CN104722249B - Multi-section reaction tower for polyoxymethylene dimethyl ether synthesis and polyoxymethylene dimethyl ether synthesis process unit - Google Patents
Multi-section reaction tower for polyoxymethylene dimethyl ether synthesis and polyoxymethylene dimethyl ether synthesis process unit Download PDFInfo
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- CN104722249B CN104722249B CN201510128444.8A CN201510128444A CN104722249B CN 104722249 B CN104722249 B CN 104722249B CN 201510128444 A CN201510128444 A CN 201510128444A CN 104722249 B CN104722249 B CN 104722249B
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 111
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 17
- 230000008569 process Effects 0.000 title claims abstract description 11
- -1 polyoxymethylene dimethyl ether Polymers 0.000 title abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 92
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 36
- 239000007789 gas Substances 0.000 claims description 27
- 239000000945 filler Substances 0.000 claims description 23
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 claims description 22
- 238000012856 packing Methods 0.000 claims description 12
- 239000007921 spray Substances 0.000 claims description 12
- 238000010521 absorption reaction Methods 0.000 claims description 11
- 239000012295 chemical reaction liquid Substances 0.000 claims description 10
- 239000007792 gaseous phase Substances 0.000 claims description 10
- 230000008676 import Effects 0.000 claims description 4
- 239000006096 absorbing agent Substances 0.000 claims description 3
- 238000005452 bending Methods 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 5
- 229920000642 polymer Polymers 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 33
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 12
- 235000019253 formic acid Nutrition 0.000 description 12
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 10
- 238000006555 catalytic reaction Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000007323 disproportionation reaction Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000002994 raw material 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
- 239000003513 alkali Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000002283 diesel fuel Substances 0.000 description 2
- 239000006280 diesel fuel additive Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229920002866 paraformaldehyde Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 238000005829 trimerization reaction Methods 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- KTFJRKWUACQCHF-UHFFFAOYSA-N dimethoxymethane;methanol Chemical compound OC.COCOC KTFJRKWUACQCHF-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002118 epoxides Chemical class 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Abstract
The invention discloses a multi-section reaction tower for polyoxymethylene dimethyl ether synthesis and a polyoxymethylene dimethyl ether synthesis process unit. A tower body of the multi-section reaction tower comprises at least two layers of reaction sections from top to bottom; each layer of reaction section is provided with a tower plate and forms a bent passageway; catalysts are arranged between the tower plates in a filling manner; gas ascension pipes are arranged between the adjacent layers of reaction sections; a gas phase outlet is formed in the tower top of the reaction tower; and each layer of reaction section is provided with an inlet with a valve and an outlet with a valve. According to the multi-section reaction tower for polyoxymethylene dimethyl ether synthesis and the polyoxymethylene dimethyl ether synthesis process unit, the conversion equilibrium point of the reaction is effectively controlled, the advancement of the reaction equilibrium toward bigger polymers is effectively deferred, the conversion rate and the selectivity are improved, the reaction is carried out under the conditions that the catalyst activity is relatively high and the temperature does not excessively influence the reaction equilibrium, and good conversion rate and selectivity are obtained.
Description
Technical field
The invention belongs to chemical production technology and equipment technical field, relate generally to the production of polymethoxy dimethyl ether
Process and device.
Background technology
The feature of China's energy resource structure is: rich coal, gas oil-poor, few, and the energy is needed by economic maintaining sustained and rapid growth
Ask increasing, the contradiction of society, expanding economy and oil supply.Since 2009, China
Crude oil external dependence degree exceedes warning line (50%) in continuous 6 years, has a strong impact on the energy strategy safety of China.From
China's energy strategy sets out safely, in conjunction with China's primary energy structure feature, Development of Coal base liquid fuel synthesis skill
Art has strategic significance undoubtedly.Additionally, China's methanol production capacity superfluous, exploitation Downstream Products of Methanol, prolong
Stretch Chemical Industry chain, all there is realistic meaning.
