CN210237494U - Multi-stage reaction rectification synthesis process device for polymethoxy dimethyl ether - Google Patents
Multi-stage reaction rectification synthesis process device for polymethoxy dimethyl ether Download PDFInfo
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- CN210237494U CN210237494U CN201920511646.4U CN201920511646U CN210237494U CN 210237494 U CN210237494 U CN 210237494U CN 201920511646 U CN201920511646 U CN 201920511646U CN 210237494 U CN210237494 U CN 210237494U
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Abstract
The utility model provides a gather multistage reaction rectification synthesis process units of methoxy dimethyl ether, including multistage reaction rectifying column and vapor permeation equipment, multistage reaction rectifying column includes the rectifying section that sets up from top to bottom, multistage reaction section, stripping section, wherein multistage reaction section is the reaction section more than two, set up the separation section between two adjacent reaction sections and carry out the separation between each material, the reaction section divide into methylal reaction section and gather methoxy dimethyl ether reaction section two kinds, two kinds of reaction sections are arranged in turn, all set up methylal aqueous solution feed inlet and methyl alcohol feed inlet on each methylal reaction section, wherein the methyl alcohol feed inlet is below the methylal feed inlet; a formaldehyde water solution feeding port is arranged on each polyoxymethylene dimethyl ether reaction section; the top of the multi-section reaction rectifying tower is provided with a gas extraction outlet which is connected with steam permeation equipment. The device has the advantages of simple process flow, low equipment investment, stable product quality, low energy consumption and the like.
Description
Technical Field
The utility model belongs to the technical field of chemical production equipment, mainly relate to a gather multistage reaction rectification synthesis process units of methoxy dimethyl ether.
Background
Polyoxymethylene dimethyl ethers, abbreviated as DMMn or PODEN, have received much attention as novel diesel additives due to their high oxygen content and cetane number. Proper amount of polymethoxy dimethyl ether is added into diesel oil, so that the combustion efficiency can be effectively improved and the emission of soot in tail gas can be reduced on the premise of not reforming the structure of a diesel engine.
At the present stage, the preparation process of polymethoxy dimethyl ether mainly adopts a process technology of first reaction and then separation, and is limited by chemical balance, the yield of a target product DMM 3-5 cannot be greatly improved, the flow rate of a circulating stream is large, the overall energy consumption of the process is high, and the economy is low, such as: the patent CN104355973B proposes a method for preparing polymethoxy dimethyl ether by fixed bed reactive distillation, which uses methylal and trioxymethylene as reactants to perform secondary series reaction in a fixed bed reactor and a reactive distillation column, and then obtains polymethoxy dimethyl ether by multi-step separation. Patent CN104722249A proposes a multistage formula reaction tower and a poly methoxy dimethyl ether synthesis process units for gathering methoxy dimethyl ether is synthetic, this technology adopts reaction absorption tower and the coupling of multistage formula reaction rectifying column to prepare gather methoxy dimethyl ether, but reactant fails in this technology in the reaction absorption tower in time to take out the reaction zone, this step reaction conversion rate is still lower, and do not have the segmentations between each reaction section of multistage formula reaction rectifying column, the effect of the reaction product of not removing fast, and the raw materials price of raw materials methylal and gaseous phase formaldehyde is higher, the whole economic nature of flow is still on the low side.
SUMMERY OF THE UTILITY MODEL
To the problem and the defect that above-mentioned exists, the utility model aims at providing a gather multistage reaction rectification synthesis process units of methoxy dimethyl ether, this device has advantages such as process flow is simple, the equipment investment is lower, product quality is stable, the energy consumption is lower.
The technical scheme of the utility model as follows:
the utility model discloses a gather multistage reaction rectification synthesis process units of methoxy dimethyl ether, including multistage reaction rectifying column and vapor permeation equipment.
The multi-section reaction rectifying tower is provided with a reboiler, 2n (n is more than or equal to 1) reaction sections are arranged in the tower, separation sections are arranged between the reaction sections for separating substances, the reaction sections comprise methylal reaction sections and polymethoxy dimethyl ether reaction sections, the two reaction sections are alternately arranged, the methylal reaction sections are arranged below the polymethoxy dimethyl ether reaction sections in a group consisting of every two reaction sections from the tower kettle, the uppermost part of the multi-section reaction rectifying tower is provided with a rectifying section, and the lowermost part of the multi-section reaction rectifying tower is provided with a stripping section for separating substances; the methylal reaction section is provided with a methylal aqueous solution feed port and a methanol feed port, the two feed ports are respectively connected with a formaldehyde aqueous solution feed pipeline and a methanol feed pipeline, and the methanol feed port is arranged below the methylal feed port; the polyoxymethylene dimethyl ether reaction section is provided with a formaldehyde water solution feed inlet and is connected with a formaldehyde water solution feed pipeline; the top of the multi-section reaction rectifying tower is provided with a gas phase extraction outlet, and the back of the tower kettle reboiler is provided with a tower kettle liquid phase extraction outlet.
