CN210237495U - Reactive distillation-steam permeation coupling device for synthesizing polymethoxy dimethyl ether - Google Patents
Reactive distillation-steam permeation coupling device for synthesizing polymethoxy dimethyl ether Download PDFInfo
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Abstract
The utility model relates to a reaction rectification-steam permeation coupling device for gathering methoxy dimethyl ether is synthetic, including gathering methoxy dimethyl ether reaction rectifying tower, one-level product refining tower, second grade product refining tower, steam permeation equipment, first light component knockout tower, high pressure knockout tower, low pressure knockout tower, gather and set up raw materials feed inlet on the methoxy dimethyl ether reaction rectifying tower, DMM6 ~ 10 retrieves the feed inlet, DMM2 retrieves the feed inlet, gather the gaseous phase feed inlet of methoxy dimethyl ether reaction rectifying tower top gas phase sampling exit linkage steam permeation equipment. The device overcomes the defects of low yield of the target product DMM3-5, large flow internal circulation amount, high energy consumption and the like in the prior art, and can break the limitation of reaction balance, greatly improve the conversion rate of raw materials and the selectivity and yield of DMM 3-5.
Description
Technical Field
The utility model belongs to the technical field of chemical production equipment, a synthetic and separation refining of gathering methoxy dimethyl ether is related to, especially a reaction rectification-vapor permeation coupling device for gathering methoxy dimethyl ether is synthetic.
Background
The reactants of polyoxymethylene dimethyl ethers are synthesized by using a compound for providing paraformaldehyde (formaldehyde, trioxymethylene and paraformaldehyde) and a compound for providing a blocked methyl group (methanol, dimethyl ether, methylal and the like) under the catalysis of an acid catalyst. For example, 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 polymethoxy dimethyl ether reactive distillation column, and then performs multi-step separation; patent CN104722249A proposes a method for obtaining polymethoxy dimethyl ether by two-part reaction of methylal and gas-phase formaldehyde through a packed reaction tower and a multi-stage reaction tower. The methods have the defects of high reaction raw material price, low product economy and lack of market competitiveness of anhydrous chain growth reactants (such as trioxymethylene, gas-phase formaldehyde and paraformaldehyde). Patent CN108383696A provides a method for preparing polymethoxy dimethyl ether by reacting water-containing trioxymethylene with methylal, but in the method, a reactor is used for preparing the polymethoxy dimethyl ether, the components of the product after reaction are complex and have trace water, the subsequent separation difficulty is high, the energy consumption is high when the process is used for obtaining DMM3-5, and the product economy is still limited.
SUMMERY OF THE UTILITY MODEL
Aiming at the problems and defects, the utility model aims at providing a reactive distillation-steam permeation coupling device for synthesizing polymethoxy dimethyl ether, which has the advantages of simple process flow, lower equipment investment, convenient operation, stable product quality, lower energy consumption and the like.
The utility model discloses a first technical scheme as follows:
a reactive distillation-steam permeation coupling device for synthesizing polymethoxy dimethyl ether comprises a polymethoxy dimethyl ether reactive distillation tower, a primary product refining tower, a secondary product refining tower, steam permeation equipment, a first light component separation tower, a high-pressure separation tower, a low-pressure separation tower, a methylal mixer and a DMM2 mixer.
The tower kettle of the polymethoxy dimethyl ether reactive rectifying tower is provided with a reboiler, the polymethoxy dimethyl ether reactive rectifying tower is provided with two raw material feed inlets, DMM 6-10 recovery feed inlets and DMM2 recovery feed inlets, the tower top is provided with a gas phase extraction outlet, the tower kettle is provided with a liquid phase extraction outlet, and the two raw material feed inlets are respectively connected with a chain growth raw material feed pipeline and a methylal mixer outlet pipeline.