Polymethoxy dimethyl ether is a kind of universally acknowledged cleaning diesel oil component, its Cetane number >=70, does not contains
Sulfur, aromatic-free.Add in diesel oil in 5%-20% ratio, it is possible to increase diesel cetane-number, promote combustion
Burn, it will be apparent that reduce the discharge of the harmful gass such as PM2.5, PM10, NOx, CO in vehicle exhaust.Due to poly-
The excellent properties of methoxyl group dimethyl ether, its synthesis technique has become the heat subject of research both at home and abroad.At present, poly-
Methoxyl group dimethyl ether is with one or more in methanol or dimethoxym ethane and formalin/metaformaldehyde/many mostly
Polyformaldehyde reacts generation under the catalytic action of acidic catalyst.And this reaction is exothermic reaction, temperature height is made
Reaction is become inversely to carry out, it is therefore desirable to withdraw heat.Regardless of whether be paraformaldehyde or first metaformaldehyde needs
Heating parse monomer formaldehyde could participate in react, therefore system reaction temperature is the highest, typically 110 DEG C with
On, and the mode of pressurization must be used to prevent the relatively low dimethoxym ethane of boiling point and methanol gasifying, therefore cause energy consumption high,
Equipment requirements is high.It addition, under hot environment so, monomer formaldehyde has the highest activity, is susceptible to
Dismutation reaction produces substantial amounts of formic acid, if do not separated by formic acid in system, formic acid can be cumulative and right
The molecular balance of polymethoxy dimethyl ether brings significant negative impact, causes the yield of reaction to reduce, therefore can only
Use in absorption or alkali and acid stripping method separating formic, cause complex process, and target product yield is low, close
Become cost high.The selectivity of product DMMn3-8 and the amount of catalyst have close relationship, commonly fix
Bed cannot realize adjusting the product degree of polymerization, thus results in n value too small or excessive, affects product quality.Test
Prove to be best suitable for doing the product that the degree of polymerization is DMMn3-5 of 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 for polymethoxy two
The multisection type reaction tower of methyl ether and polymethoxy dimethyl ether synthesis technique device, solve at present with paraformaldehyde/
The cost that brings in trimerization production process is high, Synthesis conversion and the low problem of yield, and the present invention has well
Remove thermal effect and the fixed bed reactors of adjustable product transforming degree, reaction can be efficiently promoting and carry out, turn
Change degree achieves controllability.
Technical scheme: for achieving the above object, the present invention by the following technical solutions: a kind of for poly-first
The multisection type reaction tower of epoxide DME synthesis, described reaction tower tower body includes at least two-layer reaction from top to bottom
Section, and every layer of conversion zone be provided with column plate and constitute bending runner, is filled with catalyst, adjacent two layers between column plate
Conversion zone between be additionally provided with vapor riser, reaction tower tower top is additionally provided with gaseous phase outlet；Every layer of conversion zone is all provided with
There is the inlet and outlet of band valve.
As preferably, described conversion zone has four layers.
Present invention also offers the process unit of a kind of gas formaldehyde synthesis polymethoxy dimethyl ether, anti-including filler
Answer tower, product knockout tower and multisection type reaction tower, wherein:
Described filler reaction tower is provided with the packing section being filled with catalyst, is spray above and below packing section respectively
System and bubble absorption section, described filler reaction tower is additionally provided with the dimethoxym ethane entrance being connected with spray system and drum
Formaldehyde gas entrance, the first order reaction liquid outlet of bottom and the gaseous phase outlet at top that bubble absorber portion connects；Described
Bubble absorption section connects with dimethoxym ethane entrance also by pipeline pump；
The bottom first order reaction liquid outlet of described filler reaction tower and the entrance of product knockout tower (vacuum rectification tower)
Connecting, described product knockout tower also includes being located at products export, the gaseous phase outlet of tower top and the tower top at the bottom of tower
Light fraction outlet, the light fraction outlet on described tower top is connected with the import of multisection type reaction tower by pipeline, and
Dimethoxym ethane supply pipe it is additionally provided with on this passage；And the outlet of multisection type reaction tower is by pipeline and product knockout tower
Entrance connects.
As preferably, the products export of described product knockout tower is also associated with refined rectifying column (rectification under vacuum
Tower), this refined rectifying column also includes that being located at the heavy constituent at the bottom of tower exports, is located at the target product outlet of tower top,
The pipeline of this target product outlet is provided with condenser.
As preferably, the gaseous phase outlet of described product separation column is by the formaldehyde gas of pipeline with filler reaction tower
Body entrance connects.
Beneficial effect: compared with prior art, the invention have the advantages that and effectively make formaldehyde gas contract with first
Fully absorbing of aldehyde, it is achieved bubble absorption is integrated with catalytic reaction, improves the conversion ratio of formaldehyde；And utilize
Multisection type reaction tower, is effectively controlled the inversion equilibrium point of reaction, and effective prevention molecular balance is to the most poly-
The carrying out of laminate direction, improves conversion ratio and selectivity, makes reaction higher at catalyst activity and excessive shadow
Ring and carry out at a temperature of molecular balance, achieve good conversion ratio and selectivity.
