CN105622366A - Device and method for producing polyoxymethylene dimethyl ether DMM3-5 - Google Patents

Device and method for producing polyoxymethylene dimethyl ether DMM3-5 Download PDF

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Publication number
CN105622366A
CN105622366A CN201610141418.3A CN201610141418A CN105622366A CN 105622366 A CN105622366 A CN 105622366A CN 201610141418 A CN201610141418 A CN 201610141418A CN 105622366 A CN105622366 A CN 105622366A
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extraction
tower
section
catalytic
catalyzer
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CN105622366B (en
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毛进池
刘文飞
郭为磊
王文学
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Kai Rui Environmental Protection Science And Technology Co Ltd
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Kai Rui Environmental Protection Science And Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
    • C07C41/48—Preparation of compounds having groups
    • C07C41/50—Preparation of compounds having groups by reactions producing groups
    • C07C41/56—Preparation of compounds having groups by reactions producing groups by condensation of aldehydes, paraformaldehyde, or ketones
    • 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
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
    • C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
    • C07C45/37—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups
    • C07C45/38—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups being a primary hydroxyl group
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78—Separation; Purification; Stabilisation; Use of additives
    • C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a device and method for producing polyoxymethylene dimethyl ether DMM3-5. A gaseous product which contains methanal and is prepared through two methods serves as a starting material, the gaseous product does not pass through an absorption tower, that is to say, an aqueous solution is not prepared, the gaseous product is discharged from an outlet of a methanol oxidation reactor, heat exchange and fine dehydration are conducted, the treated gaseous product is introduced into an extraction catalytic distillation tower which integrates gas phase extraction, liquid phase catalysis and liquid phase distillation to be subjected to a polycondensation reaction, technological processes such as the polycondensation reaction and fractionation are completed in one step, and original tedious processes are simplified. According to the device and method for producing polyoxymethylene dimethyl ether DMM3-5, a new technical route for producing polyoxymethylene dimethyl ether is created; compared with the prior art, a large quantity of equipment, pipelines and internal part facilities are omitted; the technological processes are optimized; the investment is saved, and the production cost is reduced; energy conservation and emission reduction are achieved to the maximum extent; the solid foundation is laid for large-scale, continuous and intensive production.

Description

A kind of device and method producing polymethoxy dimethyl ether DMM3-5
Technical field
The present invention relates to a kind of device and method producing polymethoxy dimethyl ether DMM3-5, using iron molybdenum method or silver method (hereinafter referred to as two methods) produce containing the product of formaldehyde as starting raw material, be passed into after heat exchange, essence dehydration there is gaseous extraction, liquid-phase catalysis, liquid phase distill and carry out polycondensation in the extraction catalytic distillation tower of one.
Background technology
It is pure formaldehyde raw material owing to producing the main raw material of polymethoxy dimethyl ether, again due to the character of formaldehyde raw material, it is gas at normal temperatures and is easily polymerized, be therefore all exist with the form of its aqueous solution or its polymkeric substance under normal circumstances. Solid form such as paraformaldehyde or trioxymethylene exists, therefore producing in polymethoxy dimethyl ether process, or by its aqueous solution through a series of process, such as the way such as concentrated, extraction (extracting from the aqueous solution), dehydration, parsing, and from its aqueous solution, obtain pure formaldehyde raw material; Or by formalin through evaporation, concentrated, polymerization, dry and the paraformaldehyde that obtains or trioxymethylene, then dissolved with methylal, then lead to into reactor to synthesize polymethoxy dimethyl ether. Above method or from formalin (i.e. liquid phase method) or the method producing DMMn (n >=1) from polyoxymethylene (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 by this invention is for the deficiencies in the prior art, and a kind of method producing polymethoxy dimethyl ether DMM3-5 is provided, using two methods produce containing the gas-phase product of formaldehyde as starting raw material, without absorption tower (not namely being prepared into the aqueous solution), but discharge from the outlet of methanol oxidation device, through heat exchange, after essence dehydration, it is passed into and there is gaseous extraction, liquid-phase catalysis, liquid phase is distilled and is carried out polycondensation in the extraction catalytic distillation tower of one, one step completes the technological process such as polycondensation and fractionation, simplify original tediously long flow process.
The present invention also provides a kind of device producing polymethoxy dimethyl ether DMM3-5, eliminates a large amount of equipment, simplifies flow process.
In order to realize above-mentioned purpose, the present invention adopts following technical scheme:
Produce a method of polymethoxy dimethyl ether DMM3-5, comprise the following steps:
(1) heat exchange: methyl alcohol and air, taking two traditional methods as preparation method, obtain the mixed gas containing formaldehyde gas; Obtained mixed gas is carried out heat exchange;
(2) essence dehydration: the mixed gas after step (1) heat exchange is carried out essence dehydration until the moisture molar content in mixed gas is less than 0.1%;
(3) extraction, catalysis and distillation: the mixed gas obtained after the de-moisture removal of step (2) is extracted with extraction agent DMM1-2, the mixture that extraction obtains carries out polycondensation under catalyzer existence condition and generates DMM1-10, and the gaseous component also not carrying out polycondensation in the mixture that extraction obtains proceeds extraction, polycondensation after distillation;
(4) fractionation: be passed in fractionating system to carry out fractionation by the polycondensation product DMM1-10 that step (3) obtains, wherein: target product DMM3-5 gathers, light constituent DMM1-2 is back to step (3) resume and carries out polycondensation, and heavy constituent DMM6-10 is passed in decomposer;
(5) decompose: being passed in decomposer by the heavy constituent DMM6-10 that step (4) obtains and decompose, wherein: target product DMM3-5 gathers, light constituent DMM1-2 is back to step (3) resume and carries out polycondensation.