The primary product refining tower and the secondary product refining tower are both provided with a total condenser at the tower top and a reboiler at the tower bottom, the tower body is provided with a liquid phase feed inlet, the tower top and the tower bottom are both provided with liquid phase extraction outlets, wherein the raw material feed inlet of the primary product refining tower is connected with the bottom liquid phase extraction outlet of the polymethoxy dimethyl ether reaction rectifying tower through a pipeline, and the top extraction outlet of the primary product refining tower is connected with a DMM2 mixer feed pipeline; a raw material feeding port of the secondary product refining tower is connected with a tower bottom liquid phase extraction port of the primary product refining tower through a pipeline, a tower bottom liquid phase extraction port of the secondary product refining tower is connected with a DMM 6-10 recovery feeding port through a pipeline, and a tower top liquid phase extraction port of the secondary product refining tower is connected with a target product extraction pipeline;
the steam infiltration device is provided with a gas phase feed inlet, an infiltration side extraction outlet and an interception side extraction outlet, wherein the gas phase feed inlet is connected with a gas phase extraction outlet at the top of the polymethoxy dimethyl ether reaction rectifying tower, the infiltration side extraction outlet is connected with a water extraction pipeline, a complete condenser at the top of the polymethoxy dimethyl ether reaction rectifying tower is arranged behind the steam infiltration device, the interception side extraction outlet is connected with a feed pipeline of the complete condenser, and a discharge port of the complete condenser at the top of the tower is connected with a reflux port at the top of the polymethoxy dimethyl ether reaction rectifying tower and a liquid phase extraction pipeline at the top of the tower;
the first light component separation tower, the high-pressure separation tower and the low-pressure separation tower are all provided with a total condenser at the tower top and a reboiler at the tower bottom, the tower top and the tower bottom are both provided with liquid phase extraction outlets, a feed inlet of the first light component separation tower is connected with a liquid phase extraction pipeline at the tower top of the polymethoxy dimethyl ether reaction rectification tower, and the tower bottom extraction outlet of the first light component separation tower is connected with a feed pipeline of a DMM2 mixer; the high-pressure separation tower is provided with two feed inlets, one of the two feed inlets is connected with a tower top extraction pipeline of the first light component separation tower, and a tower kettle extraction outlet of the high-pressure separation tower is connected with a feed inlet of a methylal mixer; the low-pressure separation tower is provided with a feed inlet which is connected with a top extraction outlet of the high-pressure separation tower, the top extraction outlet of the low-pressure separation tower is connected with the other feed inlet of the high-pressure separation tower, and a tower kettle of the low-pressure separation tower is connected with a methanol extraction pipeline.
The polymethoxy dimethyl ether reaction rectifying tower consists of a rectifying section, a reaction section and a stripping section, or the reaction section and the rectifying section; the inner parts of the rectifying section and the stripping section are fillers or trays; the reaction section is filled with solid acid catalyst, and the tower internals are catalytic filler type or catalytic tower plate type.
The reaction section of the polymethoxy dimethyl ether reaction rectifying tower is provided with two liquid-phase reactant feeding holes and two circulating material feeding holes; or the reaction section of the polymethoxy dimethyl ether reaction rectifying tower is provided with a liquid phase reactant feeding hole and two circulating material feeding holes, and the reaction section or the stripping section is provided with a gas phase reactant feeding hole.
The two product refining towers, the first light component separation tower, the high-pressure separation tower and the low-pressure separation tower have internal parts which are fillers or trays.
And a pervaporation membrane is arranged in the steam permeation device, and is a permeable molecular sieve membrane, preferably a NaA membrane.
The utility model discloses a second technical scheme has increased the apparatus for producing that gets into the raw materials (trioxymethylene and methylal) of gathering methoxy dimethyl ether reaction rectifying column, and concrete scheme is as follows:
the utility model provides a methylal and high concentration trioxymethylene route methanol system DMMn's new process units, includes formaldehyde preparation facilities, formaldehyde polymerization device, methylal preparation facilities, gathers methoxy dimethyl ether reaction rectification preparation facilities, and formaldehyde preparation facilities's formaldehyde is adopted the export and is passed through the raw materials feed inlet of pipeline connection formaldehyde polymerization device and methylal preparation facilities respectively, and formaldehyde polymerization device's and methylal preparation facilities's main products are adopted the export and are passed through the raw materials feed inlet of pipeline connection gathers methoxy dimethyl ether reaction rectification preparation facilities respectively.
