CN205556511U - Production gathers methoxy dimethyl ether DMM3 -5's device - Google Patents
Production gathers methoxy dimethyl ether DMM3 -5's device Download PDFInfo
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- CN205556511U CN205556511U CN201620189729.2U CN201620189729U CN205556511U CN 205556511 U CN205556511 U CN 205556511U CN 201620189729 U CN201620189729 U CN 201620189729U CN 205556511 U CN205556511 U CN 205556511U
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Abstract
The utility model discloses a does production gather methoxy dimethyl ether DMM3 5 the device, take off tower, extraction catalytic distillation tower, decomposition tower and fractionating system including consecutive methanol oxidation ware, heat exchanger, essence: upper portion be extraction section, middle part to be catalysis section, lower part is distilling period in extraction distillation column's the tower, and extraction section and distilling period structure and traditional filler extraction tower perhaps traditional perforated -plate extraction tower structure are the same, load catalyst in bulk or module catalyst in the catalysis section, and the extraction distillation column gas collection extracts mutually, liquid phase catalysis, liquid phase are distilled in an organic whole. The device compares with current technology, has saved a large amount of equipment, pipeline, internals facility, process flow has been optimized, saved the investment, reduced manufacturing cost, the energy saving and emission reduction of maximize, produce for maximization, serialization, intensification and laid solid foundation.
Description
Technical field
This utility model relates to a kind of device producing polymethoxy dimethyl ether DMM3-5, with ferrum molybdenum method or silver method (hereinafter referred to as
Two methods) product containing formaldehyde produced as initiation material, be passed into after heat exchange, loss of essence water and there is gaseous extraction, liquid phase
Catalysis, liquid phase are distilled and are carried out polycondensation reaction in the extraction catalytic distillation tower of one.
Background technology
It is pure formaldehyde raw material owing to producing the primary raw material of polymethoxy dimethyl ether, again due to the character of formaldehyde raw material, often
It is gas under temperature and is easily polymerized, be the most all presented in its aqueous solution or its polymer.Such as paraformaldehyde
Or the solid form of metaformaldehyde exists, therefore during producing polymethoxy dimethyl ether, or by its aqueous solution through one it is
The process of row, as concentrated, extraction (from aqueous solution extract), be dehydrated, the way such as parsing, and obtain pure from its aqueous solution
Clean formaldehyde raw material；Or by formalin through pervaporation, the paraformaldehyde that concentrates, be polymerized, be dried and obtain or trimerization first
Aldehyde, then dissolved with dimethoxym ethane, then it is passed through reactor to synthesize polymethoxy dimethyl ether.Above method or from formalin
(i.e. liquid phase method) or the method producing DMMn (n >=1) from polyformaldehyde (i.e. solid phase method), its flow process is tediously long, process is complicated,
The wasting of resources.Such as patent CN104722249A, CN204569778u, CN10506165A, CN204874344u.
Summary of the invention
Technical problem to be solved in the utility model is for the deficiencies in the prior art, and provides a kind of and produce poly-methoxy
The device of base dimethyl ether DMM3-5, the gas-phase product containing formaldehyde produced using two methods is as initiation material, without absorption tower
(not the most being prepared as aqueous solution), but discharge from the outlet of methanol oxidation device, after heat exchange, loss of essence water, it is passed into and has
Gaseous extraction, liquid-phase catalysis, liquid phase are distilled and are carried out polycondensation reaction in the extraction catalytic distillation tower of one, and it is anti-that a step completes polycondensation
Original tediously long flow process should be simplified with technical processs such as fractional distillation.Device described in the utility model eliminates substantial amounts of equipment, letter
Change flow process.
To achieve these goals, this utility model adopts the following technical scheme that
A kind of device producing polymethoxy dimethyl ether DMM3-5, urges including methanol oxidator, heat exchanger, fine removing tower, extraction
Change distillation column, decomposition tower and fractionating system:
The discharging opening of described methanol oxidator is connected with the air inlet a of described heat exchanger, and charging aperture derives heat with described heat exchanger
The leakage fluid dram a of methanol connects；
The inlet a of described heat exchanger is connected with the container being contained with cold methanol, air vent a and the air inlet b of described fine removing tower
It is connected；
The leakage fluid dram b of described fine removing tower is connected with the container being contained with water, the phase of air vent b and described extraction catalytic distillation tower
Connect；
Described extraction distillation column, tower top is provided with air vent c and the charging aperture with described methanol oxidator is connected, and is provided with at the bottom of tower
Leakage fluid dram c and the fluid inlet with described fractionating system are connected, tower internal upper part be extraction section, middle part be that catalytic section, bottom are
Distilling period；The bottom of described extraction section is provided with air inlet c and is connected with the air vent b of described fine removing tower；Described extraction section
Top offer inlet b, inlet b and be divided into two-way, a road exports A with light component DMM1-2 of fractionating system and is connected
Connecing, a road exports B with light component DMM1-2 of decomposition tower and is connected；
The DMM3-5 outlet A of described fractionating system is connected with recovering device, and gather target product DMM3-5,
DMM6-10 outlet is connected with the DMM6-10 import of described decomposition tower；
The DMM3-5 outlet B of described decomposition tower is connected with recovering device, and gather target product DMM3-5.
In technique scheme, described decomposition tower, bottom is provided with the heater of regulation temperature.