In technique scheme, described method is specially:
(1) heat exchange: methyl alcohol and air are in methanol oxidation device, and taking two traditional methods as preparation method, the obtained mixed gas containing formaldehyde gas, shown in the raw material of this mixed gas table composed as follows; This mixed gas is discharged to enter from methanol oxidation device discharge port and is carried out heat exchange in interchanger;
Described interchanger is tubular heat exchange, and Guan Cheng enters oxidic raw materials cold methanol, and shell side enters described mixed gas, and vice versa; Described interchanger, inlet temperature: 100-800 DEG C, it is preferable to 200-600 DEG C, temperature out: 100-200 DEG C, it is preferable that 100-150 DEG C.
Title Molecular formula Mol%
Formaldehyde CH2O 6-15
Methyl alcohol 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
Carbonic acid gas CO2 0-10
Moisture H2O 10-15
Other CH4 +Ar+ Surplus
(2) essence dehydration: the mixed gas of step (1) after interchanger heat exchange is passed in fine removing tower and carries out essence dehydration, de-except the moisture in mixed gas, until the moisture molar content in mixed gas is less than 0.1%, obtain almost moisture free mixed gas; Described smart dehydration conditions is: fine removing tower inlet mouth b place 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) extraction, catalysis and distillation: the mixed gas obtained after step (2) essence dehydration is passed in the extraction section of extraction catalytic distillation tower, the extraction liquid containing formaldehyde is formed after the mixed gas obtained after simultaneously leading to the essence dehydration described in absorbing into extraction agent light constituent DMM1-2, DMM1-2 extraction in extraction section; The described extraction liquid containing formaldehyde carries out polycondensation in the catalytic section of extraction catalytic distillation tower and under the effect of catalyzer and generates DMM1-10, the extraction liquid containing formaldehyde that part does not participate in polycondensation is flowed in the distilling period of extraction catalytic distillation tower, after distillation, gaseous component (formaldehyde) return through gas phase channel continue to extract with extraction agent DMM1-2 and/or carry out containing the extraction liquid of formaldehyde, polycondensation;
In described extraction section: in the mixed gas that described DMM1-2 and essence obtain after dewatering, the mol ratio of formaldehyde is 1-10:1, it is preferable to air speed when 1-3:1, DMM1-2 enter extraction section is 0.1-5.5h-1; Described extraction conditions is: temperature is normal 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, it is preferable that 55-120 DEG C, pressure is 0.1-3.0Mpa; The mass space velocity of the described extraction liquid containing formaldehyde is 0.1-5.5h-1;
In described distilling period: temperature 80-300 DEG C, pressure 0.1-3.0Mpa;
Described catalyzer is solid acid catalyst, it is preferable that resin catalyst, it is possible to be molecular sieve, heteropllyacids, super acids class; In the present embodiment is the resin catalyst that triumphant auspicious environmental protection science and technology limited-liability company of our company produces.
(4) fractionation: the product D MM1-10 that step (3) obtains is passed in existing fractionating system and conventionally carries out fractionation; Wherein, the target product DMM3-5 that fractionation obtains gathers, and the light constituent DMM1-2 that fractionation obtains is back in the extraction catalytic distillation tower described in step (3) recycle, and the heavy constituent DMM6-10 that fractionation obtains is passed in decomposer;
Fractionating system is existing conventional rectification tower, rectifying condition: tower top temperature is 42��150 DEG C, the negative 0.01��0.5MPa of tower top pressure, trim the top of column ratio are 0.5��5.0; Column bottom temperature 150��300 DEG C.
(5) decompose: the heavy constituent DMM6-10 that step (4) obtains is passed in existing decomposer and conventionally decomposes, wherein, decompose the target product DMM3-5 that obtains to gather, decompose the light constituent DMM1-2 obtained and be back in the extraction catalytic distillation tower described in step (3) recycle;
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.
