CN106278836A - Intermediate concentration formaldehyde and the apparatus and method of methylal synthesis polymethoxy dimethyl ether - Google Patents
Intermediate concentration formaldehyde and the apparatus and method of methylal synthesis polymethoxy dimethyl ether Download PDFInfo
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- CN106278836A CN106278836A CN201610671732.2A CN201610671732A CN106278836A CN 106278836 A CN106278836 A CN 106278836A CN 201610671732 A CN201610671732 A CN 201610671732A CN 106278836 A CN106278836 A CN 106278836A
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 91
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 title claims abstract description 70
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 19
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 19
- 230000003068 static effect Effects 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 238000007670 refining Methods 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 239000011973 solid acid Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 239000000110 cooling liquid Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 238000005265 energy consumption Methods 0.000 abstract description 9
- 238000002156 mixing Methods 0.000 abstract description 8
- 238000000746 purification Methods 0.000 abstract description 6
- 229920000642 polymer Polymers 0.000 abstract description 4
- 238000005530 etching Methods 0.000 abstract description 3
- 238000005299 abrasion Methods 0.000 abstract 1
- 239000003245 coal Substances 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000002283 diesel fuel Substances 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical compound C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 description 2
- 229930040373 Paraformaldehyde Natural products 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 229920002866 paraformaldehyde Polymers 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010959 commercial synthesis reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000013461 design 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
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical compound [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 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
- C07C41/50—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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to production method and the device of polymethoxy dimethyl ether, it is specially the apparatus and method of intermediate concentration formaldehyde and methylal synthesis polymethoxy dimethyl ether, solve existing apparatus structure complexity, operation expense is high, energy consumption is high, yield is low, be unfavorable for industrialization quantity-produced problem, scheme is: device includes static mixer, one termination is connected with input pipe, another termination is connected with pipeline reactor, and the other end of reactor is connected with refine separation equipment.Catalyst is filled out in method: a, reactor；Mix homogeneously in b, raw material input mixer；C, feedstock transportation enter reactor, control temperature, pressure, liquid volume air speed；D, refining spearation.Advantage: energy consumption is lower, production capacity is high, be applicable to maximize and continuous prodution, back-mixing are little, sectional temperature control, catalyst abrasion rate are low, can be easily separated, not etching apparatus, subsequent treatment is simple, pollute less, selectivity is high, production cost is low, high polymer is few, separation and purification energy consumption is low in product.
Description
Technical field
The present invention relates to Coal Chemical Industry application, particularly relate to produce preparation method and the device of polymethoxy dimethyl ether,
It is specially the apparatus and method of intermediate concentration formaldehyde and methylal synthesis polymethoxy dimethyl ether.
Background technology
Coal Energy Source as the important component part of China's energy resource structure, for guarantee China's the energy safety of supply have to
Close important effect, and Chemical Industry is as realizing the effective means that Coal Energy Source efficiently utilizes.Development of Novel Coal Chemical Industry can
Petroleum chemicals are substituted, for ensureing that national energy security has important strategic importance with part.(it leads to polymethoxy dimethyl ether
Formula is CH3O(CH2O)nCH3, wherein, the integer of n >=1, general value is less than 8, hereafter uses DMMnRepresent) it is that one does not contains
Sulfur, aromatic free cleaning diesel component, be also a kind of high added value product of New Coal Chemical.DMMnPhysical property and diesel oil phase
Closely, it is blended in diesel oil and is used without the engine fuel system of In-Use Motor Vehicles is made any change.Diesel oil adds
10% ~ 20%, it is possible to decrease the exhaust pollutant of 20 ~ 50%, CO, uncombusted HC compound, especially particulate matter PM are greatly reduced
Discharge, is the environmental protection fuel oil component generally acknowledged the most in the world.