Raw material methanol is subjected to oxidation reaction and water absorption in a formaldehyde preparation device to obtain a formaldehyde water solution, a part of the product is subjected to formaldehyde polymerization to obtain a mixture of trioxymethylene, formaldehyde and trace water, and the other part is subjected to reaction with methanol through a methylal preparation device to obtain high-purity methylal. The mixture of methylal, trioxymethylene, formaldehyde and trace water enters a polymethoxy dimethyl ether reactive distillation preparation device, DMM3-10 and trace DMM2 are obtained from a tower bottom in the reactive distillation process, and then DMM3-5 which is a high-purity target product is obtained through the distillation separation process; obtaining water-containing light components at the tower top, and then obtaining DMM2, methylal and methanol through a membrane separation and dehydration process and a rectification separation process, and returning the DMM2, the methylal and the methanol to the polymethoxy dimethyl ether reaction rectifying tower or a preorder device.
Moreover, the formaldehyde preparation device comprises a methanol evaporator, a gas mixer, a preheater, an oxidation reactor and a water absorption tower which are connected in sequence, wherein the methanol evaporator is provided with a methanol inlet, a steam inlet, a methanol steam outlet and a cooling water outlet, wherein the methyl alcohol steam outlet passes through one of them import of methyl alcohol steam delivery pipe connection gas mixer, another access connection oxygen delivery pipe of gas mixer, the import of gas mixture delivery pipe connection pre-heater is passed through in the export of gas mixer, the top raw materials import of pipe connection oxidation reactor is passed through in the export of pre-heater, the bottom formaldehyde gas mixture of oxidation reactor is adopted the mouth and is connected the feed inlet at the bottom of water absorption tower, the top of the tower system of water absorption tower has water inlet, the export is arranged to the impurity gas, the formaldehyde aqueous solution of the bottom of water absorption tower is adopted the mouth and is passed through the raw materials feed inlet of pipe connection formaldehyde polymerization unit and methylal preparation facilities respectively.
Raw material industrial methanol is gasified into formaldehyde gas by a methanol evaporator, and then the formaldehyde gas enters a gas mixer to be mixed with oxygen; preheating the mixed gas to a reaction temperature by a preheater, and then entering an oxidation reactor for methanol oxidation reaction to obtain formaldehyde gas; and then the formaldehyde gas and other gas impurities enter a water absorption tower, the water is used for absorbing the formaldehyde gas to obtain a formaldehyde water solution, and the impurity gas is discharged from the top of the absorption tower.
And the formaldehyde polymerization device comprises a formaldehyde polymerization rectifying tower and a steam penetration device, wherein the top of the formaldehyde polymerization rectifying tower is provided with a full condenser, the tower kettle is provided with a reboiler, the reaction section of the formaldehyde polymerization rectifying tower is provided with a formaldehyde water solution feeding port, a top extraction port of the formaldehyde polymerization rectifying tower is connected with the steam penetration device, and an interception side extraction port of the steam penetration device is connected with a raw material feeding port of the polymethoxy dimethyl ether reaction rectification preparation device.
The formaldehyde solution extracted by the formaldehyde preparation device enters a formaldehyde polymerization reaction rectifying tower to carry out polymerization reaction to generate trioxymethylene, the mixture of the trioxymethylene, the formaldehyde and the water is extracted from the top of the tower in a gas phase form after being separated by the formaldehyde polymerization reaction rectifying tower, part of the liquid phase flows back, and the water which does not participate in the reaction is extracted from the bottom of the tower after being separated by the formaldehyde polymerization reaction rectifying tower. The gas phase mixture of the trioxymethylene, the formaldehyde and the water extracted from the tower top enters the steam permeation equipment for membrane separation, the water phase penetrates through the membrane and enters the permeation side of the steam permeation equipment and is extracted, and the mixed phase of the trioxymethylene, the formaldehyde and the trace water is extracted from the interception side of the steam permeation equipment.