The present invention also provides a kind of device producing polymethoxy dimethyl ether DMM3-5, comprises methanol oxidation device, interchanger, fine removing tower, extraction catalytic distillation tower, decomposition tower and fractionating system:
The discharge port of described methanol oxidation device is connected with the inlet mouth a of described interchanger, opening for feed and described interchanger derive hot methanol with discharge opeing mouth a be connected;
The fluid inlet a of described interchanger is connected with the container being contained with cold methanol, and venting port a is connected with the inlet mouth b of described fine removing tower;
The discharge opeing mouth b of described fine removing tower is connected with the container being contained with water, and venting port b is connected with described extraction catalytic distillation tower;
Described extraction distillation column, tower top is provided with venting port c and the opening for feed with described methanol oxidation device is connected, and is provided with discharge opeing mouth c and the fluid inlet with described fractionating system is connected at the bottom of tower, and tower internal upper part to be extraction section, middle part be catalytic section, bottom are distilling period; The bottom of described extraction section is provided with inlet mouth c and is connected with the venting port b of described fine removing tower; Fluid inlet b has been offered on the top of described extraction section, and fluid inlet b is divided into two-way, and a road exports A with the light constituent DMM1-2 of fractionating system and is connected, and a road exports B with the light constituent DMM1-2 of decomposition tower and is connected;
The DMM3-5 of described fractionating system exports A and is connected with recovering device, and target product DMM3-5, DMM6-10 outlet of gathering is connected with the DMM6-10 import of described decomposition tower;
The DMM3-5 of described decomposition tower exports B and is connected with recovering device, and gather target product DMM3-5.
In technique scheme, described decomposition tower, bottom is provided with the well heater regulating temperature.
In technique scheme, described extraction catalytic distillation tower, the extraction section 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 in tower, structure is identical with traditional packed extraction tower or traditional perforated-plate extraction tower structure, and has the distillation space of heating bottom, and distillation space is equipped with the reboiler regulating temperature; The described catalyzer in catalytic section is module catalyzer or bulk catalyst;
In technique scheme, when the described catalyzer in catalytic section is bulk catalyst, described catalytic section is arranged at interval from top to bottom by catalyst layer and column plate layer, and between catalyst layer and catalyst layer, one layer, interval column plate layer forms one section of catalytic absorption section; Described column plate layer stacks 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, and the central authorities of descending trays are provided with central well down take; Described catalyst layer is arranged by each fixing a slice stainless steel liner plate in a slice grid left and right, and described grid is equipped with one layer of Stainless Steel Cloth, and the bulk catalyst described in loading in described catalyst layer, is provided with liquid distributor above described bulk catalyst.
Described catalytic section is that the catalytic absorption section described in n section stacks setting from top to bottom, and, column plate layer described in one layer, interval between adjacent catalytic absorption section; Described catalytic absorption section, every section is highly at least 1 meter; Described n is positive integer, and 1��n��100, it is preferable that 6��n��10.
In described catalytic section, the top of the superiors' catalytic absorption section is provided with the column plate that a piece has central well down take, and the lower section of orlop catalytic absorption section is provided with one layer of column plate layer.
Space between described stainless steel liner plate and extraction catalytic distillation inner wall of tower forms gas phase channel; Described downtake and catalyst layer form liquid channel.
Described column plate is valve tray or bubble cap plate or sieve plate, gas phase and liquid phase fully contact at the bubble-cap place of bubble cap plate thus mass transfer, heat transfer and carry out component distribution or distribution further, or gas phase liquid phase at float valve by locating fully contact thus mass transfer, heat transfer and carry out component distribution or distribution further; Or gas phase liquid phase at sieve plate by locating fully contact thus mass transfer, heat transfer and carry out component distribution or distribution further. (extraction liquid containing formaldehyde carries out polycondensation in catalytic section and under the effect of catalyzer and generates DMM1-10, what part did not participate in polycondensation is flowed in the distilling period of extraction catalytic distillation tower containing the extraction liquid of formaldehyde, the gaseous component (formaldehyde) obtained after distillation return by gas phase channel continue to contact with DMM1-2 and/or the extraction liquid that contains formaldehyde thus circulate carry out extracting, polycondensation).
Described liquid distributor is made up of the upflow tube (16) that multiple diameter is 20mm.
Described bulk catalyst, for spherical particle in bulk, column, ring-type, the solid acid resin catalyst of strip; Described solid acid resin catalyst is modified resin catalyst or molecular sieve catalyst, the resin catalyst that the scientific and technological limited-liability company of auspicious environmental protection as triumphant in our company produces.
In technique scheme, when the described catalyzer in catalytic section is module catalyzer, described module catalyzer comprises active catalyst, wire cloth and wire weave plate: described module catalyzer is by described wire cloth, the spaced and parallel setting of wire cloth waved plate, between two panels wire cloth, granules of catalyst described in splendid attire forms catalyst layer, and the described granules of catalyst in this catalyst layer is separated placement by described wire cloth waved plate; Catalyst layer interval described in described module catalyzer is arranged;
Described module catalyzer is fixed in periphery by wire;
Described module catalyzer outline is wrapped by described wire cloth to be closed in geometrical shape; Described geometrical shape is cubes, right cylinder;
One layer, interval or double layer of metal screen waviness plate between described wire cloth and wire cloth;
One layer, described catalyst layer interval or double layer of metal screen waviness plate are arranged; Described catalyst layer arranges by one layer, interval between two layers of described wire cloth or double layer of metal screen waviness plate and the described granules of catalyst of inner filling; Described catalyst layer forms liquid channel, and the wire weave plate layer between adjacent described catalyst layer forms gas phase channel;
Described wire cloth, wire cloth waved plate are made up of stainless material, and described wire cloth or wire cloth waved plate also can be replaced by the stainless steel plate in band hole;
Described wire cloth, wire cloth waved plate are vertically arranged up and down;
Described catalyst layer arranges reinforcement outer wall, using double-deck to described wire cloth and the Stainless Steel Band hole waved plate outer wall as described catalyst layer;
Module catalyzer described in loading in catalytic section, and be reserved with charging space up and down or feed distributor space is installed, described module catalyzer is polylith, stacks setting from top to bottom, and described gas phase channel, liquid channel vertically arrange up and down;
In described catalytic section, gas phase channel and the liquid channel of the module catalyzer described in adjacent layers are oppositely arranged;
Liquid phase feeding in described catalytic section is the extraction liquid containing formaldehyde, gas-phase feed be distilling period distill obtain gaseous component (extraction liquid containing formaldehyde carry out in catalytic section and under the effect of catalyzer polycondensation generate DMM1-10, the extraction liquid containing formaldehyde that part does not participate in polycondensation is flowed in the distilling period of extraction catalytic distillation tower, after distillation, gaseous component (formaldehyde) return through gas phase channel as gas-phase feed continue to contact with DMM1-2 and/or the extraction liquid that contains formaldehyde thus circulate carry out extracting, polycondensation).