The steam permeation device is provided with a multi-section reaction rectifying tower top complete condenser behind, the device is provided with a gas phase feed inlet, a permeation side extraction outlet and a interception side extraction outlet, the gas phase feed inlet is connected with the multi-section reaction rectifying tower top gas phase extraction outlet, the permeation side extraction outlet is connected with a water extraction pipeline, the interception side extraction outlet is connected with the tower top complete condenser feed inlet, a tower top reflux pipeline and a tower top extraction pipeline are arranged behind the complete condenser, and the tower top reflux pipeline is connected with the multi-section reaction rectifying tower top reflux outlet.
Filling a methylal reaction section of the multi-section reaction rectifying tower with a methylal reaction acidic solid catalyst, filling a polymethoxy dimethyl ether reaction section with a polymerization reaction acidic solid catalyst, wherein the partial tower internals are catalytic filler type or catalytic tower plate type tower internals; the tower top rectifying section, the tower bottom stripping section and the separating section tower internals among the reaction sections of the multi-section reaction rectifying tower are packing or tower trays.
A pervaporation membrane is arranged in the steam permeation device, and is a permeable molecular sieve membrane, preferably a NaA membrane.
The methylal reaction section comprises catalytic fillers or catalytic trays, the fillers are 0.1-2 m/layer, the trays are 2-15 blocks/layer, the polymethoxy dimethyl ether reaction section comprises catalytic fillers or catalytic trays, the fillers are 0.1-3 m/layer, the trays are 2-25 blocks/layer, the separation section between the two reaction sections comprises fillers or trays, the fillers are 0.2-2.5 m, the trays are 4-20 blocks, the rectification section comprises fillers or trays, the fillers are 0.2-3 m, the trays are 4-25 blocks, the stripping section comprises fillers or trays, the fillers are 0.2-2.5 m, and the trays are 4-20 blocks.
Compared with the prior art, the utility model discloses there is following beneficial effect:
1. the device couples the preparation process of methylal with the preparation process of polymethoxy dimethyl ether, and can directly utilize methylal generated by the reaction of methanol and formaldehyde to carry out polymerization reaction, and simultaneously, methanol in the hydrolysis process of methylal can also carry out secondary reaction in the methylal reaction section, thereby eliminating the separation and circulation process of methanol.
2. The device utilizes the vapor permeation equipment to separate in a water system, avoids the separation difficulty caused by azeotropic composition in the system, effectively removes water in the reaction system, does not need to introduce other substances in the separation process, and shortens the flow of the separation process.
Drawings
FIG. 1 is a schematic diagram of a multi-stage reaction rectification synthesis process device of polymethoxy dimethyl ether.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments, which are illustrative, not restrictive, and the scope of the invention should not be limited thereto.
The utility model discloses a gather multistage reaction rectification synthesis process units of methoxy dimethyl ether, including multistage reaction rectifying column 1 and vapor permeation equipment 2.
The multi-section reactive distillation tower is provided with a reboiler 4 at the bottom, 2n (n is more than or equal to 1) reaction sections are arranged in the tower, separation sections are arranged between the reaction sections for separating substances, the reaction sections comprise methylal reaction sections and polymethoxy dimethyl ether reaction sections, the two reaction sections are alternately arranged, the methylal reaction sections are arranged below the polymethoxy dimethyl ether reaction sections in a group consisting of every two reaction sections from the tower bottom, the rectifying section is arranged at the upper part of the multi-section reactive distillation tower, and the stripping section is arranged at the lower part of the multi-section reactive distillation tower and used for separating substances; the methylal reaction section is provided with a methylal aqueous solution feed port and a methanol feed port, the two feed ports are respectively connected with a formaldehyde aqueous solution feed pipeline and a methanol feed pipeline, and the methanol feed port is arranged below the methylal feed port; the polyoxymethylene dimethyl ether reaction section is provided with a formaldehyde water solution feed inlet and is connected with a formaldehyde water solution feed pipeline; the top of the multi-section reaction rectifying tower is provided with a gas phase extraction outlet, and the back of the tower kettle reboiler is provided with a tower kettle liquid phase extraction outlet.
The steam permeation equipment is provided with a multi-section reaction rectifying tower top complete condenser 3 at the back, the equipment is provided with a gas phase feed inlet, a permeation side extraction outlet and a interception side extraction outlet, the gas phase feed inlet is connected with the gas phase extraction outlet at the top of the multi-section reaction rectifying tower, the permeation side extraction outlet is connected with a water extraction pipeline, the interception side extraction outlet is connected with the feed inlet of the tower top complete condenser, a tower top reflux pipeline and a tower top extraction pipeline are arranged at the back of the complete condenser, and the tower top reflux pipeline is connected with the tower top reflux port of the multi-section reaction rectifying tower.
