The reactor reaction pressure 0.6MPa~4MPa.It is preferred that reaction pressure is 2~2.5MPa.
The mol ratio of the reactor dimethoxym ethane and metaformaldehyde is 1.5~4.Preferred molar ratio 2~3.
A kind of method of synthesizing polymethoxy methylal of the present invention, raw material dimethoxym ethane and metaformaldehyde are pre- by blender
Enter reactor of the First with catalyst filtration film by pipeline after heat to be reacted, entered after reaction by pipeline
Water filter with water filtration film, the water of the generation in course of reaction is discharged, and then entering next carry through piping urges
The reactor of agent filter membrane is reacted；Last reactor with catalyst filtration film passes through pipeline and the first rectifying
Tower is connected, and first rectifying column bottom is connected by pipeline with Second distillation column, and the top of first rectifying column passes through pipeline and reaction
Device is connected, and the bottom of Second distillation column is connected by pipeline with blender；Final product is obtained from Second distillation column top.
It is described as follows：
Certain series connection one carries water mistake between two reactors with catalyst filtration film of this device of the present invention
The water filter of filter membrane, charging aperture is connected with the reactor with catalyst filtration film, it is last be connected with first rectifying column be
Reactor with catalyst filtration film, the water filter with water filtration film is always than the reactor few one with catalyst filtration film
It is individual.The water produced in course of reaction, influence of the reduction water to reaction can be separated in time by way of this series connection.
The catalyst filtration film is various tubulose stainless steel filter membranes, and water filtration film is stainless steel filter membrane and permeable membrane
Some collector tubes being connected.
Using technological process as shown in Figure 1, Figure 2 and Figure 3, including reactor containing catalyst filtration film, with water
Water filter, rectifying column, blender and the pipeline of filter membrane.Raw material dimethoxym ethane A and metaformaldehyde B leads to after the preheating of blender 5
Cross pipeline to be reacted into reactor 1 of the First with catalyst filtration film, entered after reaction by pipeline and carried
The water filter 2 (without catalyst in the water filter wherein with water filtration film) of water filtration film arranges the water of the generation in course of reaction
Go out, then reacted through piping into next reactor 1 with catalyst filtration film；All reactors and drainage
Device is connected by pipeline, the filter that certain series connection one carries water filtration film between two reactors 1 with catalyst filtration film
Hydrophone 2, last reactor 1 with catalyst filtration film is connected by pipeline with first rectifying column 3, first rectifying column 3
Bottom is connected by pipeline with Second distillation column 4, and the top of first rectifying column 3 is connected by pipeline with reactor 1, the second rectifying
The bottom of tower 4 is connected by pipeline with blender 5；Final product is obtained from the top of Second distillation column 4.
In the inventive solutions, cationic catalysts reactive resin is used for catalyst, catalyst in operating process
All the time rest in the reactor with catalyst filtration film, using dimethoxym ethane and metaformaldehyde as reactant, under nitrogen atmosphere
Reacted.
Compared with prior art, the present invention has advantages below：Using the filter with catalyst filtration film and water filtration film
Hydrophone is connected, the water of the product of reaction in course of reaction is discharged in time by the water filter with water filtration film, it is to avoid water
Influence to reaction, improves production efficiency, while using the method for rectifying by n<3 and n>8 DMMnSeparation, is sent by pipeline
Into reactor, recycle.Substantially increase reaction conversion ratio and product DMM3-8Yield.
Brief description of the drawings
Fig. 1：2 reactors and 1 water filter tandem arrangement flow for carrying water filtration film with catalyst filtration film
Figure；
Fig. 2：3 reactors and 2 water filter tandem arrangement flows for carrying water filtration film with catalyst filtration film
Figure；
Fig. 3：5 reactors and 4 water filter tandem arrangement flows for carrying water filtration film with catalyst filtration film
Figure；
Wherein：1st, with catalyst filtration membrane reactor 2, with water filtration film water filter 3, first rectifying column 4,
Second distillation column 5, blender.
Embodiment
Technical scheme is further illustrated with reference to specific embodiment.
Embodiment 1：
Reference picture 1, has 2 reactors 1 and 1 water filter 2 with water filtration film with catalyst filtration film to connect.