Produce at present polymethoxy dimethyl ether and mainly have paste state bed reactor and fixed bed reactors:
Utilize paste state bed reactor to have the disadvantage in that 1 when producing polymethoxy dimethyl ether, in paste state bed reactor reaction close
In complete mixing flow, after reaction reaches balance, it is difficult to the direction to generating product and moves, DMMnEquilibrium composition can only achieve 38-53%
Between；2, the intermittent slurry reactor charging discharge time is long, unfavorable industrialized production；3, seriality slurry reactor is used
Device, if using series connection still number few, then must have a number of unreacted material directly to flow out from last still, due to this
The particularity of reaction, if reaction raw materials unreacted is expelled directly out, then can bring the biggest trouble to subsequent filter and refining step；
If using series connection still number many, then can greatly increase investment and operating cost, be unfavorable for industrialization；4, due to paste state bed reactor
The stirring paddle serious wear to catalyst, the raising of catalyst cost can be directly contributed.
Utilize fixed bed reactors to have the disadvantage in that 1 when producing polymethoxy dimethyl ether, conventional internal structure fixing
Bed heat transfer is poor, and structure is complicated, is unfavorable for maintenance, and brings burden for subsequent separation process；2, traditional mode of production polymethoxy
Dimethyl ether uses concentrated formaldehyde, metaformaldehyde or paraformaldehyde to be that raw material is prepared with dimethoxym ethane or other raw materials, its raw material
Complicated process of preparation, energy consumption is higher, and unit scale is relatively big, and industrialized production investment is bigger.
At present the process of commercial synthesis polymethoxy dimethyl ether all uses concentrated formaldehyde, metaformaldehyde, the paraformaldehyde to be
Raw material, because of formaldehyde concentration and evaporation, inevitably improves production cost, produces while also result in there being substantial amounts of high polymer in product
Raw, target product polymethoxy dimethyl ether yield reduces.
As can be seen here, a kind of simple in construction of design, be easy to safeguard, invest little, unit scale is moderate, energy consumption is low, Neng Goulian
Device and the process of the polymethoxy dimethyl ether of high, the applicable industrialization continuous prodution of continuous discharge, efficiency of pcr product are very
It is necessary.
Summary of the invention
The present invention solves the apparatus structure complexity of existing production polymethoxy dimethyl ether, operation expense height, energy consumption
High, yield is low, be unfavorable for industrialization quantity-produced problem, it is provided that a kind of intermediate concentration formaldehyde and methylal synthesis polymethoxy
The apparatus and method of dimethyl ether.
The present invention is achieved by the following technical solutions: intermediate concentration formaldehyde and methylal synthesis polymethoxy dimethyl ether
Device, including horizontally disposed tubular static mixer, described static mixer one termination connects two raw material input pipes,
Top, described static mixer one end is provided with steam inlet, and other end bottom is provided with cooling liquid outlet, and described static mixer is another
One termination connects the multitube parallel pipeline reactor arranged from the bottom to top having each pipe horizontally disposed, described static mixing
Device is connected with the infraoral of pipeline reactor, and the connection end bottom of described pipeline reactor and static mixer is provided with coolant and goes out
Mouthful, the top of the described pipeline reactor other end is provided with steam inlet, and the other end of described pipeline reactor connects has refine to divide
From equipment.Horizontally disposed tubular static mixer makes reactant be sufficiently mixed.The molecule of reactant is in tubular reactor
The time of staying is equal, and in reactor, the reactant concentration on any point and chemical reaction velocity all do not change over time, only with
Pipe range changes.
Intermediate concentration formaldehyde and the method for methylal synthesis polymethoxy dimethyl ether, including following operating procedure: a, manage
The straight length of road reactor fills superpower solid acid catalyst；B, by the formalin of intermediate concentration and dimethoxym ethane by two
Raw material input pipe is added separately to mix homogeneously in static mixer；C, the reaction raw materials of mix homogeneously is delivered into by pipeline
Entering in pipeline reactor, controlling pipeline reactor temperature constant everywhere is 70 ~ 150 DEG C, and reaction pressure is 0.1 ~ 1.0MPa, regulation
Feed flow rate makes liquid volume air speed in pipeline reactor be 0.2 ~ 0.5h-1；D, material through pipeline reactor react after by pipeline
Reactor upper oral part is delivered to refining spearation equipment to carry out separating and refining.