Described catalyzer is solid acid resin catalyst, is modified resin catalyst or molecular sieve catalyst, the resin catalyst that the scientific and technological limited-liability company of auspicious environmental protection as triumphant in our company produces.
In technique scheme, described extraction section or distilling period, when structure is identical with traditional filler extraction tower structure, inside is provided with the high filler of N rice, and N is positive integer, 1��N��200, it is preferable that 10��N��100; Filler is stainless steel wave pit plate filler, it is also possible to be Stainless Steel Wire corrugated wire gauze packing.
In technique scheme, described extraction section or distilling period, when structure is identical with traditional perforated-plate extraction tower structure, inside is provided with N layer tower tray, and N is positive integer, 1��N��200, it is preferable that 10��N��100; Its sieve plate can be common sieve plate or efficient sieve plate, and plate spacing can be 100-900mm, it is preferable that 400-600mm.
In technique scheme, described methanol oxidation device, interchanger, fine removing tower, fractionating system, decomposer are existing device.
The advantage of the present invention
1, the outlet gas phase component of methanol oxidation device, the water directly by high-efficiency dehydration tower, oxidation produced is taken off, and residue gas phase is just led to into extraction catalytic distillation tower, collection gaseous extraction, liquid-phase catalysis, and liquid phase is distilled in one, and a step completes;
2, the new technological line preparing polymethoxy dimethyl ether is created;
3, compared with existing Technology, large number quipments, pipeline, internals facility is eliminated;
4, technical process is optimized;
5, save investment, reduce production cost;
6, maximized energy-saving and emission-reduction.
7, for maximization, serialization, intensive manufacture have laid solid foundation.
Accompanying drawing illustrates:
Fig. 1: the process flow sheet of the inventive method;
Fig. 2: the diagrammatic cross-section extracting catalytic distillation tower when catalyzer of the present invention is bulk catalyst;
Fig. 3: the diagrammatic cross-section of catalyst layer, liquid distributor and upflow tube when catalyzer of the present invention is bulk catalyst;
Fig. 4: the diagrammatic cross-section of catalyst layer when catalyzer of the present invention is bulk catalyst;
Fig. 5: the diagrammatic cross-section of module catalyzer when catalyzer of the present invention is module catalyzer;
Fig. 6: the diagrammatic cross-section extracting catalytic distillation tower when catalyzer of the present invention is module catalyzer;
Wherein, 1-methanol oxidation device, 2-interchanger, 3-fine removing tower, 4-reboiler, 5-extracts catalytic distillation tower, 6-decomposition tower, 7-well heater, 8-fractionating system, 9-extraction section, 10-catalytic section, 11-distilling period, 12-stainless steel liner plate, 13-grid, 14-bulk catalyst, 15-liquid distributor, the upflow tube of 16-liquid distributor, 17-central well down take, 18-gas phase channel, 19-column plate, the active catalyst of 20-module catalyzer, 21-wire cloth waved plate, 22-wire cloth, catalyst layer in 23-module catalyzer, the wire cloth of 24-stuck-module catalyzer outline, 25-liquid channel, 26-module catalyzer, 27-charging space, 28-distills space, 29-chord downcomer.
Embodiment
Hereinafter the embodiment of technical solution of the present invention is described in detail, but the present invention is not limited to following description content:
Produce a device of polymethoxy dimethyl ether DMM3-5, as shown in Fig. 1,2,3,4,5,6, comprise methanol oxidation device 1, interchanger 2, fine removing tower 3, extraction catalytic distillation tower 5, decomposition tower 6 and fractionating system 8:
The discharge port of described methanol oxidation device 1 is connected with the inlet mouth a of described interchanger, opening for feed and described interchanger derive hot methanol with discharge opeing mouth a be connected;
The fluid inlet a of described interchanger 2 is connected with the container being contained with cold methanol, and venting port a is connected with the inlet mouth b of described fine removing tower;
The discharge opeing mouth b of described fine removing tower 3 is connected with the container being contained with water, and venting port b is connected with described extraction catalytic distillation tower;
Described extraction distillation column 5, tower top is provided with venting port c and the opening for feed with described methanol oxidation device is connected, being provided with discharge opeing mouth c at the bottom of tower and the fluid inlet with described fractionating system is connected, tower internal upper part to be extraction section 9, middle part be catalytic section 10, bottom are distilling period 11; The bottom of described extraction section is provided with inlet mouth c and the venting port b with described fine removing tower 3 is connected; Fluid inlet b has been offered on the top of described extraction section, and fluid inlet b is divided into two-way, and a road exports A with the light constituent DMM1-2 of fractionating system 8 and is connected, and a road exports B with the light constituent DMM1-2 of decomposition tower 6 and is connected;
The DMM3-5 of described fractionating system 8 exports A and is connected with recovering device, and target product DMM3-5, DMM6-10 outlet of gathering is connected with the DMM6-10 import of described decomposition tower 6;
The DMM3-5 of described decomposition tower 6 exports B and is connected with recovering device, and gather target product DMM3-5.