In technique scheme, described extraction catalytic distillation tower, the extraction section in tower is equivalent to an extraction tower, structure and biography
Packed extraction tower or traditional perforated-plate extraction tower structure of system are identical；Distilling period in tower, structure and traditional packed extraction tower
Or traditional perforated-plate extraction tower structure is identical, and bottom has the distillation space of heating, and distillation space is equipped with regulation
The reboiler of temperature；The described catalyst in catalytic section is module catalyst or bulk catalyst；
In technique scheme, when the described catalyst in catalytic section is bulk catalyst, described catalytic section is by catalyst layer
With column plate layer is spaced setting from top to bottom, between catalyst layer and catalyst layer between alternating floor column plate layer constitute one section of catalytic absorption section；
Described column plate layer is stacked setting from top to bottom by two blocks of column plates, and the both sides of upper strata column plate are provided with chord downcomer, descending trays
Central authorities are provided with central well down take；Described catalyst layer is arranged by each fixing a piece of rustless steel liner plate in a piece of grid left and right, described
One layer of stainless steel cloth it is equipped with on grid, the bulk catalyst described in the interior filling of described catalyst layer, described catalysis in bulk
Agent is arranged above with liquid distribution trough.
Described catalytic section is that the catalytic absorption section described in n section stacks setting from top to bottom, and, adjacent catalytic absorption section it
Column plate layer described in alternating floor between；Described catalytic absorption section, every section of height is at least 1 meter；Described n is positive integer,
And 1≤n≤100, preferably 6≤n≤10.
In described catalytic section, the superiors' catalytic absorption section be provided above one block of column plate with central well down take, orlop
The lower section of catalytic absorption section is provided with one layer of column plate layer.
Space between described rustless steel liner plate and extraction catalytic distillation inner wall of tower constitutes gas phase channel；Described downspout and urging
Agent layer constitutes liquid channel.
Described column plate is valve plate or bubble cap plate or sieve plate, gas phase and liquid phase fully connect at the bubble-cap of bubble cap plate
Touch thus mass transfer, heat transfer and carry out component distribution or distribution further, or gas phase liquid phase float valve by place be fully contacted from
And mass transfer, heat transfer and carry out component distribution or distribution further；Or gas phase liquid phase is fully contacted by place sieve plate thus passes
Matter, heat transfer and carry out component distribution or distribution further.(extract containing formaldehyde is in catalytic section and under the effect of catalyst
Carrying out polycondensation reaction and generate DMM1-10, part is not participated in the extract containing formaldehyde of polycondensation reaction and is flowed into extraction catalytic distillation
In the distilling period of tower, after distillation, the gaseous component (formaldehyde) that obtains is returned by gas phase channel and continues and DMM1-2 and/or contain
The extract contact of formaldehyde thus circulation carries out extracting, polycondensation reaction).
Described liquid distribution trough is made up of the overflow pipe (16) of multiple a diameter of 20mm.
Described bulk catalyst, for spherical particle in bulk, column, solid acidic resin ring-type, strip urges
Agent；Described solid acidic resin catalyst is modified resin catalyst or molecular sieve catalyst, such as Kai Rui environmental protection section of our company
The resin catalyst that skill limited company produces.
In technique scheme, when the described catalyst in catalytic section is module catalyst, described module catalyst includes living
Property catalyst, metal gauze and wire weave plate: described module catalyst is by described metal gauze, metal gauze ripple
The spaced and parallel setting of plate, contains described catalyst granules and is formed in catalyst layer, and this catalyst layer between two panels metal gauze
Described catalyst granules by described metal gauze corrugated plating apart from；Catalyst layer described in described module catalyst
Interval is arranged；
Described module catalyst is fixed in periphery by tinsel；
Described module catalyst outline is wrapped closing in geometry by described metal gauze；Described geometry is
Cube, cylinder；
Alternating floor or double layer of metal screen waviness plate between described metal gauze and metal gauze；
Between described catalyst layer, alternating floor or double layer of metal screen waviness plate are arranged；Described catalyst layer is by metal described in two-layer
Between between silk screen, alternating floor or double layer of metal screen waviness plate are arranged and the described catalyst granules of internal filling；Described catalyst layer
Forming liquid channel, the wire weave flaggy between adjacent described catalyst layer constitutes gas phase channel；
Described metal gauze, metal gauze corrugated plating are made up of stainless steel material, described metal gauze or metal gauze ripple
Card also can be replaced by corrosion resistant plate with holes；
Described metal gauze, metal gauze corrugated plating are vertically arranged up and down；
Described catalyst layer arranges reinforcement outer wall, is urged as described by corrugated plating bilayer with holes to described metal gauze and rustless steel
The outer wall of agent layer；
Module catalyst described in loading in catalytic section, and be reserved with charging space up and down or feed distributor space is installed, described
Module catalyst be polylith, stack setting from top to bottom, and described gas phase channel, liquid channel be to be vertically arranged up and down；
In described catalytic section, the gas phase channel of the module catalyst described in adjacent layer is oppositely arranged with liquid channel；
Liquid phase feeding in described catalytic section is the extract containing formaldehyde, and gas-phase feed is that distilling period distills the gaseous component obtained
(extract containing formaldehyde carries out polycondensation reaction in catalytic section and under the effect of catalyst and generates DMM1-10, and part is not joined
The extract containing formaldehyde adding polycondensation reaction is flowed in the distilling period of extraction catalytic distillation tower, after distillation, and gaseous component (first
Aldehyde) return through gas phase channel as gas-phase feed and to continue to contact with DMM1-2 and/or the extract that contains formaldehyde thus circulate and carry out
Extraction, polycondensation reaction).