Raw material enters after the mixing of blender 5 in reactor 1 of the First with catalyst filtration film, enters after reaction and carries water mistake
In the water filter 2 of filter membrane, except the water generated in dereaction, the material for water of then going out enters second with catalysis through piping
In the reactor of agent filter membrane.After the completion of reaction, crude product enters first rectifying column 3, the tower top of first rectifying column by pipeline
Reactor as First carries catalyst filtration film is connected, and bottom of towe is connected by the middle part of pipeline with Second distillation column 4,
The bottom of Second distillation column is connected by pipeline with blender 5, top output of the product from Second distillation column 4.
Added in reactor with catalyst filtration film in cationic catalysts reactive resin catalyst, control reactor
Temperature is 120 DEG C, and it is 1.5MPa to control reaction pressure, and the mol ratio for feeding dimethoxym ethane and metaformaldehyde is 2.5, the air speed of reaction
For 0.5h-1.The polymethoxy methylal crude product come out from reactor continuously enters first rectifying column and carries out rectifying, from the first essence
Evaporate the DMM that the top of tower comes outn(n<3) it is sent in reactor by pipeline, the products of rectifier bottoms is sent to the by pipeline
In two rectifying columns, the DMM flowed out from rectifier bottomsn(n>8) it is sent to by pipeline in reactor, final product is smart from second
Evaporate the top discharge of tower.Sampling, by gas chromatographic analysis, the conversion ratio of metaformaldehyde is 81.5%, DMMn(n=3~8)
Yield is 29.5%
Embodiment 2
With example 1, catalyst is cationic catalysts reactive resin, and it is 80 DEG C to control the temperature in reactor, is pressed in reactor
Power is 4MPa, and the mol ratio of charging dimethoxym ethane and metaformaldehyde is 4, and the air speed of reaction is 0.3h-1.The poly- first come out from reactor
Epoxide dimethoxym ethane crude product continuously enters first rectifying column and carries out rectifying, the DMM come out from the top of first rectifying columnn(n<3)
It is sent to by pipeline in reactor, the product of rectifier bottoms is sent in Second distillation column by pipeline, from rectifier bottoms stream
The DMM gone outn(n>8) it is sent to by pipeline in reactor, final product is discharged from the top of Second distillation column.Sampling, passes through
Gas chromatographic analysis, the yield that the conversion ratio of metaformaldehyde is 85.7%, DMMn (n=3~8) is 30.1%
Embodiment 3
The technique of present invention production polymethoxy methylal is with example 1, simply using 3 reactions for carrying catalyst filtration film
Device and 2 water filters with water filtration film are connected.As shown in Fig. 2 raw material is carried after the mixing of blender 5 into First
In the reactor 1 of catalyst filtration film, enter after reaction in the water filter 2 with water filtration film, except the water generated in dereaction,
Then the go out material of water enters in second reactor 1 with catalyst filtration film through piping.After the completion of reaction, pass through
Pipeline enters in second water filter 2 with water filtration film, further goes out the water generated in dereaction, subsequently into the 3rd
Reacted in reactor with catalyst filtration film.After the completion of reaction, crude product enters first rectifying column 3, first by pipeline
Reactor of the tower top of the rectifying column such as First with catalyst filtration film is connected, and bottom of towe passes through pipeline and Second distillation column 4
Middle part be connected, the bottom of Second distillation column is connected by pipeline with blender 5, and product is from the top of Second distillation column 4
Output.
