CN210229171U - Reaction rectification process unit for synthesizing DMMn from methanol and high-concentration formaldehyde - Google Patents

Reaction rectification process unit for synthesizing DMMn from methanol and high-concentration formaldehyde Download PDF

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CN210229171U
CN210229171U CN201920520495.9U CN201920520495U CN210229171U CN 210229171 U CN210229171 U CN 210229171U CN 201920520495 U CN201920520495 U CN 201920520495U CN 210229171 U CN210229171 U CN 210229171U
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tower
formaldehyde
dimethyl ether
pipeline
gas
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Xin Gao
高鑫
Ying Meng
孟莹
Zhenwei Han
韩振为
Hong Li
李洪
Xingang Li
李鑫钢
Haifeng Cong
从海峰
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Tianjin University
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Tianjin University
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Abstract

The utility model discloses a reaction rectification process device for synthesizing DMMn from methanol and high-concentration formaldehyde, which comprises a polymethoxy dimethyl ether reaction rectification tower, wherein a raw material feed inlet of a primary product refining tower is connected with a bottom liquid phase extraction outlet of the polymethoxy dimethyl ether reaction rectification tower through a pipeline; the raw material feeding port of the secondary product refining tower is connected with the tower bottom liquid phase extraction port of the primary product refining tower through a pipeline, the tower bottom liquid phase extraction port of the secondary product refining tower is connected with the circulating material feeding port through a pipeline, and the tower top liquid phase extraction port of the secondary product refining tower is connected with a target product extraction pipeline. The utility model discloses full play gathers methoxy dimethyl ether reaction rectifying column's advantage, gathers methoxy dimethyl ether reaction rectifying column top of the tower component and relies on vapor permeation equipment to get rid of moisture, eliminates the azeotropic composition in the system, has both saved the equipment investment, has reduced subsequent operating cost again, greatly reduced DMM3 ~ 5's manufacturing cost, annual economic benefits improves greatly.