Described catalyst, for solid acidic resin catalyst, for modified resin catalyst or molecular sieve catalyst, such as our company
The resin catalyst that Kai Rui environmental protection Science and Technology Co., Ltd. produces.
In technique scheme, described extraction section or distilling period, when structure is identical with traditional filler extraction tower structure, internal
It is provided with the filler that N rice is high, and N is positive integer, 1≤N≤200, preferably 10≤N≤100；Filler is stainless steel wave pit plate
Filler, it is also possible to be stainless steel silk corrugated wire gauze packing.
In technique scheme, described extraction section or distilling period, when structure is identical with traditional perforated-plate extraction tower structure, internal
It is provided with N shell tower tray, and N is positive integer, 1≤N≤200, preferably 10≤N≤100；Its sieve plate can be common sieve plate or height
Effect sieve plate, plate spacing can be 100-900mm, preferably 400-600mm.
In technique scheme, described methanol oxidator, heat exchanger, fine removing tower, fractionating system, decomposer are existing
Device.
A kind of method producing polymethoxy dimethyl ether DMM3-5, comprises the following steps:
(1) heat exchange: methanol and air, with two traditional methods as preparation method, prepare the mixed gas containing formaldehyde gas；Will system
The mixed gas obtained carries out heat exchange；
(2) loss of essence water: the mixed gas after step (1) heat exchange is carried out loss of essence water until the moisture mole in mixed gas contains
Amount is less than 0.1%；
(3) extract, be catalyzed and distill: with extractant DMM1-2, the mixed gas obtained after step (2) removing moisture is entered
Row extraction, the mixture being obtained by extraction carries out polycondensation reaction under catalyst existence condition and generates DMM1-10, and be obtained by extraction is mixed
The gaseous component also not carrying out polycondensation reaction in compound proceeds extraction, polycondensation reaction after distillation；
(4) fractional distillation: the polycondensation product DMM1-10 that step (3) obtains is passed in fractionating system and carries out fractional distillation, wherein:
Target product DMM3-5 gathers, and light component DMM1-2 is back in step (3) proceed polycondensation reaction, heavy constituent
DMM6-10 is passed in decomposer；
(5) decompose: heavy constituent DMM6-10 that step (4) obtains is passed in decomposer and decomposes, wherein: mesh
Mark product DMM3-5 gathers, and light component DMM1-2 is back in step (3) proceed polycondensation reaction.
In technique scheme, described method particularly as follows:
(1) heat exchange: methanol and air are in methanol oxidator, with two traditional methods as preparation method, prepares containing formaldehyde gas
Mixed gas, this mixed gas raw material composition as shown in the table；This mixed gas is discharged into from methanol oxidator discharging opening
Heat exchanger carries out heat exchange；
Described heat exchanger is tubular heat exchanger, and tube side enters oxidic raw materials cold methanol, and shell side enters described mixed gas, otherwise also
So；Described heat exchanger, inlet temperature: 100-800 DEG C, preferably 200-600 DEG C, outlet temperature: 100-200 DEG C, preferably
100-150℃。
| Title | Molecular formula | Mol% |
| Formaldehyde | CH2O | 6-15 |
| Methanol | CH3OH | 0-2 |
| Formic acid | CH2O2 | 20-500PPm |
| Nitrogen | N2 | 50-80 |
| Oxygen | O2 | 1-10 |
| Hydrogen | H2 | 0-5 |
| Carbon monoxide | CO | 1-5 |
| Carbon dioxide | CO2 | 0-10 |
| Moisture | H2O | 10-15 |
| Other | CH4 +Ar+ | Surplus |
(2) loss of essence water: the step (1) mixed gas after heat exchanger heat exchange is passed in fine removing tower and carries out loss of essence water, removing
Moisture in mixed gas, until the moisture molar content in mixed gas is less than 0.1%, obtains being practically free of the gaseous mixture of moisture
Body；Described loss of essence water condition is: at fine removing tower air inlet b, temperature is 40-150 DEG C, and tower top temperature is 45-100 DEG C, pressure
0.35-0.42Mpa, column bottom temperature 75-80 DEG C；
(3) extract, be catalyzed and distill: the mixed gas obtained after step (2) loss of essence water is passed into extraction catalytic distillation tower
In extraction section, in extraction section, it is passed through light component DMM1-2 of extractant, after the loss of essence water described in DMM1-2 extraction absorption simultaneously
The extract containing formaldehyde is formed after the mixed gas obtained；The described extract containing formaldehyde is urged extraction catalytic distillation tower
Change and carry out polycondensation reaction in section and under the effect of catalyst and generate DMM1-10, part do not participate in polycondensation reaction containing formaldehyde
Extract is flowed in the distilling period of extraction catalytic distillation tower, and after distillation, gaseous component (formaldehyde) returns through gas phase channel and continues
Continuous carry out with extractant DMM1-2 and/or the extract containing formaldehyde extracting, polycondensation；
In described extraction section: in the mixed gas obtained after described DMM1-2 and loss of essence water, the mol ratio of formaldehyde is 1-10:1,
Air speed when being preferably 1-3:1, DMM1-2 entrance extraction section is 0.1-5.5h-1；Described extraction conditions is: temperature be room temperature or
Not higher than 150 DEG C, pressure is 0.1-3.0Mpa；
In described catalytic section: condensation temperature is 35-180 DEG C, preferably 55-120 DEG C, pressure is 0.1-3.0Mpa；Described contains
The mass space velocity of the extract of formaldehyde is 0.1-5.5h-1；
In described distilling period: temperature 80-300 DEG C, pressure 0.1-3.0Mpa；
Described catalyst is solid acid catalyst, preferred resin catalyst, it is possible to be molecular sieve, heteropllyacids, superpower acids；
In the present embodiment is the resin catalyst of Kai Rui environmental protection Science and Technology Co., Ltd. of our company production.