And the methylal preparation device comprises a methylal reaction rectifying tower, the top of the methylal reaction rectifying tower is provided with a full condenser, the tower kettle is provided with a reboiler, two reactant feeding holes, namely a formaldehyde water solution feeding hole and a methanol feeding hole, are arranged on the reaction section of the methylal reaction rectifying tower, the methanol feeding holes are connected with a methanol pipeline through a methanol mixer, and the top methylal extraction port of the methylal reaction rectifying tower is connected with the raw material feeding hole of the polymethoxy dimethyl ether reaction rectifying preparation device through the methylal mixer.
The formaldehyde solution and the methanol in the formaldehyde preparation device are added into a methylal reaction rectifying tower in a formaldehyde micro-excess mode for reaction and separation, high-concentration methylal is extracted from the top of the methylal reaction rectifying tower, and water containing trace formaldehyde is extracted from the bottom of the methylal reaction rectifying tower.
The polymethoxy dimethyl ether reaction rectification preparation device is the same as the first technical scheme.
The utility model discloses a third technical scheme has increased the apparatus for producing that gets into the raw materials (gaseous phase formaldehyde and methylal) of gathering methoxy dimethyl ether reaction rectifying column, and concrete scheme is as follows:
the utility model provides a methylal and gaseous phase formaldehyde route methanol to DMMn's new process units, includes formaldehyde preparation facilities, gaseous phase formaldehyde preparation facilities, methylal preparation facilities, gathers methoxy dimethyl ether reaction rectification preparation facilities, formaldehyde preparation facilities's formaldehyde aqueous solution is adopted the mouth and is passed through the raw materials feed inlet of pipeline connection gaseous phase formaldehyde preparation facilities and methylal preparation facilities respectively, gaseous phase formaldehyde of gaseous phase formaldehyde preparation facilities is adopted the mouth and methylal of methylal preparation facilities is adopted the mouth and is passed through the raw materials feed inlet of pipeline connection poly methoxy dimethyl ether reaction rectification preparation facilities respectively.
And the gas-phase formaldehyde preparation device comprises a formaldehyde aqueous solution evaporator and a steam permeation device, wherein the formaldehyde aqueous solution evaporator is provided with a formaldehyde aqueous solution raw material feeding hole, a steam feeding hole, a gas-phase formaldehyde and water mixture extraction hole and a cooling water extraction hole, the gas-phase formaldehyde and water mixture extraction hole is connected with the feeding hole of the steam permeation device through a pipeline, a permeation side extraction hole of the steam permeation device is connected with a water extraction pipeline, and a interception side extraction hole of the steam permeation device is connected with a raw material feeding hole of the polymethoxy dimethyl ether reaction rectification preparation device through a gas-phase formaldehyde extraction pipeline.
The formaldehyde preparation device, the methylal preparation device and the polymethoxy dimethyl ether reaction rectification preparation device are the same as the second technical scheme.
The utility model has the advantages and beneficial effect:
1. the device adopts the polymethoxy dimethyl ether reaction rectifying tower, utilizes the advantages of the reaction rectifying process, adopts excessive methylal reactant, greatly improves the formaldehyde conversion rate, reduces the subsequent separation difficulty caused by the existence of formaldehyde, can timely carry reaction products away from a reaction zone by reaction rectification to prevent excessive polymerization of the polymethoxy dimethyl ether, breaks the reaction balance limitation, promotes DMM2 to continue to polymerize to generate target products DMM3-5, reduces the generation amount of DMM2, reduces the circulating stream flow of DMM2 and DMM 6-10, and effectively improves the yield and selectivity of DMM 3-5.
2. The device adopts the steam permeable membrane equipment to remove water in the light component, reduces the energy consumption of a subsequent separation azeotropic system while not introducing a third substance, greatly reduces the operation cost of removing water in a reaction system, and is a high-efficiency and environment-friendly production separation technology.
3. The utility model discloses an used flow of process units is simple, and initial stage equipment cost and later stage operating cost are low, have good application prospect.
Drawings
FIG. 1 is a schematic view of an apparatus according to example 1;
FIG. 2 is a schematic view of the apparatus of example 2;
FIG. 3 is a schematic view of the apparatus of example 3.
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.