Catalyst is temperature in cationic catalysts reactive resin, control reactor when reaching 150 DEG C, and reaction pressure is
The mol ratio of 0.6MPa, charging dimethoxym ethane and metaformaldehyde is 1.5, and the air speed of reaction is 1.5h-1.The poly- first come out from reactor
Epoxide dimethoxym ethane crude product continuously enters first rectifying column and carries out rectifying, the DMM come out from the top of first rectifying columnn(n<3)
It is sent to by pipeline in reactor, the product of rectifier bottoms is sent in Second distillation column by pipeline, from rectifier bottoms stream
The DMM gone outn(n>8) it is sent to by pipeline in reactor, final product is discharged from the top of Second distillation column.Sampling, passes through
Gas chromatographic analysis, the yield that the conversion ratio of metaformaldehyde is 90.5%, DMMn (n=3~8) is 31.2%
Embodiment 4
With example 3, catalyst is cationic catalysts reactive resin, and when control the temperature in reactor be 125 DEG C, control is reacted
Pressure is 2.5MPa, and the mol ratio of charging dimethoxym ethane and metaformaldehyde is 2, and the air speed of reaction is 0.4h-1.Come out from reactor
Polymethoxy methylal crude product continuously enters first rectifying column and carries out rectifying, the DMM come out from the top of first rectifying columnn(n
<3) it is sent to by pipeline in reactor, the product of rectifier bottoms is sent in Second distillation column by pipeline, from rectifier bottoms
The DMM of outflown(n>8) it is sent to by pipeline in reactor, final product is discharged from the top of Second distillation column.Sampling, warp
Gas chromatographic analysis is crossed, the yield that the conversion ratio of metaformaldehyde is 94.4%, DMMn (n=3~8) is 31.5%
Embodiment 5
The technique of present invention production polymethoxy methylal is with example 1, simply using 5 reactions for carrying catalyst filtration film
Device and 4 water filters with water filtration film are connected, as shown in Figure 3.Raw material is carried after the mixing of blender 5 into First
Enter in the reactor 1 of catalyst filtration film, after reaction in water filter 2 of the First with water filtration film, except raw in dereaction
Into water, the material of water of then going out enters in second reactor 1 with catalyst filtration film through piping.Reaction is completed
Afterwards, entered by pipeline in second water filter 2 with water filtration film, further go out the water generated in dereaction, Ran Houjin
Enter and reacted in the 3rd reactor 1 with catalyst filtration film.Then crude product enters the 3rd filter for carrying water filtration film
In hydrophone 2, further go out the water generated in dereaction.Then the 4th reaction for carrying catalyst filtration film is entered by pipeline
Entered in device 1, after reaction by pipeline in the 4th water filter 2 with water filtration film and remove the water generated in course of reaction,
Subsequently into reaction in the 5th anti-lead device 1 with catalyst filtration film.After the completion of reaction, crude product enters by pipeline
One rectifying column 3, reactor of the tower top such as First with catalyst filtration film of first rectifying column is connected, and bottom of towe passes through pipeline
It is connected with the middle part of Second distillation column 4, the bottom of Second distillation column is connected by pipeline with blender 5, product is from second
The top output of rectifying column 4.
Catalyst is cationic catalysts reactive resin, control temperature in reactor for 115 DEG C when, reaction pressure is
The mol ratio of 2MPa, charging dimethoxym ethane and metaformaldehyde is 3, and the air speed of reaction is 1h-1.The polymethoxy first come out from reactor
Acetal crude product continuously enters first rectifying column and carries out rectifying, the DMM come out from the top of first rectifying columnn(n<3) by pipe
Line is sent in reactor, and the product of rectifier bottoms is sent in Second distillation column by pipeline, is flowed out from rectifier bottoms
DMMn(n>8) it is sent to by pipeline in reactor, final product is discharged from the top of Second distillation column.Sampling, by gas phase
Chromatography, the yield that the conversion ratio of metaformaldehyde is 95.4%, DMMn (n=3~8) is 32.4%
Embodiment 6
The technique of present invention production polymethoxy methylal is with example 1, simply using 6 reactions for carrying catalyst filtration film
Device and 5 water filters with water filtration film are connected.Its connected mode is with feature as Fig. 1, Fig. 2, Fig. 3.
Catalyst is cationic catalysts reactive resin, and it is 150 DEG C to control the temperature in reactor, and pressure is 2.5MPa, is entered
The mol ratio for expecting dimethoxym ethane and metaformaldehyde is 2, and air speed during reaction is 0.2h-1.The polymethoxy first contracting come out from reactor
Aldehyde crude product continuously enters first rectifying column and carries out rectifying, the DMM come out from the top of first rectifying columnn(n<3) pipeline is passed through
It is sent in reactor, the product of rectifier bottoms is sent in Second distillation column by pipeline, the DMM flowed out from rectifier bottomsn
(n>8) it is sent to by pipeline in reactor, final product is discharged from the top of Second distillation column..Sampling, by gas-chromatography
Analysis, the conversion ratio of metaformaldehyde is 96.5%.DMMn (n=3~8) yield is 33.4%
Embodiment 7
The technique of present invention production polymethoxy methylal is with example 1, simply using 8 reactions for carrying catalyst filtration film
Device and 7 water filters with water filtration film are connected.Its connected mode is with feature as Fig. 1, Fig. 2, Fig. 3.