(4) fractional distillation: be passed in existing fractionating system conventionally to enter by the product DMM1-10 that step (3) obtains
Row fractional distillation；Wherein, the target product DMM3-5 that fractional distillation obtains gathers, and light component DMM1-2 that fractional distillation obtains is back to step
Suddenly recycling in the extraction catalytic distillation tower described in (3), heavy constituent DMM6-10 that fractional distillation obtains is passed in decomposer；
Fractionating system is existing conventional rectification tower, rectification condition: tower top temperature is 42～150 DEG C, tower top pressure is born
0.01～0.5MPa, overhead reflux ratio is 0.5～5.0；Column bottom temperature 150～300 DEG C.
(5) decompose: heavy constituent DMM6-10 that step (4) obtains is passed in existing decomposer conventionally
Decompose, wherein, decompose the target product DMM3-5 obtained and gather, decompose light component DMM1-2 obtained and be back to
Extraction catalytic distillation tower described in step (3) recycles；
Decomposer is existing decomposition tower, and the temperature of tower top is 50～150 DEG C, and pressure is 0.1～5.0MPa；Temperature at the bottom of tower is
80～300 DEG C.
Advantage of the present utility model
1, the outlet gas phase component of methanol oxidator, the water directly by high-efficiency dehydration tower, oxidation produced is taken off, and remains gas phase
Just being passed through extraction catalytic distillation tower, collect gaseous extraction, liquid-phase catalysis, liquid phase is distilled in one, and a step completes；
2, the new technology path preparing polymethoxy dimethyl ether is created；
3, compared with existing Technology, large number quipments, pipeline, internals facility are eliminated；
4, technological process is optimized；
5, save investment, reduce production cost；
6, maximized energy-saving and emission-reduction.
7, solid foundation has been laid for maximization, serialization, intensive manufacture.
Accompanying drawing illustrates:
The overall structure schematic diagram of Fig. 1: this utility model device；
Fig. 2: extract the generalized section of catalytic distillation tower when this utility model catalyst is bulk catalyst；
Fig. 3: the generalized section of catalyst layer, liquid distribution trough and overflow pipe when this utility model catalyst is bulk catalyst；
Fig. 4: the generalized section of catalyst layer when this utility model catalyst is bulk catalyst；
Fig. 5: the generalized section of module catalyst when this utility model catalyst is module catalyst；
Fig. 6: extract the generalized section of catalytic distillation tower when this utility model catalyst is module catalyst；
Wherein, 1-methanol oxidator, 2-heat exchanger, 3-fine removing tower, 4-reboiler, 5-extracts catalytic distillation tower, 6-decomposition tower,
7-heater, 8-fractionating system, 9-extraction section, 10-catalytic section, 11-distilling period, 12-rustless steel liner plate, 13-grid, 14-dissipates
Dress catalyst, 15-liquid distribution trough, the overflow pipe of 16-liquid distribution trough, 17-central well down take, 18-gas phase channel, 19-tower
Plate, the active catalyst of 20-module catalyst, 21-metal gauze corrugated plating, 22-metal gauze, urging in 23-module catalyst
Agent layer, the metal gauze of 24-stuck-module catalyst outline, 25-liquid channel, 26-module catalyst, 27-feeds space,
28-distills space, 29-chord downcomer.
Detailed description of the invention
Hereinafter the detailed description of the invention of technical solutions of the utility model is described in detail, but this utility model is not limited to following description
Content:
A kind of device producing polymethoxy dimethyl ether DMM3-5, as shown in Fig. 1,2,3,4,5,6, including methanol oxygen
Change device 1, heat exchanger 2, fine removing tower 3, extract catalytic distillation tower 5, decomposition tower 6 and fractionating system 8:
The discharging opening of described methanol oxidator 1 is connected with the air inlet a of described heat exchanger, and charging aperture is derived with described heat exchanger
The leakage fluid dram a of hot methanol connects；
The inlet a of described heat exchanger 2 is connected with the container being contained with cold methanol, air vent a and the air inlet of described fine removing tower
Mouth b is connected；
The leakage fluid dram b of described fine removing tower 3 is connected with the container being contained with water, air vent b and described extraction catalytic distillation tower
It is connected；
Described extraction distillation column 5, tower top is provided with air vent c and the charging aperture with described methanol oxidator is connected, and sets at the bottom of tower
Have leakage fluid dram c and the fluid inlet with described fractionating system to be connected, tower internal upper part be extraction section 9, middle part be catalytic section 10,
Bottom is distilling period 11；The bottom of described extraction section is provided with air inlet c and the air vent b with described fine removing tower 3 is connected；Institute
The top of the extraction section stated offers inlet b, inlet b and is divided into two-way, a road and light component DMM1-2 of fractionating system 8
Outlet A is connected, and a road exports B with light component DMM1-2 of decomposition tower 6 and is connected；
The DMM3-5 outlet A of described fractionating system 8 is connected with recovering device, and gather target product DMM3-5,
DMM6-10 outlet is connected with the DMM6-10 import of described decomposition tower 6；
The DMM3-5 outlet B of described decomposition tower 6 is connected with recovering device, and gather target product DMM3-5.