Described decomposition tower 6, bottom is provided with the well heater 7 regulating temperature.
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 has the distillation space 28 of heating bottom, and distillation space is equipped with the reboiler 4 regulating temperature; The described catalyzer in catalytic section is module catalyzer 26 or bulk catalyst 14:
When the described catalyzer in catalytic section 10 is bulk catalyst 14, described catalytic section is arranged at interval from top to bottom by catalyst layer and column plate layer, and between catalyst layer and catalyst layer, one layer, interval column plate layer forms one section of catalytic absorption section; Described column plate layer stacks 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, and the central authorities of descending trays are provided with central well down take 17; Described catalyst layer is arranged by each fixing a slice stainless steel liner plate 12 of a slice grid about 13, described grid is equipped with one layer of Stainless Steel Cloth, bulk catalyst described in loading in described catalyst layer, is provided with liquid distributor 15 above described bulk catalyst.
Described catalytic section 10 stacks setting from top to bottom for the catalytic absorption section described in n section, and, column plate layer described in one layer, interval between adjacent catalytic absorption section; Described catalytic absorption section, every section is highly at least 1 meter; Described n is positive integer, and 1��n��100, it is preferable that 6��n��10.
In described catalytic section 10, the top of the superiors' catalytic absorption section is provided with the column plate 19 that a piece has central well down take 17, and the lower section of orlop catalytic absorption section is provided with one layer of column plate layer.
Space between described stainless steel liner plate and extraction catalytic distillation inner wall of tower forms gas phase channel 18; Described downtake 17 and catalyst layer form liquid channel.
Described column plate 19 is valve tray or bubble cap plate or sieve plate, gas phase and liquid phase fully contact at the bubble-cap place of bubble cap plate thus mass transfer, heat transfer and carry out component distribution or distribution further, or gas phase liquid phase at float valve by locating fully contact thus mass transfer, heat transfer and carry out component distribution or distribution further; Or gas phase liquid phase at sieve plate by locating fully contact thus mass transfer, heat transfer and carry out component distribution or distribution further.
The upflow tube 16 that described liquid distributor 15 is 20mm by multiple diameter forms.
Described bulk catalyst 14, for spherical particle in bulk, column, ring-type, the solid acid resin catalyst of strip; Described solid acid resin catalyst is modified resin catalyst or molecular sieve catalyst.
When the described catalyzer in catalytic section is module catalyzer 26, described module catalyzer comprises active catalyst 20, wire cloth 22 and wire weave plate 21: described module catalyzer is by described wire cloth, the spaced and parallel setting of wire cloth waved plate, between two panels wire cloth, catalyzer 20 particle described in splendid attire forms catalyst layer 23, and the described granules of catalyst in this catalyst layer is separated placement by described wire cloth waved plate; Catalyst layer interval described in described module catalyzer is arranged;
Described module catalyzer is fixed in periphery by wire;
Described module catalyzer outline is wrapped by described wire cloth 24 to be closed in geometrical shape; Described geometrical shape is cubes, right cylinder;
One layer, interval or double layer of metal screen waviness plate between described wire cloth and wire cloth;
One layer, described catalyst layer interval or double layer of metal screen waviness plate are arranged; Described catalyst layer arranges by one layer, interval between two layers of described wire cloth or double layer of metal screen waviness plate and the described granules of catalyst of inner filling; Described catalyst layer forms liquid channel 25, and the wire weave plate layer between adjacent described catalyst layer forms gas phase channel 18;
Described wire cloth, wire cloth waved plate are made up of stainless material, and described wire cloth or wire cloth waved plate also can be replaced by the stainless steel plate in band hole;
Described wire cloth, wire cloth waved plate are vertically arranged up and down;
Described catalyst layer arranges reinforcement outer wall, using double-deck to described wire cloth and the Stainless Steel Band hole waved plate outer wall as described catalyst layer;
Module catalyzer 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 catalyzer is polylith, stacks setting from top to bottom, and described gas phase channel, liquid channel vertically arrange up and down;
In described catalytic section, gas phase channel and the liquid channel of the module catalyzer described in adjacent layers are oppositely arranged;
Liquid phase feeding in described catalytic section is the extraction liquid containing formaldehyde, and gas-phase feed is that distilling period distills the gaseous component obtained.