Example 1
As shown in figure 1, a reactive distillation-steam permeation coupling device for synthesizing polymethoxy dimethyl ether comprises a polymethoxy dimethyl ether reactive distillation tower 1, a primary product refining tower 6, a secondary product refining tower 7, a steam permeation device 2, a first light component separation tower 3, a high-pressure separation tower 4 and a low-pressure separation tower 5, wherein the polymethoxy dimethyl ether reactive distillation tower is provided with a water-containing chain extension reactant reducing port and a methylal feed port, DMM 6-10 recovery feed ports and a DMM2 recovery feed port, a gas phase extraction outlet at the top of the polymethoxy dimethyl ether reactive distillation tower is connected with a gas phase feed port of the steam permeation device, a permeation side extraction outlet of the steam permeation device is connected with a water extraction pipeline, a interception side extraction outlet of the steam permeation device is connected with a full condenser, and discharge outlets of the full condenser are respectively connected with a reflux outlet at the top of the polymethoxy dimethyl ether reactive distillation tower and a feed port of the first light component separation tower through pipelines, a tower bottom extraction outlet of the first light component separation tower is connected with a DMM2 mixer feeding pipeline, a tower top extraction outlet is connected with a high-pressure separation tower feeding hole, a tower bottom extraction outlet of the high-pressure separation tower is connected with a methylal mixer feeding hole, a tower top extraction outlet is connected with a low-pressure separation tower feeding hole, a tower bottom extraction outlet of the low-pressure separation tower is connected with a methanol extraction pipeline, and a tower top extraction outlet of the low-pressure separation tower is connected with a high-pressure separation tower feeding hole; the tower kettle of the polymethoxy dimethyl ether reaction rectifying tower is connected with a feed inlet of a primary product refining tower, and a tower top extraction outlet of the primary product refining tower is connected with a DMM2 mixer feed pipeline; a tower kettle extraction outlet of the primary product refining tower is connected with a raw material feeding port of the secondary product refining tower, a tower kettle liquid phase extraction outlet of the secondary product refining tower is connected with DMM 6-10 recovery feeding ports through a pipeline, and a tower top liquid phase extraction outlet of the secondary product refining tower is connected with a target product DMM3-5 extraction pipeline.
The process flow adopting the device is as follows:
step 1, feeding a mixture of one or more than two of methylal providing product chain end capping and formaldehyde solution providing product chain growth, aqueous trioxymethylene and aqueous paraformaldehyde from a methylal mixer and a chain growth reactant feeding pipeline respectively through two liquid-phase feeding ports on a reaction section of a polymethoxy dimethyl ether reaction rectifying tower, or feeding methylal and gas-phase formaldehyde from a raw material liquid-phase feeding port and a gas-phase feeding port on the polymethoxy dimethyl ether reaction rectifying tower respectively, and reacting;
step 4, sequentially conveying the liquid phase extracted from the tower top of the polymethoxy dimethyl ether reaction rectifying tower to a first light component separating tower, a high-pressure separating tower and a low-pressure separating tower for light component separation, separating a low-polymerization-degree product DMM2 from the tower kettle of the first light component separating tower, mixing methylal extracted from the tower kettle of the high-pressure separating tower with a methylal raw material in a mixer, and then feeding the mixture into the polymethoxy dimethyl ether reaction rectifying tower for reaction, extracting a methylal-methanol azeotrope from the tower top of the high-pressure separating tower and feeding the methylal-methanol azeotrope into the low-pressure separating tower, extracting the methylal-methanol azeotrope from the tower top of the low-pressure separating tower and returning the methylal-methanol azeotrope into the high-pressure separating tower, and directly extracting methanol from a pipeline from the;
Example 2
As shown in fig. 2, a formaldehyde preparation device is added on the basis of the embodiment 1; a formaldehyde polymerization device; methylal preparation facilities.