Accompanying drawing explanation
Fig. 1 is the structural representation of the synthesis technique device of polymethoxy dimethyl ether of the present invention；
Fig. 2 is the structural representation of refined rectifying column process unit of the present invention.
Wherein, filler reaction tower 1, product knockout tower 2, multisection type reaction tower 3, refined rectifying column 4.
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 only used for
The present invention is described rather than limits the scope of the present invention, after having read the present invention, those skilled in the art
Amendment to the various equivalent form of values of the present invention all falls within the application claims limited range.
As it is shown in figure 1, the process unit of the gas formaldehyde synthesis polymethoxy dimethyl ether of the present invention, including filler
Reaction tower, product knockout tower and multisection type reaction tower, wherein:
Described filler reaction tower is provided with the packing section being filled with catalyst, is spray above and below packing section respectively
System and bubble absorption section, described filler reaction tower is additionally provided with the dimethoxym ethane entrance being connected with spray system and drum
Formaldehyde gas entrance, the first order reaction liquid outlet of bottom and the gaseous phase outlet at top that bubble absorber portion connects；Described
Bubble absorption section connects with dimethoxym ethane entrance also by pipeline pump；
The bottom first order reaction liquid outlet of described filler reaction tower and the entrance of product knockout tower (vacuum rectification tower)
Connecting, described product knockout tower also includes being located at products export, the gaseous phase outlet of tower top and the tower top at the bottom of tower
Light fraction outlet, the light fraction outlet on described tower top is connected with the import of multisection type reaction tower by pipeline, and
Dimethoxym ethane supply pipe it is additionally provided with on this passage；And the outlet of multisection type reaction tower is by pipeline and product knockout tower
Entrance connects.
Described multisection type reaction tower includes at least four layers of conversion zone from top to bottom, and every layer of conversion zone is provided with column plate also
Constitute bending runner (i.e. to set up hydraulic barrier, it is to avoid possible Biased flow phenomenon, add material on a catalyst
The time of staying), be filled with catalyst between column plate, be additionally provided with between the conversion zone of adjacent two layers gas rise
Pipe (so that gas phase connection), reaction tower tower top is additionally provided with gaseous phase outlet；Every layer of conversion zone is equipped with band valve
The inlet and outlet of door.
The products export of described product knockout tower is also associated with refined rectifying column (vacuum rectification tower), this refined essence
Evaporating tower and also include that being located at the heavy constituent at the bottom of tower exports, is located at the target product outlet of tower top, this target product exports
Pipeline be provided with condenser.
The present invention with pure formaldehyde gas and dimethoxym ethane as raw material, high-temperature anhydrous formaldehyde gas and 90%--99% concentration first
Acetal enters from the bottom of filler reaction tower and top respectively, and formaldehyde gas, after bubble absorption, is not inhaled
The part received rises through packing material absorbing section, now sprays out fresh dimethoxym ethane solution in spray system and from tower
The dimethoxym ethane containing formaldehyde gas come on end pump.And the first half of the packing material absorbing section in tower is equipped with catalysis
Agent, spray and under formalin absorb further in packing section with the formaldehyde gas not fully absorbed, and carry out
Catalytic reaction generates polymethoxy dimethyl ether, and now the operation temperature of filler reaction tower is 40～100 DEG C, pressure
For normal pressure～0.5MPa, relatively low reaction temperature can suppress the formic acid that the dismutation reaction of formaldehyde generates, it is thus possible to carry
The conversion ratio of high formaldehyde, promotes the forward reaction of polymethoxy dimethyl ether.From the initial reaction of filler reaction tower,
Obtaining the I order reaction liquid at the bottom of tower, component comprises formaldehyde 5-30%, and DMM1 contains 10-containing 40-60%, DMM3-8
20%.Tower top withdraws the heat that reaction heat, absorption heat and formaldehyde self bring.Multisection type reaction tower of the present invention
Using four sections of shunting means, liquid phase can be by Valve controlling, it is achieved series-parallel freely change, and gas phase phase
Logical so that the dimethoxym ethane that can volatilize, to tower top, takes away heat of reaction, promotes moving to right of balance.Therefore, many
Segmentation reaction tower four sections can realize being used in series between any two by valve opening and closing.It is effectively controlled reaction
Inversion equilibrium point, especially in catalyst activity changes, it is achieved utilize catalysis efficiently.