Described catalyzer 20 is solid acid resin catalyst, is 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 high filler of N rice, and N is positive integer, 1��N��200, it is preferable that 10��N��100; Filler is stainless steel wave pit plate filler, it is also possible to be Stainless Steel Wire corrugated wire gauze packing.
Described extraction section or distilling period, when structure is identical with traditional perforated-plate extraction tower structure, inside is provided with N layer tower tray, and N is positive integer, 1��N��200, it is preferable that 10��N��100; Its sieve plate can be common sieve plate or efficient sieve plate, and plate spacing can be 100-900mm, it is preferable that 400-600mm.
Described methanol oxidation device, interchanger, fine removing tower, fractionating system, decomposer are existing device.
Below in conjunction with specific embodiment, the inventive method is set forth further:
Embodiment 1:
Prepare a method of polymethoxy dimethyl ether DMM3-5, comprise the following steps:
(1) heat exchange:
Methyl alcohol and air are in methanol oxidation device, taking traditional two methods as preparation method, produce the gas mixture containing formaldehyde gas, this gas mixture is discharged from methanol oxidation device discharge port and is entered in interchanger, this interchanger is tubular heat exchange, Guan Cheng enters the cold methyl alcohol of oxidic raw materials, and shell side enters the gas mixture obtained; Interchanger inlet temperature: 260 DEG C, temperature out: 125 DEG C.
(2) essence dehydration:
Described gas mixture imports to after step (1) heat exchange and carries out essence dehydration in fine removing tower, and fine removing tower inlet temperature is: 110-115 DEG C, and 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; In the material of detection tower top outlet, the molar content of water is less than 0.1% for qualified, obtains almost not moisture mixed gas;
(3) extraction, catalysis and distillation:
The qualified material of step 2 being imported in extraction catalytic distillation tower, catalyzer is module catalyzer (our company's self-control D006 type acid resin catalyst) operational condition:
Extraction section: upper temp 55-60 DEG C, pressure 0.10-0.20Mpa, temperature of lower 70-80 DEG C; Extraction agent DMM1-2 molar weight is 2 times of formaldehyde molar weight in the mixed gas obtained after essence dehydration, and the air speed of extraction agent 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, the air speed of the extraction liquid containing formaldehyde is 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, thief hole is top (i.e. the top of extraction section) and bottom (i.e. the bottom of the distilling period) thief hole of extraction catalytic distillation tower, analytical instrument: gas chromatograph Agilent 7820, top gaseous formaldehyde content is about 0, bottom liquid phases export goal product content is 91.5%, and namely DMM3-5 selectivity is 91.5%.
Embodiment 2:
Preparing a method of polymethoxy dimethyl ether DMM3-5, operation steps is substantially the same manner as Example 1, institute the difference is that catalyzer be bulk catalyst (our company self-control the high temperature resistant acid resin catalyst of D008 type):
Sampling in four hours one is analyzed, thief hole is top (i.e. the top of extraction section) and bottom (i.e. the bottom of the distilling period) thief hole of extraction catalytic distillation tower, analytical instrument: gas chromatograph Agilent 7820, top gaseous formaldehyde content is about 0, bottom liquid phases export goal product content is 91.0%, and namely DMM3-5 selectivity is 91.0%.
Embodiment 3:
Preparing a method of polymethoxy dimethyl ether DMM3-5, operation steps is substantially the same manner as Example 1, institute the difference is 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; Extraction agent DMM1-2 molar weight is 2 times of formaldehyde molar weight in the mixed gas obtained after essence dehydration, and the air speed of extraction agent 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, the air speed of the extraction liquid containing formaldehyde is 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, thief hole is top (i.e. the top of extraction section) and bottom (i.e. the bottom of the distilling period) thief hole of extraction catalytic distillation tower, analytical instrument: gas chromatograph Agilent 7820, top gaseous formaldehyde content is about 0, bottom liquid phases export goal product content is 92.5%, and namely DMM3-5 selectivity is 92.5%.
Embodiment 4:
Preparing a method of polymethoxy dimethyl ether DMM3-5, operation steps is substantially the same manner as Example 2, institute the difference is 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; Extraction agent DMM1-2 molar weight is 2 times of formaldehyde molar weight in the mixed gas obtained after essence dehydration, and the air speed of extraction agent 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, the air speed of the extraction liquid containing formaldehyde is 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, thief hole is top (i.e. the top of extraction section) and bottom (i.e. the bottom of the distilling period) thief hole of extraction catalytic distillation tower, analytical instrument: gas chromatograph Agilent 7820, top gaseous formaldehyde content is about 0, bottom liquid phases export goal product content is 91.5%, and namely DMM3-5 selectivity is 91.5%.
Embodiment 5:
Preparing a method of polymethoxy dimethyl ether DMM3-5, operation steps is substantially the same manner as Example 1, institute the difference is 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; Extraction agent DMM1-2 molar weight is 2 times of formaldehyde molar weight in the mixed gas obtained after essence dehydration, and the air speed of extraction agent 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, the air speed of the extraction liquid containing formaldehyde is 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, thief hole is top (i.e. the top of extraction section) and bottom (i.e. the bottom of the distilling period) thief hole of extraction catalytic distillation tower, analytical instrument: gas chromatograph Agilent 7820, top gaseous formaldehyde content is about 0, bottom liquid phases export goal product content is 92.0%, and namely DMM3-5 selectivity is 92.0%.