Described decomposition tower 6, bottom is provided with the heater 7 of regulation temperature.
Described extraction catalytic distillation tower 5, the extraction section 9 in tower is equivalent to an extraction tower, structure and traditional filler extraction
Tower or traditional perforated-plate extraction tower structure are identical；Distilling period 11 in tower, structure and traditional packed extraction tower or traditional
Perforated-plate extraction tower structure is identical, and bottom has the distillation space 28 of heating, and distillation space is equipped with regulation temperature
Reboiler 4；The described catalyst in catalytic section is module catalyst 26 or bulk catalyst 14:
When the described catalyst in catalytic section 10 is bulk catalyst 14, described catalytic section by catalyst layer and column plate layer from
Upper and lower interval is arranged, between catalyst layer and catalyst layer between alternating floor column plate layer constitute one section of catalytic absorption section；Described tower
Flaggy is stacked setting from top to bottom by two blocks of column plates 19, and the both sides of upper strata column plate are provided with chord downcomer 29, in descending trays
Centre is provided with central well down take 17；Described catalyst layer is arranged by each fixing a piece of rustless steel liner plate 12 of a piece of grid about 13,
Being equipped with one layer of stainless steel cloth on described grid, the bulk catalyst described in the interior filling of described catalyst layer, described dissipates
Dress catalyst is arranged above with liquid distribution trough 15.
Described catalytic section 10 stacks setting from top to bottom for the catalytic absorption section described in n section, and, adjacent catalytic absorption section
Column plate layer described in alternating floor between；Described catalytic absorption section, every section of height is at least 1 meter；Described n is positive integer,
And 1≤n≤100, preferably 6≤n≤10.
In described catalytic section 10, the superiors' catalytic absorption section be provided above one block of column plate 19 with central well down take 17,
The lower section of orlop catalytic absorption section is provided with one layer of column plate layer.
Space between described rustless steel liner plate and extraction catalytic distillation inner wall of tower constitutes gas phase channel 18；Described downspout 17
Liquid channel is constituted with catalyst layer.
Described column plate 19 be valve plate or bubble cap plate or sieve plate, gas phase and liquid phase abundant at the bubble-cap of bubble cap plate
Contact thus mass transfer, heat transfer and carry out component distribution or distribution further, or gas phase liquid phase being fully contacted by place at float valve
Thus mass transfer, heat transfer and carry out component distribution or distribution further；Or gas phase liquid phase sieve plate be fully contacted by place thus
Mass transfer, heat transfer and carry out component distribution or distribution further.
Described liquid distribution trough 15 is made up of the overflow pipe 16 of multiple a diameter of 20mm.
Described bulk catalyst 14, for spherical particle in bulk, column, ring-type, the solid acidic resin of strip
Catalyst；Described solid acidic resin catalyst is modified resin catalyst or molecular sieve catalyst.
When the described catalyst in catalytic section is module catalyst 26, described module catalyst include active catalyst 20,
Metal gauze 22 and wire weave plate 21: described module catalyst is by between described metal gauze, metal gauze corrugated plating
Every be arrangeding in parallel, contain described catalyst 20 granule between two panels metal gauze and form catalyst layer 23, and this catalyst layer
In described catalyst granules by described metal gauze corrugated plating apart from；Catalyst described in described module catalyst
Interlayer is every setting；
Described module catalyst is fixed in periphery by tinsel；
Described module catalyst outline is wrapped closing in geometry by described metal gauze 24；Described geometric form
Shape is cube, cylinder；
Alternating floor or double layer of metal screen waviness plate between described metal gauze and metal gauze；
Between described catalyst layer, alternating floor or double layer of metal screen waviness plate are arranged；Described catalyst layer is by gold described in two-layer
Between belonging between silk screen, alternating floor or double layer of metal screen waviness plate are arranged and the described catalyst granules of internal filling；Described catalyst
Layer forming liquid phase passage 25, the wire weave flaggy between adjacent described catalyst layer constitutes gas phase channel 18；
Described metal gauze, metal gauze corrugated plating are made up of stainless steel material, described metal gauze or metal gauze ripple
Card also can be replaced by corrosion resistant plate with holes；
Described metal gauze, metal gauze corrugated plating are vertically arranged up and down；
Described catalyst layer arranges reinforcement outer wall, using described metal gauze and rustless steel corrugated plating with holes bilayer as described
The outer wall of catalyst layer；
Module catalyst 26 described in loading in catalytic section, and be reserved with charging space 27 up and down or feed distributor space is installed,
Described module catalyst is polylith, stacks setting from top to bottom, and described gas phase channel, liquid channel is the most vertically to set
Put；
In described catalytic section, the gas phase channel of the module catalyst described in adjacent layer is oppositely arranged with liquid channel；
Liquid phase feeding in described catalytic section is the extract containing formaldehyde, and gas-phase feed is that distilling period distills the gaseous component obtained.