The formalin concentration of the intermediate concentration in described step B input static mixer is 55% mass fraction.Described
Dimethoxym ethane in b step input static mixer is 1 ~ 4:1 with the mol ratio of formaldehyde in the formalin of intermediate concentration.Use
Superpower solid acid catalyst can be substantially reduced the wear rate of catalyst, easily separate with liquid reaction system, not etching apparatus, after
Environment, selectivity height simply, are seldom polluted in continuous process.Polymethoxy is prepared for raw material with the formalin of 55% mass fraction
Dimethyl ether, not only reduces the high production cost problem that extensive formaldehyde concentration and evaporation brings, and solves at synthesis polymethoxy simultaneously
The appearance of high polymerization degree polymer during dimethyl ether, solves the high energy consumption problem during separation and purification.
The process units of the present invention and process and existing production polymethoxy dimethyl ether device and process phase
Ratio has the advantage that 1, tubular reactor volume is little, specific surface big, the heat transfer area of unit volume is big, energy consumption is lower；2, anti-
Answer that thing response speed in tubular reactor is fast, flow velocity is fast, production capacity is high；3, tubular reactor is more suitable for maximizing and connecting
The commercial production of continuousization；4 compared with tank reactor, its back-mixing less；5, tubular reactor is not only suitable for liquid phase reactor,
It is applicable to again gas phase reaction, especially suitable for compressive reaction；6, tubular reactor can realize two-stage temperature control；7, use is super
Strong solid acids catalyst can be substantially reduced the wear rate of catalyst, easily separates with liquid reaction system, not etching apparatus, follow-up
Process and simply, seldom pollute environment, selectivity height；8, the formalin using intermediate concentration is raw material, reduces extensive formaldehyde
The high production cost problem that concentration and evaporation brings, solves high polymerization degree polymer during synthesis polymethoxy dimethyl ether simultaneously
Appearance, solve the high energy consumption problem during separation and purification.
Accompanying drawing explanation
Fig. 1 is the structure diagram of invention synthesis polymethoxy dimethyl ether device reaction device；
In figure: 1-static mixer, 2-raw material input pipe, 3-pipeline reactor.
Detailed description of the invention
Intermediate concentration formaldehyde and the device of methylal synthesis polymethoxy dimethyl ether, mix including horizontally disposed tubular type static state
Clutch 1, described static mixer 1 one termination connects has two raw material input pipes 2, top, described static mixer 1 one end to be provided with
Steam inlet, other end bottom is provided with cooling liquid outlet, and described another termination of static mixer 1 connects has each pipe in the horizontal direction
The multitube parallel pipeline reactor 3 arranged from the bottom to top arranged, described static mixer 1 and the infraoral of pipeline reactor 3
Connecting, described pipeline reactor 3 is provided with cooling liquid outlet with the connection end bottom of static mixer 1, and described pipeline reactor 3 is another
The top of one end is provided with steam inlet, and the other end of described pipeline reactor 3 connects refine separation equipment.
Embodiment one: intermediate concentration formaldehyde and the method for methylal synthesis polymethoxy dimethyl ether, walks including following operation
Rapid: a, pipeline reactor straight length fill superpower solid acid catalyst；B, by formalin that mass fraction is 55% with
Dimethoxym ethane is added separately to mix homogeneously in static mixer according to mol ratio 1:1 by two raw material input pipes；C, general's mixing
Uniform reaction raw materials delivers in pipeline reactor by pipeline, and controlling pipeline reactor temperature constant everywhere is 100 DEG C,
Reaction pressure is 1.0MPa, and regulation feed flow rate makes liquid volume air speed in pipeline reactor be 0.3h-1；D, material are anti-through pipeline
It is delivered to refining spearation equipment by pipeline reactor upper oral part after answering device reaction carry out separating and refining.To the product after separation and purification
Thing is analyzed, and in detection equilibrium products, the content of each degree of polymerization polymethoxy dimethyl ether, the results are shown in Table 1.