Above-mentioned example just for technical conceive and the technology feature of the present invention are described, can not limit the scope of the invention with this. All equivalent transformations of doing according to the essence of the present invention or modification, all should be encompassed within protection scope of the present invention.

Claims (10)

1. produce a method of polymethoxy dimethyl ether DMM3-5, comprise the following steps:
(1) heat exchange: methyl alcohol and air, taking two traditional methods as preparation method, obtain the mixed gas containing formaldehyde gas; Obtained mixed gas is carried out heat exchange;
(2) essence dehydration: the mixed gas after step (1) heat exchange is carried out essence dehydration until the moisture molar content in mixed gas is less than 0.1%;
(3) extraction, catalysis and distillation: the mixed gas obtained after the de-moisture removal of step (2) is extracted with extraction agent DMM1-2, the mixture that extraction obtains carries out polycondensation under catalyzer existence condition and generates DMM1-10, in extraction, the mixture that obtains of catalysis, non-targeted product and light constituent continue as extraction agent after distillation, again carry out extracting, polycondensation;
(4) fractionation: be passed in fractionating system to carry out fractionation by the polycondensation product DMM1-10 that step (3) obtains, wherein: target product DMM3-5 gathers, light constituent DMM1-2 is back to step (3) resume and carries out polycondensation, and heavy constituent DMM6-10 is passed in decomposer;
(5) decompose: being passed in decomposer by the heavy constituent DMM6-10 that step (4) obtains and decompose, wherein: target product DMM3-5 gathers, light constituent DMM1-2 is back to step (3) resume and carries out polycondensation.
2. method according to claim 1, it is characterised in that, described method is specially:
(1) heat exchange: by methyl alcohol and air in methanol oxidation device (1) taking two traditional methods as preparation method, the obtained mixed gas containing formaldehyde gas; Described mixed gas is expelled in interchanger (2) from methanol oxidation device and carries out heat exchange;
The inlet temperature of described interchanger is 100-800 DEG C, and temperature out is 100-200 DEG C;
(2) essence dehydration: the mixed gas of step (1) after interchanger heat exchange is passed in fine removing tower (3) and carries out essence dehydration, be less than 0.1% to the moisture molar content in mixed gas;
Described smart dehydration conditions is: fine removing tower inlet mouth b place 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) extraction, catalysis and distillation: the mixed gas obtained after step (2) essence dehydration is passed in the extraction section (9) of extraction catalytic distillation tower (5), form the extraction liquid containing formaldehyde after leading to the mixed gas described in absorbing into extraction agent DMM1-2, DMM1-2 extraction in extraction section simultaneously; The described extraction liquid containing formaldehyde carries out polycondensation in the catalytic section (10) of extraction catalytic distillation tower and under the effect of catalyzer and generates DMM1-10, the extraction liquid containing formaldehyde that part does not participate in polycondensation is flowed in the distilling period (11) of extraction catalytic distillation tower, after distillation, gaseous component return through gas phase channel (18) continue to contact with extraction agent DMM1-2 and/or the extraction liquid that contains formaldehyde carry out extracting, polycondensation;
In described extraction section: in the mixed gas that described DMM1-2 and essence obtain after dewatering, the mol ratio of formaldehyde is 1-10:1; Air speed when DMM1-2 enters extraction section is 0.1-5.5h-1; Described extraction conditions is: temperature is normal 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, pressure is 0.1-3.0Mpa; The mass space velocity of the described extraction liquid containing formaldehyde is 0.1-5.5h-1; Described catalyzer is solid acid resin catalyst;
In described distilling period: temperature 80-300 DEG C, pressure 0.1-3.0Mpa.
(4) fractionation: the product D MM1-10 that step (3) obtains is passed in fractionating system (8) and carries out fractionation; Wherein, the target product DMM3-5 that fractionation obtains gathers, the light constituent DMM1-2 that fractionation obtains is back to recycle in the extraction catalytic distillation tower (5) described in step (3), and the heavy constituent DMM6-10 that fractionation obtains is passed in decomposer (6);
(5) decompose: the heavy constituent DMM6-10 that step (4) obtains is passed in decomposer (6) and decomposes, wherein, decompose the target product DMM3-5 obtained to gather, decompose the light constituent DMM1-2 obtained and be back to recycle in the extraction catalytic distillation tower (5) described in step (3).