Described catalyst 20, for solid acidic resin catalyst, for modified resin catalyst or molecular sieve catalyst.
Described extraction section or distilling period, when structure is identical with traditional filler extraction tower structure, inside is provided with the filler that N rice is high,
And N is positive integer, 1≤N≤200, preferably 10≤N≤100；Filler is stainless steel wave pit plate filler, it is also possible to be stainless
Steel wire ripple packing.
Described extraction section or distilling period, when structure is identical with traditional perforated-plate extraction tower structure, inside is provided with N shell tower tray, and
N is positive integer, 1≤N≤200, preferably 10≤N≤100；Its sieve plate can be common sieve plate or efficient sieve plate, and plate spacing can
To be 100-900mm, preferably 400-600mm.
Described methanol oxidator, heat exchanger, fine removing tower, fractionating system, decomposer are existing device.
Below in conjunction with specific embodiment, this utility model is expanded on further:
Embodiment 1:
A kind of method preparing polymethoxy dimethyl ether DMM3-5, comprises the following steps:
(1) heat exchange:
Methanol and air, in methanol oxidator, with traditional two methods as preparation method, produce the gas mixture containing formaldehyde gas,
This gas mixture is discharged in heat exchanger from methanol oxidator discharging opening, and this heat exchanger is tubular heat exchanger, and tube side enters oxygen
Changing the methanol that raw material is cold, shell side enters the gas mixture obtained；Heat exchanger inlet temperature: 260 DEG C, outlet temperature: 125 DEG C.
(2) loss of essence water:
Described gas mixture imports to carry out in fine removing tower loss of essence water after step (1) heat exchange, and fine removing tower inlet temperature is:
110-115 DEG C, tower top temperature is 95-100 DEG C, and tower top pressure is 0.35-0.42Mpa, and column bottom temperature is: 75-80 DEG C；Detection tower
Ejecting the molar content of water in the material of mouth is qualified less than 0.1%, has obtained the most aqueous mixed gas；
(3) extract, be catalyzed and distill:
The qualified material of step 2 being imported in extraction catalytic distillation tower, catalyst is module catalyst (our company self-control D006
Type acid resin catalyst) operating condition:
Extraction section: upper temp 55-60 DEG C, pressure 0.10-0.20Mpa, temperature of lower 70-80 DEG C；Extractant DMM1-2 rubs
Your amount is in the mixed gas that obtains after loss of essence water 2 times of formaldehyde mole, and the air speed of extractant DMM1-2 is 2.8h-1；
Catalytic section: upper temp 70-80 DEG C, pressure 0.10-0.20Mpa, temperature of lower 80-90 DEG C, containing the extract of formaldehyde
Air speed be 2.8h-1；
Distilling period: upper temp 80-90 DEG C, pressure 0.10-0.20Mpa, bottom temp 110-130 DEG C；
Sampling in four hours one is analyzed, and sample tap is top (i.e. the top of extraction section) and the bottom of extraction catalytic distillation tower
(i.e. the bottom of distilling period) sample tap, analytical tool: gas chromatograph Agilent 7820, top gas phase content of formaldehyde is about 0,
Bottom liquid phases export goal product assay is 91.5%, i.e. DMM3-5 selectivity is 91.5%.
Embodiment 2:
A kind of method preparing polymethoxy dimethyl ether DMM3-5, operating procedure is substantially the same manner as Example 1, except that
Catalyst is bulk catalyst (our company's self-control D008 type high temperature resistant acidic resin catalyst):
Sampling in four hours one is analyzed, and sample tap is top (i.e. the top of extraction section) and the bottom of extraction catalytic distillation tower
(i.e. the bottom of distilling period) sample tap, analytical tool: gas chromatograph Agilent 7820, top gas phase content of formaldehyde is about 0,
Bottom liquid phases export goal product assay is 91.0%, i.e. DMM3-5 selectivity is 91.0%.
Embodiment 3:
A kind of method preparing polymethoxy dimethyl ether DMM3-5, operating procedure is substantially the same manner as Example 1, except that
Extraction, catalysis different with distillation condition:
Extraction section: upper temp 55-60 DEG C, pressure 0.10-0.20Mpa, temperature of lower 80-85 DEG C；Extractant DMM1-2 rubs
Your amount is in the mixed gas that obtains after loss of essence water 2 times of formaldehyde mole, and the air speed of extractant DMM1-2 is 2.8h-1；
Catalytic section: upper temp 80-85 DEG C, pressure 0.10-0.20Mpa, temperature of lower 85-95 DEG C, containing the extract of formaldehyde
Air speed be 2.8h-1；
Distilling period: upper temp 85-95 DEG C, pressure 0.10-0.20Mpa, bottom temp 115-135 DEG C；
Sampling in four hours one is analyzed, and sample tap is top (i.e. the top of extraction section) and the bottom of extraction catalytic distillation tower
(i.e. the bottom of distilling period) sample tap, analytical tool: gas chromatograph Agilent 7820, top gas phase content of formaldehyde is about 0,
Bottom liquid phases export goal product assay is 92.5%, i.e. DMM3-5 selectivity is 92.5%.