With pure formaldehyde gas and dimethoxym ethane as raw material, high-temperature anhydrous formaldehyde gas divides with 90%--99% concentration dimethoxym ethane
Not do not enter from the bottom of filler reaction tower and top, formaldehyde gas after bubble absorption, unabsorbed portion
Divide and rise through packing material absorbing section, spray system now sprays out fresh dimethoxym ethane solution and from column bottoms pump
And the dimethoxym ethane containing formaldehyde gas come.And the first half of the packing material absorbing section in tower is equipped with catalyst, spray
Formalin under and absorbs in packing section further with the formaldehyde gas not fully absorbed, and carries out catalytic reaction
Generate polymethoxy dimethyl ether, now the operation temperature of filler reaction tower is 40～100 DEG C, pressure be normal pressure-
0.5MPa, relatively low reaction temperature can suppress the formic acid that the dismutation reaction of formaldehyde generates, it is thus possible to improve formaldehyde
Conversion ratio, promotes the forward reaction of polymethoxy dimethyl ether.Additionally in reaction system, formic acid also carries with dimethoxym ethane
Methanol carry out esterification, and by the tower top of filler reaction tower with the form fractionation of gas methyl formate
Go out, such that it is able to avoid formic acid accumulation maintenance system in formic acid content a relatively low content under, it is achieved
The catalytic distillation mode that production limit, limit separates.And the formic acid of the poly/trimerization/formalin used in commonsense method
Too much, it is impossible to only by the way of methyl formate, remove formic acid and maintain the forward reaction of polymethoxy dimethyl ether,
Along with the formic acid content that carries out of reaction is gradually increased and causes the conversion ratio of reaction to reduce rapidly, alkali therefore can only be used
Neutralize or the way removing formic acid of adsorption deacidification, the problem having resulted in environmental pollution and waste of raw materials.
I order reaction liquid enters product knockout tower, and the product of extraction DMM3-8 at the bottom of tower, in the middle part of tower, extraction does not meets product
The light component that product require, this light component comprises in the middle of the DMM1 participating in reaction the most completely, formaldehyde, methanol and reaction
Component DMM2.The light component of this part through with dimethoxym ethane again dispensing after, enter 4 grades of multisection type reaction towers.II
Order reaction liquid component comprises formaldehyde 5-15%, and DMM1 contains 20-40% containing 30-50%, DMM3-8.II order reaction liquid
Pump into product knockout tower, take out the semi-finished product of DMM3-8, and it is refined it to be reduced pressure in refined rectifying column, takes
Must be more suitable for doing the product of the DMM3-5 of diesel fuel additives.The composition of the DMMn ＞ 5 that component is relatively heavy returns
Returning multisection type reaction tower, effective prevention molecular balance, to the carrying out in bigger polymer direction, improves conversion ratio
And selectivity.Solve the uppity problem of fixed bed reactors temperature, effectively raise what reaction was carried out
Degree.
Meanwhile, condensation is first passed through, at warp from the dimethoxym ethane gas containing methyl formate of filler reaction tower extraction
The mode of compression rectification isolates highly purified methyl formate as by-product, and the dimethoxym ethane of the separation at the bottom of tower is then
Returning to again filler reaction tower and continue reaction, methyl formate recovery tower operation temperature 40 DEG C-100 DEG C, pressure is normal
Pressure-0.8MPa.
Claims (3)
1. the process unit of a gas formaldehyde synthesis polymethoxy dimethyl ether, it is characterised in that: include filler
Reaction tower, product knockout tower and multisection type reaction tower, wherein:
Described filler reaction tower is provided with the packing section being filled with catalyst, is spray above and below packing section respectively
System and bubble absorption section, described filler reaction tower is additionally provided with the dimethoxym ethane entrance being connected with spray system and drum
Formaldehyde gas entrance, the first order reaction liquid outlet of bottom and the gaseous phase outlet at top that bubble absorber portion connects；Described
Bubble absorption section connects with dimethoxym ethane entrance also by pipeline pump；
The bottom first order reaction liquid outlet of described filler reaction tower is connected with the entrance of product knockout tower, described product
Knockout tower also includes products export, the gaseous phase outlet of tower top and the light fraction outlet on tower top being located at the bottom of tower, institute
The light fraction outlet stating tower top is connected with the import of multisection type reaction tower by pipeline, and is additionally provided with on this pipeline
Dimethoxym ethane supply pipe；And the outlet of multisection type reaction tower is connected by the entrance of pipeline with product knockout tower；
Described multisection type reaction tower tower body includes at least two-layer conversion zone from top to bottom, and every layer of conversion zone is provided with tower
Plate also constitutes bending runner, is filled with catalyst, is additionally provided with gas between the conversion zone of adjacent two layers between column plate
Tedge, multisection type reaction tower tower top is additionally provided with gaseous phase outlet；Every layer of conversion zone be equipped with band valve import and
Outlet；Described conversion zone has four layers.