The formaldehyde preparation device comprises a methanol evaporator 8, a gas mixer 9, a preheater 10, an oxidation reactor 11 and a water absorption tower 12. The system has the methyl alcohol import on the methyl alcohol evaporimeter, steam inlet, methyl alcohol steam outlet, the cooling water export, wherein methyl alcohol steam outlet passes through one of them import of methyl alcohol steam conveying pipe connection gas mixer, another access connection oxygen conveying pipe of gas mixer, the export of gas mixer passes through the import of gas mixture conveying pipe connection preheater, the export of preheater passes through the top raw materials import of pipe connection oxidation reactor, the bottom formaldehyde gas mixture of oxidation reactor is adopted the mouth and is connected the feed inlet at the bottom of the water absorption tower, the top of the tower system of water absorption tower has water inlet, the export is arranged to the impurity gas, the formaldehyde aqueous solution of the bottom of the water absorption tower is adopted the mouth and is passed through the raw materials feed inlet of pipe connection formaldehyde polymerization device and methylal preparation facilities respectively.
The formaldehyde polymerization device comprises a formaldehyde polymerization reaction rectifying tower 13 and a steam penetration device 14. The top of the formaldehyde polymerization rectifying tower is provided with a complete condenser, the tower kettle is provided with a reboiler, the reaction section of the formaldehyde polymerization rectifying tower is provided with a formaldehyde water solution feed inlet, a top extraction outlet of the formaldehyde polymerization rectifying tower is connected with a steam permeation device, and an interception side extraction outlet of the steam permeation device is connected with a raw material feed inlet of the polymethoxy dimethyl ether reaction rectifying tower of the polymethoxy dimethyl ether reaction rectifying preparation device.
The methylal preparation device comprises a methylal reaction rectifying tower 15. The top of the methylal reaction rectifying tower is provided with a complete condenser, the tower kettle is provided with a reboiler, two reactant feed inlets are arranged on a reaction section of the methylal reaction rectifying tower and are respectively a formaldehyde water solution feed inlet and a methanol feed inlet, the methanol feed inlet is connected with a methanol pipeline through a methanol mixer, and a top methylal extraction outlet of the methylal reaction rectifying tower is connected with a raw material feed inlet of the polymethoxy dimethyl ether reaction rectifying tower of the polymethoxy dimethyl ether reaction rectifying preparation device through the methylal mixer.
Example 3
As shown in fig. 3, a formaldehyde preparation device is added on the basis of the embodiment 1; a gas phase formaldehyde preparation device; methylal preparation facilities.
The formaldehyde preparation apparatus and the methylal preparation apparatus were the same as in example 2.
The gas-phase formaldehyde preparation device comprises a formaldehyde aqueous solution evaporator 16 and a steam penetration device 17. The formaldehyde aqueous solution evaporator is provided with a formaldehyde aqueous solution raw material feeding port, a steam feeding port, a gas-phase formaldehyde and water mixture extraction port and a cooling water extraction port, wherein the gas-phase formaldehyde and water mixture extraction port is connected with a feeding port of a steam permeation device through a pipeline, a permeation side extraction port of the steam permeation device is connected with a water extraction pipeline, and a interception side extraction port of the steam permeation device is connected with a raw material feeding port of the polymethoxy dimethyl ether reaction rectification preparation device through a gas-phase formaldehyde extraction pipeline.