Embodiment two: intermediate concentration formaldehyde and the method for methylal synthesis polymethoxy dimethyl ether, walks including following operation
Rapid: a, pipeline reactor straight length fill superpower solid acid catalyst；B, by formalin that mass fraction is 55% with
Dimethoxym ethane is added separately to mix homogeneously in static mixer according to mol ratio 1:2 by two raw material input pipes；C, general's mixing
Uniform reaction raw materials delivers in pipeline reactor by pipeline, and controlling pipeline reactor temperature constant everywhere is 150 DEG C,
Reaction pressure is 0.4MPa, and regulation feed flow rate makes liquid volume air speed in pipeline reactor be 0.4h-1；D, material are anti-through pipeline
It is delivered to refining spearation equipment by pipeline reactor upper oral part after answering device reaction carry out separating and refining.To the product after separation and purification
Thing is analyzed, and in detection equilibrium products, the content of each degree of polymerization polymethoxy dimethyl ether, the results are shown in Table 1.
Embodiment three: intermediate concentration formaldehyde and the method for methylal synthesis polymethoxy dimethyl ether, walks including following operation
Rapid: a, pipeline reactor straight length fill superpower solid acid catalyst；B, by formalin that mass fraction is 55% with
Dimethoxym ethane is added separately to mix homogeneously in static mixer according to mol ratio 1:4 by two raw material input pipes；C, general's mixing
Uniform reaction raw materials delivers in pipeline reactor by pipeline, and controlling pipeline reactor temperature constant everywhere is 70 DEG C,
Reaction pressure is 0.7MPa, and regulation feed flow rate makes liquid volume air speed in pipeline reactor be 0.2h-1；D, material are anti-through pipeline
It is delivered to refining spearation equipment by pipeline reactor upper oral part after answering device reaction carry out separating and refining.To the product after separation and purification
Thing is analyzed, and in detection equilibrium products, the content of each degree of polymerization polymethoxy dimethyl ether, the results are shown in Table 1.
Embodiment four: intermediate concentration formaldehyde and the method for methylal synthesis polymethoxy dimethyl ether, walks including following operation
Rapid: a, pipeline reactor straight length fill superpower solid acid catalyst；B, by formalin that mass fraction is 55% with
Dimethoxym ethane is added separately to mix homogeneously in static mixer according to mol ratio 1:3 by two raw material input pipes；C, general's mixing
Uniform reaction raw materials delivers in pipeline reactor by pipeline, and controlling pipeline reactor temperature constant everywhere is 120 DEG C,
Reaction pressure is 0.1MPa, and regulation feed flow rate makes liquid volume air speed in pipeline reactor be 0.5h-1；D, material are anti-through pipeline
It is delivered to refining spearation equipment by pipeline reactor upper oral part after answering device reaction carry out separating and refining.To reaction except putting down after water
Weighing apparatus product is analyzed, and the results are shown in Table 1.