Process unit the most according to claim 1, it is characterised in that: the product of described product knockout tower goes out
Mouth is also associated with refined rectifying column, and this refined rectifying column also includes that being located at the heavy constituent at the bottom of tower exports, is located at tower top
Target product outlet, this target product outlet pipeline be provided with condenser.
Process unit the most according to claim 1, it is characterised in that: the gas of described product separation column
Export mutually and connected with the formaldehyde gas entrance of filler reaction tower by pipeline.
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| CN201510128444.8A CN104722249B (en) | 2015-03-24 | 2015-03-24 | Multi-section reaction tower for polyoxymethylene dimethyl ether synthesis and polyoxymethylene dimethyl ether synthesis process unit |
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| CN105601479B (en) * | 2016-02-03 | 2017-12-08 | 陕西恒华能源科技有限公司 | A kind of preparation method of polymethoxy dimethyl ether |
| CN105693479A (en) * | 2016-03-15 | 2016-06-22 | 江苏凯茂石化科技有限公司 | Process device special for preparing polyoxymethylene dimethyl ethers through formaldehyde gas |
| CN107285999A (en) * | 2017-07-13 | 2017-10-24 | 湖北三里枫香科技有限公司 | A kind of alkyl polyoxyether DMMn reaction tower and manufacturing technique method |
| CN107445808B (en) * | 2017-09-08 | 2022-05-20 | 青岛迈特达新材料有限公司 | Process and system for preparing poly-methoxy-dimethyl ether |
| CN107522601B (en) * | 2017-09-08 | 2022-08-23 | 青岛迈特达新材料有限公司 | Polyoxymethylene dimethyl ether separation device and process |
| CN107721831B (en) * | 2017-11-08 | 2023-05-16 | 无锡赫利邦化工科技有限公司 | Bubbling externally hung reaction system for synthesizing polymethoxy dimethyl ether and synthesis method |
| CN109232202B (en) * | 2018-11-08 | 2024-02-06 | 凯瑞环保科技股份有限公司 | One-step method for synthesizing DMM 3-8 Apparatus and method of (2) |
| CN110090464A (en) * | 2019-04-16 | 2019-08-06 | 天津大学 | Partition wall reactive distillation method and device for polymethoxy dimethyl ether synthesis |
| CN110078598B (en) * | 2019-04-16 | 2023-06-30 | 天津大学 | Multi-stage reactive distillation synthesis process method and device for polymethoxy dimethyl ether |
| CN110156575B (en) * | 2019-04-17 | 2023-06-06 | 天津大学 | Reactive distillation-vapor permeation coupling process for polymethoxy dimethyl ether synthesis |
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| US7534922B2 (en) * | 2004-12-13 | 2009-05-19 | Ticona Gmbh | Processes for the manufacture of acetals |
| CN102249868A (en) * | 2010-05-18 | 2011-11-23 | 中国科学院兰州化学物理研究所 | Technical process for preparing polymethoxy dimethyl ether by subjecting formaldehyde and methanol to acetalation reaction |
| CN102249869A (en) * | 2010-05-18 | 2011-11-23 | 中国科学院兰州化学物理研究所 | Technical process for catalytically synthesizing polymethoxy dimethyl ether by ionic liquid |
| CN102371079B (en) * | 2010-08-09 | 2015-01-21 | 江苏凯茂石化科技有限公司 | High concentration methylal pressure distillation process and preparation device thereof |
| CN103772163B (en) * | 2012-10-18 | 2016-04-13 | 中国科学院兰州化学物理研究所 | The reactive system of continuous production polymethoxy dimethyl ether and processing method |
| CN104230854A (en) * | 2013-06-17 | 2014-12-24 | 中国石油化工股份有限公司 | Cumyl hydroperoxide and propylene epoxidation method for preparing epoxypropane |
| CN203677977U (en) * | 2014-01-06 | 2014-07-02 | 山东辰信新能源有限公司 | Reactive distillation column and device for preparing methylal |
| CN204685069U (en) * | 2015-03-24 | 2015-10-07 | 江苏凯茂石化科技有限公司 | A kind of multisection type reaction tower for polymethoxy dimethyl ether synthesis and polymethoxy dimethyl ether synthesis technique device |
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