The reactive distillation-steam permeation coupling process for polyoxymethylene dimethyl ether synthesis provided by the present invention has been described in the preferred embodiments, and it is obvious to those skilled in the art that the apparatus and process flow described herein can be modified or properly changed and combined without departing from the contents, spirit and scope of the present invention to implement the present invention. 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 (10)
1. A reactive distillation-steam permeation coupling device for synthesizing polymethoxy dimethyl ether is characterized in that: the device comprises a polymethoxy dimethyl ether reaction rectifying tower, a primary product refining tower, a secondary product refining tower, a steam permeation device, a first light component separating tower, a high-pressure separating tower and a low-pressure separating tower, wherein a raw material feeding port, DMM 6-10 recovery feeding ports and DMM2 recovery feeding ports are arranged on the polymethoxy dimethyl ether reaction rectifying tower, a gas phase extraction outlet at the top of the polymethoxy dimethyl ether reaction rectifying tower is connected with a gas phase feeding port of the steam permeation device, a permeation side extraction outlet of the steam permeation device is connected with a water extraction pipeline, an interception side extraction outlet of the steam permeation device is connected with a feeding port of a full condenser, a discharge port of the full condenser is respectively connected with a reflux port at the top of the polymethoxy dimethyl ether reaction rectifying tower and a feeding port of the first light component separating tower through pipelines, a kettle extraction outlet of the first light component separating tower is connected with a DMM2 mixer feeding pipeline, a tower top extraction outlet is connected with the high-, the tower bottom extraction outlet of the high-pressure separation tower is connected with a feeding hole of a methylal mixer, the tower top extraction outlet is connected with a feeding hole of a low-pressure separation tower, the tower bottom extraction outlet of the low-pressure separation tower is connected with a methanol extraction pipeline, and the tower top extraction outlet of the low-pressure separation tower is connected with a feeding hole of the high-pressure separation tower; the tower kettle of the polymethoxy dimethyl ether reaction rectifying tower is connected with a feed inlet of a primary product refining tower, and a tower top extraction outlet of the primary product refining tower is connected with a DMM2 mixer feed pipeline; a tower kettle extraction outlet of the primary product refining tower is connected with a raw material feeding port of the secondary product refining tower, a tower kettle liquid phase extraction outlet of the secondary product refining tower is connected with DMM 6-10 recovery feeding ports through a pipeline, and a tower top liquid phase extraction outlet of the secondary product refining tower is connected with a target product DMM3-5 extraction pipeline.
2. The reactive distillation-steam permeation coupling device for polyoxymethylene dimethyl ether synthesis according to claim 1, wherein: the device is characterized by further comprising a formaldehyde preparation device, a formaldehyde polymerization device and a methylal preparation device, wherein the formaldehyde extraction port of the formaldehyde preparation device is respectively connected with the raw material feeding ports of the formaldehyde polymerization device and the methylal preparation device through pipelines, and the main product extraction ports of the formaldehyde polymerization device and the methylal preparation device are respectively connected with the raw material feeding port of the polymethoxy dimethyl ether reaction rectifying tower through pipelines.
3. The reactive distillation-steam permeation coupling device for polyoxymethylene dimethyl ether synthesis according to claim 1, wherein: the formaldehyde solution extraction port of the formaldehyde preparation device is respectively connected with the raw material feeding ports of the gas-phase formaldehyde preparation device and the methylal preparation device through pipelines, and the gas-phase formaldehyde extraction port of the gas-phase formaldehyde preparation device and the methylal extraction port of the methylal preparation device are respectively connected with the raw material feeding ports of the polymethoxy dimethyl ether reaction rectifying tower through pipelines.
4. The reactive distillation-steam permeation coupling device for polyoxymethylene dimethyl ether synthesis according to claim 2 or 3, wherein: the formaldehyde preparation device comprises a methanol evaporator, a gas mixer, a preheater, an oxidation reactor and a water absorption tower which are connected in sequence, wherein the methanol evaporator is provided with a methanol inlet, a steam inlet, a methanol steam outlet and a cooling water outlet, wherein the methyl alcohol steam outlet passes through one of them import of methyl alcohol steam delivery pipe connection gas mixer, another access connection oxygen delivery pipe of gas mixer, the import of gas mixture delivery pipe connection pre-heater is passed through in the export of gas mixer, the top raw materials import of pipe connection oxidation reactor is passed through in the export of pre-heater, the bottom formaldehyde gas mixture of oxidation reactor is adopted the mouth and is connected the feed inlet at the bottom of water absorption tower, the top of the tower system of water absorption tower has water inlet, the export is arranged to the impurity gas, the bottom formaldehyde aqueous solution of water absorption tower is adopted the mouth and is passed through the raw materials feed inlet of pipe connection formaldehyde polymerization plant or gaseous phase formaldehyde preparation facilities and methylal preparation facilities respectively.