3. produce a device of polymethoxy dimethyl ether DMM3-5, comprise methanol oxidation device (1), interchanger (2), fine removing tower (3), extraction catalytic distillation tower (5), decomposition tower (6) and fractionating system (8):
The described discharge port of methanol oxidation device (1) is connected with the inlet mouth a of described interchanger, opening for feed and described interchanger derive hot methanol with discharge opeing mouth a be connected;
The fluid inlet a of described interchanger (2) is connected with the container being contained with cold methanol, and venting port a is connected with the inlet mouth b of described fine removing tower;
The discharge opeing mouth b of described fine removing tower (3) is connected with the container being contained with water, and venting port b is connected with described extraction catalytic distillation tower;
Described extraction distillation column (5), tower top is provided with venting port c and the opening for feed with described methanol oxidation device is connected, being provided with discharge opeing mouth c at the bottom of tower and the fluid inlet with described fractionating system is connected, tower internal upper part to be extraction section (9), middle part be catalytic section (10), bottom are distilling period (11); The bottom of described extraction section is provided with inlet mouth c and the venting port b with described fine removing tower (3) is connected; Fluid inlet b has been offered on the top of described extraction section, and fluid inlet b is divided into two-way, and a road exports A with the light constituent DMM1-2 of fractionating system (8) and is connected, and a road exports B with the light constituent DMM1-2 of decomposition tower (6) and is connected;
The DMM3-5 of described fractionating system (8) exports A and is connected with recovering device, and target product DMM3-5, DMM6-10 outlet of gathering is connected with the DMM6-10 import of described decomposition tower (6);
The DMM3-5 of described decomposition tower (6) exports B and is connected with recovering device, and gather target product DMM3-5;
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 the distillation space (28) bottom with heating, distillation space is equipped with the reboiler (4) regulating temperature; The described catalyzer in catalytic section is module catalyzer (26) or bulk catalyst (14);
Described decomposition tower (6), bottom is provided with the well heater (7) regulating temperature.
4. device according to claim 3, it is characterized in that, when the described catalyzer in catalytic section (10) is bulk catalyst (14), described catalytic section is arranged at interval from top to bottom by catalyst layer and column plate layer, and between catalyst layer and catalyst layer, one layer, interval column plate layer forms one section of catalytic absorption section; Described column plate layer stacks 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 slice stainless steel liner plate (12) in a slice grid (13) left and right, described grid is equipped with one layer of Stainless Steel Cloth, bulk catalyst described in loading in described catalyst layer, is provided with liquid distributor (15) above described bulk catalyst;
Described catalytic section (10) stacks setting from top to bottom for the catalytic absorption section described in n section, and, column plate layer described in one layer, interval between adjacent catalytic absorption section; Described catalytic absorption section, every section is highly at least 1 meter; Described n is positive integer, and 1��n��100;
In described catalytic section (10), the top of the superiors' catalytic absorption section is provided with the column plate (19) that a piece has central well down take (17), and the lower section of orlop catalytic absorption section is provided with one layer of column plate layer;
The upflow tube (16) that described liquid distributor (15) is 20mm by multiple diameter forms.
5. device according to claim 4, it is characterised in that, the space between described stainless steel liner plate (12) and extraction catalytic distillation tower (5) inwall forms gas phase channel (18); Described downtake (17) and catalyst layer form liquid channel (25).
6. device according to claim 4, it is characterized in that, described column plate (19) is valve tray or bubble cap plate or sieve plate, gas phase and liquid phase fully contact at the bubble-cap place of bubble cap plate thus mass transfer, heat transfer and carry out component distribution or distribution further, or gas phase liquid phase at float valve by locating fully contact thus mass transfer, heat transfer and carry out component distribution or distribution further; Or gas phase liquid phase at sieve plate by locating fully contact thus mass transfer, heat transfer and carry out component distribution or distribution further.
7. device according to claim 3, it is characterized in that, when the described catalyzer in catalytic section is module catalyzer (26), described module catalyzer comprises catalyzer (20), wire cloth (22) and wire weave plate (21): described module catalyzer is by described wire cloth, the spaced and parallel setting of wire cloth waved plate, between two panels wire cloth, catalyzer (20) particle described in splendid attire forms catalyst layer (23), and the described granules of catalyst in this catalyst layer is separated placement by described wire cloth waved plate, catalyst layer interval described in described module catalyzer is arranged, described wire cloth, wire cloth waved plate are made up of stainless material, and described wire cloth or wire cloth waved plate also can be replaced by the stainless steel plate in band hole.
8. device according to claim 7, it is characterised in that, one layer, interval or double layer of metal screen waviness plate between described wire cloth and wire cloth; One layer, described catalyst layer interval or double layer of metal screen waviness plate are arranged; Described catalyst layer arranges by one layer, interval between two layers of described wire cloth or double layer of metal screen waviness plate and the described granules of catalyst of inner filling; Described catalyst layer forms liquid channel (25), and the wire weave plate layer between adjacent described catalyst layer forms gas phase channel (18).
9. device according to claim 7, it is characterized in that, module catalyzer (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 catalyzer is polylith, stack setting from top to bottom, and described gas phase channel, liquid channel vertically arrange up and down; Described wire cloth, wire cloth waved plate are vertically arranged up and down; In described catalytic section, gas phase channel and the liquid channel of the module catalyzer described in adjacent layers are oppositely arranged.
10. device according to claim 7, it is characterised in that, described module catalyzer is fixed in periphery by wire; Described module catalyzer outline is wrapped by described wire cloth (24) to be closed in geometrical shape; Described geometrical shape is cubes, right cylinder; Described catalyst layer arranges reinforcement outer wall, using double-deck to described wire cloth and the Stainless Steel Band hole waved plate outer wall as described catalyst layer.
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