The process method of the device comprises the following steps:
feeding methanol and formaldehyde aqueous solution from a feed inlet on a methylal reaction section of the multistage reaction rectifying tower, reacting to generate methylal, and allowing the methylal with a lower boiling point to enter a polymethoxy dimethyl ether reaction section on the upper side of the methylal reaction section under the rectifying action of the methylal reaction section and a separation section on the upper side of the reaction section; feeding a formaldehyde water solution from a feed inlet of the polymethoxy dimethyl ether reaction section, reacting with methylal to generate a mixture with a target product polymerization degree larger than 2 and methylal hydrolysis product methanol, wherein due to the rectification action of the polymethoxy dimethyl ether reaction section and separation sections at the upper side and the lower side of the polymethoxy dimethyl ether reaction section, methanol, water and methylal which is not completely reacted enter the upper side area of the polymethoxy dimethyl ether reaction section, and the target product enters the lower side area of the polymethoxy dimethyl ether reaction section; if a methylal reaction section exists on the upper side of the polymethoxy dimethyl ether reaction section, the methanol generated by the side reaction of the polymethoxy dimethyl ether reaction section, namely hydrolysis of methylal, can carry out secondary reaction at the section to generate methylal; according to the boiling points of all substances in the tower, a target product DMM3-8 is finally extracted from the tower bottom of the multi-stage reaction rectifying tower, a mixture of methylal, methanol, water and DMM2 is finally extracted from the tower top, the mixture enters steam permeation equipment to remove water in the mixture, and part of the dehydrated substances reflows to the top of the multi-stage reaction rectifying tower and is extracted partially; the extract at the top of the tower can be separated by a subsequent light component separation tower and returns to the corresponding reaction area of the multi-section reaction rectifying tower for secondary reaction.
The utility model provides a poly methoxy dimethyl ether's multistage reaction rectification synthesis process units has described through preferred embodiment, and relevant technical personnel obviously can not deviate from the utility model discloses content, spirit and within range change or suitable change and constitute equipment and process flow this paper, realize the utility model discloses the technique. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.
Claims (4)
1. A multi-stage reaction rectification synthesis process device of polymethoxy dimethyl ether is characterized in that: comprises a multi-section reactive distillation tower and vapor permeation equipment,
the multi-section reaction rectifying tower comprises a rectifying section, a multi-section reaction section and a stripping section which are arranged from top to bottom, wherein the multi-section reaction section comprises more than two reaction sections, a separation section is arranged between every two adjacent reaction sections for separating substances, the reaction sections are divided into a methylal reaction section and a polymethoxy dimethyl ether reaction section, the two reaction sections are alternately arranged, the methylal reaction section is arranged at the bottom end, and the polymethoxy dimethyl ether reaction section is arranged at the top end; a methylal aqueous solution feed port and a methanol feed port are arranged on each methylal reaction section, the two feed ports are respectively connected with a formaldehyde aqueous solution feed pipeline and a methanol feed pipeline, and the methanol feed port is arranged below the methylal feed port; a formaldehyde water solution feeding port is arranged on each polyoxymethylene dimethyl ether reaction section and is connected with a formaldehyde water solution feeding pipeline; the top of the multi-section reaction rectifying tower is provided with a gas extraction outlet which is connected with steam permeation equipment; the tower kettle of the multi-section reaction rectifying tower is provided with a reboiler, and a tower kettle liquid phase extraction port is arranged behind the reboiler;
the steam permeation device is provided with a multi-section reaction rectifying tower top complete condenser behind, the device is provided with a gas phase feed inlet, a permeation side extraction outlet and a interception side extraction outlet, the gas phase feed inlet is connected with the multi-section reaction rectifying tower top gas phase extraction outlet, the permeation side extraction outlet is connected with a water extraction pipeline, the interception side extraction outlet is connected with the tower top complete condenser feed inlet, a tower top reflux pipeline and a tower top extraction pipeline are arranged behind the complete condenser, and the tower top reflux pipeline is connected with the multi-section reaction rectifying tower top reflux outlet.
2. The multi-stage reaction rectification synthesis process device of polymethoxy dimethyl ether according to claim 1, characterized in that: the tower internals of each reaction section are catalytic filler type or catalytic tower plate type tower internals.
3. The multi-stage reaction rectification synthesis process device of polymethoxy dimethyl ether according to claim 1, characterized in that: the internal parts of the rectifying section, the stripping section and the separating section are all packing or trays.
4. The multi-stage reaction rectification synthesis process device of polymethoxy dimethyl ether according to claim 1, characterized in that: the vapor permeation equipment is internally provided with a pervaporation membrane which is a permeable molecular sieve membrane.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920511646.4U CN210237494U (en) | 2019-04-16 | 2019-04-16 | Multi-stage reaction rectification synthesis process device for polymethoxy dimethyl ether |
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| CN201920511646.4U CN210237494U (en) | 2019-04-16 | 2019-04-16 | Multi-stage reaction rectification synthesis process device for polymethoxy dimethyl ether |
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| CN210237494U true CN210237494U (en) | 2020-04-03 |
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