Embodiment 4:
A kind of method preparing polymethoxy dimethyl ether DMM3-5, operating procedure is substantially the same manner as Example 2, except that
Extraction, catalysis different with distillation condition:
Extraction section: upper temp 55-60 DEG C, pressure 0.10-0.20Mpa, temperature of lower 80-85 DEG C；Extractant DMM1-2 rubs
Your amount is in the mixed gas that obtains after loss of essence water 2 times of formaldehyde mole, and the air speed of extractant DMM1-2 is 2.8h-1；
Catalytic section: upper temp 80-85 DEG C, pressure 0.10-0.20Mpa, temperature of lower 85-95 DEG C, containing the extract of formaldehyde
Air speed be 2.8h-1；
Distilling period: upper temp 85-95 DEG C, pressure 0.10-0.20Mpa, bottom temp 115-135 DEG C；
Sampling in four hours one is analyzed, and sample tap is top (i.e. the top of extraction section) and the bottom of extraction catalytic distillation tower
(i.e. the bottom of distilling period) sample tap, analytical tool: gas chromatograph Agilent 7820, top gas phase content of formaldehyde is about 0,
Bottom liquid phases export goal product assay is 91.5%, i.e. DMM3-5 selectivity is 91.5%.
Embodiment 5:
A kind of method preparing polymethoxy dimethyl ether DMM3-5, operating procedure is substantially the same manner as Example 1, except that
Extraction, catalysis different with distillation condition:
Extraction section: upper temp 55-60 DEG C, pressure 0.10-0.20Mpa, temperature of lower 80-85 DEG C；Extractant DMM1-2 rubs
Your amount is in the mixed gas that obtains after loss of essence water 2 times of formaldehyde mole, and the air speed of extractant DMM1-2 is 2.8h-1；
Catalytic section: upper temp 80-85 DEG C, pressure 0.10-0.20Mpa, temperature of lower 85-95 DEG C, containing the extract of formaldehyde
Air speed be 2.8h-1；
Distilling period: upper temp 85-95 DEG C, pressure 0.10-0.20Mpa, bottom temp 115-135 DEG C；
Sampling in four hours one is analyzed, and sample tap is top (i.e. the top of extraction section) and the bottom of extraction catalytic distillation tower
(i.e. the bottom of distilling period) sample tap, analytical tool: gas chromatograph Agilent 7820, top gas phase content of formaldehyde is about 0,
Bottom liquid phases export goal product assay is 92.0%, i.e. DMM3-5 selectivity is 92.0%.
Examples detailed above simply for technology of the present utility model design and technical characterstic are described, can not limit this utility model with this
Protection domain.All equivalent transformations done according to essence of the present utility model or modification, all should contain of the present utility model
Within protection domain.
Claims (10)
1. produce a device of polymethoxy dimethyl ether DMM3-5, including methanol oxidator (1), heat exchanger (2), fine removing tower (3), extraction catalytic distillation tower (5), decomposition tower (6) and fractionating system (8):
The described discharging opening of methanol oxidator (1) is connected with the air inlet a of described heat exchanger, and the leakage fluid dram a that charging aperture derives hot methanol with described heat exchanger is connected；
The inlet a of described heat exchanger (2) is connected with the container being contained with cold methanol, and air vent a is connected with the air inlet b of described fine removing tower；
The leakage fluid dram b of described fine removing tower (3) is connected with the container being contained with water, and air vent b is connected with described extraction catalytic distillation tower；
Described extraction distillation column (5), tower top is provided with air vent c and the charging aperture with described methanol oxidator is connected, be provided with leakage fluid dram c at the bottom of tower and the fluid inlet with described fractionating system be connected, tower internal upper part be extraction section (9), middle part be catalytic section (10), bottom be distilling period (11)；The bottom of described extraction section is provided with air inlet c and the air vent b with described fine removing tower (3) is connected；The top of described extraction section offers inlet b, inlet b and is divided into two-way, and a road exports A with light component DMM1-2 of fractionating system (8) and is connected, and a road exports B with light component DMM1-2 of decomposition tower (6) and is connected；
The DMM3-5 outlet A of described fractionating system (8) is connected with recovering device, and gather target product DMM3-5, and DMM6-10 outlet is connected with the DMM6-10 import of described decomposition tower (6)；
The DMM3-5 outlet B of described decomposition tower (6) is connected with recovering device, and gather target product DMM3-5；Described decomposition tower (6), bottom is provided with the heater (7) of regulation temperature.
Device the most according to claim 1, it is characterized in that, described extraction catalytic distillation tower (5), the extraction section (9) in tower is equivalent to an extraction tower, and structure is identical with traditional packed extraction tower or traditional perforated-plate extraction tower structure；Distilling period (11) in tower, structure is identical with traditional packed extraction tower or traditional perforated-plate extraction tower structure, and bottom has the distillation space (28) of heating, distillation space is equipped with the reboiler (4) of regulation temperature；The described catalyst in catalytic section is module catalyst (26) or bulk catalyst (14).