Table 1 product composition (%)
| Component | Embodiment one | Embodiment two | Embodiment three | Embodiment four |
| Methanol | 3.66 | 3.23 | 2.03 | 2.95 |
| Formaldehyde | 7.15 | 6.98 | 5.56 | 7.11 |
| Dimethoxym ethane | 35.33 | 33.83 | 22.41 | 23.39 |
| DMM2 | 21.05 | 22.14 | 25.87 | 27.10 |
| DMM3 | 13.98 | 14 | 19.34 | 17.68 |
| DMM4 | 7.66 | 8.32 | 10.63 | 9.04 |
| DMM5 | 4.28 | 4.42 | 5.79 | 5.49 |
| DMM6 | 3.71 | 3.78 | 4.83 | 3.90 |
| DMM7 | 2.01 | 2.01 | 2.19 | 2.11 |
| DMM8 | 1.17 | 1.29 | 1.35 | 1.23 |
| ∑DMM2-8 | 53.86 | 55.96 | 70 | 66.55 |
Claims (4)
1. an intermediate concentration formaldehyde and the device of methylal synthesis polymethoxy dimethyl ether, it is characterised in that: include that level sets
The tubular static mixer (1) put, described static mixer (1) termination connects two raw material input pipes (2), described static state
Blender (1) top, one end is provided with steam inlet, and other end bottom is provided with cooling liquid outlet, described static mixer (1) another
Termination connects the multitube parallel pipeline reactor (3) arranged from the bottom to top having each pipe horizontally disposed, and described static state is mixed
Clutch (1) is connected with the infraoral of pipeline reactor (3), under the connection end of described pipeline reactor (3) and static mixer (1)
Portion is provided with cooling liquid outlet, and the top of described pipeline reactor (3) other end is provided with steam inlet, described pipeline reactor (3)
The other end connect have refine separation equipment.
2. an intermediate concentration formaldehyde and the method for methylal synthesis polymethoxy dimethyl ether, it is characterised in that: include following behaviour
Make step: a, pipeline reactor straight length fill superpower solid acid catalyst；B, by the formalin of intermediate concentration with
Dimethoxym ethane is added separately to mix homogeneously in static mixer by two raw material input pipes；C, by the reaction raw materials of mix homogeneously
Delivering in pipeline reactor by pipeline, controlling pipeline reactor temperature constant everywhere is 70 ~ 150 DEG C, and reaction pressure is
0.1 ~ 1.0MPa, regulation feed flow rate makes liquid volume air speed in pipeline reactor be 0.2 ~ 0.5h-1；D, material are through pipe reaction
It is delivered to refining spearation equipment by pipeline reactor upper oral part after device reaction carry out separating and refining.
Intermediate concentration formaldehyde the most according to claim 2 and the method for methylal synthesis polymethoxy dimethyl ether, its feature
It is: the formalin concentration of the intermediate concentration in described step B input static mixer is 55% mass fraction.
4., according to the method for the intermediate concentration formaldehyde described in Claims 2 or 3 Yu methylal synthesis polymethoxy dimethyl ether, it is special
Levy and be: the dimethoxym ethane in described b step input static mixer and the mol ratio of formaldehyde in the formalin of intermediate concentration
It is 1 ~ 4:1.
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| CN201610671732.2A CN106278836A (en) | 2016-08-16 | 2016-08-16 | Intermediate concentration formaldehyde and the apparatus and method of methylal synthesis polymethoxy dimethyl ether |
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Cited By (5)
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| CN107626277A (en) * | 2017-11-02 | 2018-01-26 | 南通海珥玛科技股份有限公司 | A kind of multi-stage pipeline reaction unit and method for being used to produce epoxidized soybean oil |
| CN109384652A (en) * | 2017-08-07 | 2019-02-26 | 中国石化扬子石油化工有限公司 | The synthetic method and application of polyethoxy dimethyl ether |
| 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 |
| CN112169711A (en) * | 2020-09-26 | 2021-01-05 | 安徽金禾实业股份有限公司 | A kind of thionyl chloride sulfur mixing system continuous sulfur adding device and method |
| CN112794793A (en) * | 2021-04-14 | 2021-05-14 | 维思普新材料（苏州）有限公司 | Method for preparing 9, 10-dialkoxyanthracene |
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| CN112794793A (en) * | 2021-04-14 | 2021-05-14 | 维思普新材料（苏州）有限公司 | Method for preparing 9, 10-dialkoxyanthracene |
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