Catalyst is cationic catalysts reactive resin, and reaction pressure is 2MPa, mole of charging dimethoxym ethane and metaformaldehyde
Than for 2, reaction temperature is 150 DEG C, air speed during reaction is 0.5h-1.The polymethoxy methylal crude product come out from reactor
Continuously enter first rectifying column and carry out rectifying, the DMM come out from the top of first rectifying columnn(n<3) it is sent to reaction by pipeline
In device, the product of rectifier bottoms is sent in Second distillation column by pipeline, the DMM flowed out from rectifier bottomsn(n>8) pass through
Pipeline is sent in reactor, and final product discharges sampling from the top of Second distillation column.Sampling, by gas chromatographic analysis,
The conversion ratio of metaformaldehyde is 96.5%, DMMnThe yield of (n=3~8) is 33.5%.
Exemplary description is done to the present invention above, it should explanation, in the situation for the core for not departing from the present invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent substitution of creative work equal
Fall into protection scope of the present invention.
Claims (10)
1. a kind of device of synthesizing polymethoxy methylal；Including the reactor with catalyst filtration film and with water filtration film
Water filter；It is characterized in that the drainage that series connection one carries water filtration film between two reactors with catalyst filtration film
Device, first reactor with catalyst filtration film is provided with charging aperture, and last carries the reaction of catalyst filtration film
Device connects first rectifying column；The reactor of catalyst filtration film is at least 2；Water filter with water filtration film is at least 1.
2. device as claimed in claim 1, it is characterized in that the catalyst filtration film is various tubulose stainless steel filter membranes.
3. device as claimed in claim 1, is connected it is characterized in that the water filtration film is stainless steel filter membrane with permeable membrane
Collector tube.
4. device as claimed in claim 1, it is characterized in that the catalyst is cationic catalysts reactive resin.
5. device as claimed in claim 1, it is characterized in that the reactor of catalyst filtration film is 2~8.
6. device as claimed in claim 1, it is characterized in that the water filter with water filtration film is 1~7.
7. a kind of method of synthesizing polymethoxy methylal, it is characterized in that raw material dimethoxym ethane and metaformaldehyde are pre- by blender 5
Enter reactor of the First with catalyst filtration film by pipeline after heat to be reacted, entered after reaction by pipeline
Water filter with water filtration film, the water of the generation in course of reaction is discharged, and then entering next carry through piping urges
The reactor of agent filter membrane is reacted；Last reactor with catalyst filtration film passes through pipeline and the first rectifying
Tower is connected, and first rectifying column bottom is connected by pipeline with Second distillation column, and the top of first rectifying column passes through pipeline and reaction
Device is connected, and the bottom of Second distillation column is connected by pipeline with blender；Final product is obtained from Second distillation column top.
8. method as claimed in claim 7, it is characterized in that reactor air speed is 0.2~1.5h-1。
9. method as claimed in claim 7, it is characterized in that 80~150 DEG C of reactor reaction temperature；Reaction pressure 0.6MPa~
4MPa。
10. method as claimed in claim 7, it is characterized in that the mol ratio of reactor dimethoxym ethane and metaformaldehyde is 1.5~4.
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| EP2853524B1 (en) * | 2013-09-29 | 2017-08-02 | Suzhou OST Advanced Materials Co., Ltd. | Reaction system and process for preparing polymethoxy dimethyl ether |
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| CN201596496U (en) * | 2010-01-19 | 2010-10-06 | 河北瑞通美邦工程有限公司 | Cyclohexanone Ammoximation reactor |
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| EP2853524B1 (en) * | 2013-09-29 | 2017-08-02 | Suzhou OST Advanced Materials Co., Ltd. | Reaction system and process for preparing polymethoxy dimethyl ether |
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