Device the most according to claim 2, it is characterized in that, when the described catalyst in catalytic section (10) is bulk catalyst (14), described catalytic section is spaced setting from top to bottom by catalyst layer and column plate layer, between catalyst layer and catalyst layer between alternating floor column plate layer constitute one section of catalytic absorption section；Described column plate layer is stacked setting from top to bottom by two pieces of column plates (19), and the both sides of upper strata column plate are provided with chord downcomer (29), and the central authorities of descending trays are provided with central well down take (17)；Described catalyst layer is arranged by each fixing a piece of rustless steel liner plate (12) in a piece of grid (13) left and right, one layer of stainless steel cloth it is equipped with on described grid, bulk catalyst described in loading in described catalyst layer, described bulk catalyst is arranged above with liquid distribution trough (15)；Described liquid distribution trough (15) is made up of the overflow pipe (16) of multiple a diameter of 20mm.
Device the most according to claim 3, it is characterised in that described catalytic section (10) is that the catalytic absorption section described in n section stacks setting from top to bottom, and, between adjacent catalytic absorption section between column plate layer described in alternating floor；Described catalytic absorption section, every section of height is at least 1 meter；Described n is positive integer, and 1≤n≤100；
In described catalytic section (10), the superiors' catalytic absorption section be provided above one block of column plate (19) with central well down take (17), the lower section of orlop catalytic absorption section is provided with one layer of column plate layer.
Device the most according to claim 3, it is characterised in that the space between described rustless steel liner plate (12) and extraction catalytic distillation tower (5) inwall constitutes gas phase channel (18)；Described central well down take (17) and catalyst layer constitute liquid channel (25).
Device the most according to claim 3, it is characterized in that, described column plate (19) is valve plate or bubble cap plate or sieve plate, gas phase and liquid phase are fully contacted at the bubble-cap of bubble cap plate thus mass transfer, heat transfer and carry out component distribution or distribution further, or gas phase liquid phase being fully contacted by place thus mass transfer, heat transfer and carry out component distribution or distribution further at float valve；Or gas phase liquid phase being fully contacted by place thus mass transfer, heat transfer and carry out component distribution or distribution further at sieve plate.
Device the most according to claim 2, it is characterized in that, when the described catalyst in catalytic section is module catalyst (26), described module catalyst includes catalyst (20), metal gauze (22) and wire weave plate (21): described module catalyst is by described metal gauze, the spaced and parallel setting of metal gauze corrugated plating, contain described catalyst (20) granule between two panels metal gauze and form catalyst layer (23), and the described catalyst granules in this catalyst layer by described metal gauze corrugated plating apart from；Catalyst layer interval described in described module catalyst is arranged；Described metal gauze, metal gauze corrugated plating are made up of stainless steel material, and described metal gauze or metal gauze corrugated plating also can be replaced by corrosion resistant plate with holes.
Device the most according to claim 7, it is characterised in that alternating floor or double layer of metal screen waviness plate between described metal gauze and metal gauze；Between described catalyst layer, alternating floor or double layer of metal screen waviness plate are arranged；Described catalyst layer is to be arranged by alternating floor between metal gauze described in two-layer or double layer of metal screen waviness plate and internal fill described catalyst granules；Described catalyst layer forms liquid channel (25), and the wire weave flaggy between adjacent described catalyst layer constitutes gas phase channel (18).
Device the most according to claim 7, it is characterized in that, module catalyst (26) described in loading in catalytic section, and be reserved with charging space (27) up and down or feed distributor space is installed, described module catalyst is polylith, stack setting from top to bottom, and gas phase channel, liquid channel are to be vertically arranged up and down；Described metal gauze, metal gauze corrugated plating are vertically arranged up and down；In described catalytic section, the gas phase channel of adjacent layer module catalyst is oppositely arranged with liquid channel.
Device the most according to claim 7, it is characterised in that described module catalyst is fixed in periphery by tinsel；Described module catalyst outline is wrapped closing in geometry by the metal gauze (24) of stuck-module catalyst outline；Described geometry is cube, cylinder；Described catalyst layer arranges reinforcement outer wall, using described metal gauze and rustless steel corrugated plating with holes bilayer as the outer wall of described catalyst layer.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620189729.2U CN205556511U (en) | 2016-03-14 | 2016-03-14 | Production gathers methoxy dimethyl ether DMM3 -5's device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620189729.2U CN205556511U (en) | 2016-03-14 | 2016-03-14 | Production gathers methoxy dimethyl ether DMM3 -5's device |
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| CN205556511U true CN205556511U (en) | 2016-09-07 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105622366A (en) * | 2016-03-14 | 2016-06-01 | 凯瑞环保科技股份有限公司 | Device and method for producing polyoxymethylene dimethyl ether DMM3-5 |
| CN110508018A (en) * | 2019-09-03 | 2019-11-29 | 中国石油大学(华东) | Produce the device and method of polymethoxy dimethyl ether |
-
2016
- 2016-03-14 CN CN201620189729.2U patent/CN205556511U/en not_active Withdrawn - After Issue
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105622366A (en) * | 2016-03-14 | 2016-06-01 | 凯瑞环保科技股份有限公司 | Device and method for producing polyoxymethylene dimethyl ether DMM3-5 |
| CN105622366B (en) * | 2016-03-14 | 2017-09-12 | 凯瑞环保科技股份有限公司 | A kind of device and method for producing polymethoxy dimethyl ether DMM3 5 |
| CN110508018A (en) * | 2019-09-03 | 2019-11-29 | 中国石油大学(华东) | Produce the device and method of polymethoxy dimethyl ether |
| CN110508018B (en) * | 2019-09-03 | 2022-02-25 | 中国石油大学(华东) | Device and method for producing polymethoxy dimethyl ether |
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