5. The reactive distillation-steam permeation coupling device for polyoxymethylene dimethyl ether synthesis according to claim 2 or 3, wherein: the methylal preparation device comprises a methylal reaction rectifying tower, wherein the top of the methylal reaction rectifying tower is provided with a full condenser, the tower kettle is provided with a reboiler, two reactant feed inlets, namely a formaldehyde water solution feed inlet and a methanol feed inlet, are arranged on a reaction section of the methylal reaction rectifying tower, the methanol feed inlets are connected with a methanol pipeline through a methanol mixer, and a top methylal extraction outlet of the methylal reaction rectifying tower is connected with a raw material feed inlet of the polymethoxy dimethyl ether reaction rectifying tower through the methylal mixer.
6. The reactive distillation-steam permeation coupling device for polyoxymethylene dimethyl ether synthesis according to claim 2, wherein: the formaldehyde polymerization device comprises a formaldehyde polymerization rectifying tower and steam permeation equipment, wherein the top of the formaldehyde polymerization rectifying tower is provided with a full condenser, the tower kettle is provided with a reboiler, the reaction section of the formaldehyde polymerization rectifying tower is provided with a formaldehyde water solution feeding port, a top extraction port of the formaldehyde polymerization rectifying tower is connected with the steam permeation equipment, and an interception side extraction port of the steam permeation equipment is connected with a raw material feeding port of the polymethoxy dimethyl ether reaction rectifying tower.
7. The reactive distillation-steam permeation coupling device for polyoxymethylene dimethyl ether synthesis according to claim 3, wherein: the gas-phase formaldehyde preparation device comprises a formaldehyde aqueous solution evaporator and a steam permeation device, wherein the formaldehyde aqueous solution evaporator is provided with a formaldehyde aqueous solution raw material feeding port, a steam feeding port, a gas-phase formaldehyde and water mixture extraction port and a cooling water extraction port, the gas-phase formaldehyde and water mixture extraction port is connected with the feeding port of the steam permeation device through a pipeline, a permeation side extraction port of the steam permeation device is connected with a water extraction pipeline, and a interception side extraction port of the steam permeation device is connected with a raw material feeding port of a polymethoxy dimethyl ether reaction rectifying tower through a gas-phase formaldehyde extraction pipeline.
8. The reactive distillation-steam permeation coupling device for polyoxymethylene dimethyl ether synthesis according to claim 1, wherein: the first light component separation tower, the high-pressure separation tower, the low-pressure separation tower, the primary product refining tower and the secondary product refining tower are all provided with a total condenser at the top of the tower and a reboiler at the bottom of the tower.
9. The reactive distillation-steam permeation coupling device for polyoxymethylene dimethyl ether synthesis according to claim 1, wherein: the polymethoxy dimethyl ether reaction rectifying tower consists of a rectifying section, a reaction section and a stripping section, or the reaction section and the rectifying section; the internal parts of the rectifying section and the stripping section are fillers or trays; the reaction section is filled with solid acid catalyst, and the tower internals are catalytic filler type or catalytic tower plate type.
10. The reactive distillation-steam permeation coupling device for polyoxymethylene dimethyl ether synthesis according to claim 1, wherein: the first-stage product refining tower, the second-stage product refining tower, the first light component separation tower, the high-pressure separation tower and the low-pressure separation tower are filled with materials or trays.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110156575A (en) * | 2019-04-17 | 2019-08-23 | 天津大学 | Reactive distillation-Steam soak coupling technique for polymethoxy dimethyl ether synthesis |
| CN117599690A (en) * | 2024-01-23 | 2024-02-27 | 中建安装集团有限公司 | Device and method for producing methyl ethyl carbonate and diethyl carbonate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110156575A (en) * | 2019-04-17 | 2019-08-23 | 天津大学 | Reactive distillation-Steam soak coupling technique for polymethoxy dimethyl ether synthesis |
| CN110156575B (en) * | 2019-04-17 | 2023-06-06 | 天津大学 | Reactive distillation-vapor permeation coupling process for polymethoxy dimethyl ether synthesis |
| CN117599690A (en) * | 2024-01-23 | 2024-02-27 | 中建安装集团有限公司 | Device and method for producing methyl ethyl carbonate and diethyl carbonate |
| CN117599690B (en) * | 2024-01-23 | 2024-05-14 | 中建安装集团有限公司 | Device and method for producing methyl ethyl carbonate and diethyl carbonate |
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