Description

Reaction rectification process unit for synthesizing DMMn from methanol and high-concentration formaldehyde
Technical Field
The utility model belongs to the technical field of chemical production equipment, mainly relate to methanol and the synthetic DMMn's of high concentration formaldehyde reaction rectification process units under the acid condition.
Background
The polymethoxy dimethyl ether is a low molecular weight acetal polymer with methoxyl as a main chain, and the structural formula of the polymethoxy dimethyl ether is as follows: CH (CH)3O(CH2O)nCH3Abbreviated DMMn (or PODEn). When n is 3-8 (especially 3-5), the material has high cetane number and oxygen content, no sulfur element exists in the material, and the diesel oil oxygenating agent is a diesel oil oxygenating agent with excellent performance, can greatly reduce the emission of carbon monoxide and nitrogen oxides in the tail gas of diesel oil vehicles, and does not generate sulfides. Meanwhile, the addition of the substance can improve the combustion performance of the diesel without modifying a vehicle engine, and has high popularization value.
The water-containing process using methanol as raw material in the polymethoxy dimethyl ether synthesis process is widely concerned and researched due to the fact that the raw material price is low, and the economical efficiency of products can be improved. The process using methanol as reactant at present comprises the following steps: the patent CN105601479A proposes that an industrial grade methanol and formaldehyde aqueous solution are used as raw materials to react in an expansion bed reactor to obtain polymethoxy dimethyl ether, and DMM 3-8 in the reaction product accounts for only 41% at most; patent CN103420812A proposes that under the condition that a molecular sieve with an RUT topological structure is used as a catalyst, methanol and formaldehyde react to prepare polymethoxy dimethyl ether, and DMM 3-8 in the product after the reaction only accounts for about 30%. The processes are all carried out in a polymerization reactor, reactants are limited by chemical equilibrium and cannot reach higher conversion rate, most of reaction products are DMM2, the selectivity and yield of target products DMM3-5 are lower, the amount of circulating materials in the process is large, and in the subsequent separation process, due to the fact that water is contained, azeotrope in the system is more, the separation difficulty is large, and the energy consumption is high. These process defects can make such process technology economically unattractive and result in poor product competitiveness.
SUMMERY OF THE UTILITY MODEL
To the problem and the defect that above-mentioned exists, the utility model aims at providing a methyl alcohol and high concentration formaldehyde synthetic DMMn's reaction rectification process units, the utility model has the advantages of process units are simple, the equipment investment is lower, convenient operation, the energy consumption is lower.
The technical scheme of the utility model as follows:
the utility model discloses a first technical scheme as follows:
a reaction rectification process unit for synthesizing DMMn from methanol and high-concentration formaldehyde comprises: a polymethoxy dimethyl ether reaction rectifying tower, two product refining towers, a vapor permeation device, related feeding pipelines and pipelines for connecting the devices. The polymethoxy dimethyl ether reaction rectifying tower is provided with a tower kettle reboiler, and a tower top complete condenser is arranged behind the steam permeation equipment. The polymethoxy dimethyl ether reaction rectifying tower is characterized in that a raw material feeding port and a circulating material feeding port are arranged on a reaction section of the polymethoxy dimethyl ether reaction rectifying tower, a liquid phase extraction port is arranged behind a tower kettle reboiler, a gas phase extraction port is arranged at the top of the tower, and the raw material feeding port is connected with a raw material feeding pipeline. The first-stage product refining tower and the second-stage product refining tower are both provided with a tower kettle reboiler and a tower top complete condenser, a tower body is provided with a raw material feed inlet, a tower kettle is provided with a liquid phase extraction outlet, and a tower top is provided with a liquid phase extraction outlet, wherein the raw material feed inlet of the first-stage product refining tower is connected with the bottom liquid phase extraction outlet of the polymethoxy dimethyl ether reaction rectifying tower through a pipeline; the raw material feeding port of the secondary product refining tower is connected with the liquid phase extraction port of the primary product refining tower through a pipeline, the liquid phase extraction port of the tower kettle is connected with the circulating material feeding port through a pipeline, and the liquid phase extraction port of the tower top is connected with the target product extraction pipeline. The vapor permeation equipment is provided with a gas phase feed inlet, a permeation 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 through a pipeline, the permeation side extraction outlet is connected with a water extraction pipeline, the interception side extraction outlet is connected with a feed inlet of a top complete condenser, and a discharge outlet of the top complete condenser is connected with a reflux port at the top of the polymethoxy dimethyl ether reaction rectifying tower and an extraction pipeline at the top of the tower.
The polymethoxy dimethyl ether reaction rectifying tower consists of a rectifying section, a reaction section and a stripping section; or consists of a reaction section and a stripping section; or consists of a reaction section and a rectification section; the rectifying section is filled with solid acidic catalyst, preferably acidic resin or acidic molecular sieve catalyst, and the stripping section is filled with catalytic filler or catalytic tower tray.
Two liquid phase reactant feed inlets and a circulating material feed inlet are arranged on the reaction section of the polymethoxy dimethyl ether reaction rectifying tower; or the reaction section of the polymethoxy dimethyl ether reaction rectifying tower is provided with a liquid phase reactant feeding hole and a circulating material feeding hole, and the reaction section or the stripping section is provided with a gas phase reactant feeding hole.
The inner parts of the first-stage product refining tower and the second-stage product refining tower are fillers or trays.
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) of gathering methoxy dimethyl ether reaction rectifying column, and concrete scheme is as follows:
the utility model provides a methanol and high concentration trioxymethylene synthetic DMMn's process units, is including connecting gradually formaldehyde preparation facilities, trioxymethylene preparation facilities, poly methoxy dimethyl ether reaction rectification preparation facilities, and the raw materials feed inlet of trioxymethylene preparation facilities is connected through the pipeline to formaldehyde aqueous solution extraction outlet of formaldehyde preparation facilities, and the raw materials feed inlet of poly methoxy dimethyl ether reaction rectification preparation facilities is connected through the pipeline to the product trioxymethylene extraction outlet of trioxymethylene preparation facilities.
The raw material methanol is subjected to oxidation reaction, absorption and other processes in a formaldehyde preparation device to obtain a formaldehyde water solution, and the product is subjected to a reaction-separation process in a trioxymethylene preparation device to obtain a mixture of trioxymethylene, formaldehyde and trace water. The mixture of excessive methanol, 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; and obtaining a water-containing light component at the tower top, and then obtaining a mixture of DMM2, methylal and methanol through a membrane separation and water removal process, returning the mixture to the polymethoxy dimethyl ether reaction rectifying tower.
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 export of methyl alcohol steam 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 export of gas mixer passes through the import of gas mixture delivery pipe connection pre-heater, the export of pre-heater passes through the top raw materials import of pipe connection oxidation reactor, the bottom formaldehyde gas mixture of oxidation reactor is adopted the export and is connected the feed inlet at the bottom of water absorption tower, the top system of water absorption tower has the water import, the export is arranged to the impurity gas, the bottom formaldehyde aqueous solution of water absorption tower is adopted the export and is passed through the raw materials feed inlet of pipe connection trioxymethylene preparation facilities.
Raw material industrial methanol is gasified into methanol gas by a methanol evaporator, and then the methanol 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 trioxymethylene preparation device comprises a formaldehyde polymerization reaction rectifying tower and a steam permeation device, wherein a full condenser is arranged at the top of the formaldehyde polymerization reaction rectifying tower, a reboiler is arranged at the bottom of the formaldehyde polymerization reaction rectifying tower, a formaldehyde water solution feeding port is arranged at the reaction section of the formaldehyde polymerization reaction rectifying tower, trioxymethylene, formaldehyde and water azeotrope extraction ports at the top of the formaldehyde polymerization reaction rectifying tower are connected with the steam permeation device, and an extraction port at the interception side of the steam permeation device is connected with a raw material feeding port of the polymethoxy dimethyl ether reaction rectifying tower.
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.
Moreover, the reaction section of the formaldehyde polymerization rectifying tower adopts reaction separation tower internals, and the rectifying section and the stripping section adopt packing or tower trays; the pervaporation membrane in the steam permeation equipment is a permeable molecular sieve membrane. The height of the catalytic filler is 2-6 m, the catalytic trays are 8-30, the rectifying section and the stripping section adopt fillers or trays, the filler of the rectifying section is 1-5 m, the trays are 4-25, the filler of the stripping section is 0.5-3 m, and the trays are 2-15.
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) of gathering methoxy dimethyl ether reaction rectifying column, and concrete scheme is as follows:
the utility model provides a methanol and gaseous phase formaldehyde system DMMn's process units, is including the formaldehyde preparation facilities, gaseous phase formaldehyde preparation facilities, the poly methoxy dimethyl ether reaction rectification preparation facilities that connect gradually, and the product formaldehyde aqueous solution of formaldehyde preparation facilities is adopted the export and is passed through the raw materials import of pipeline connection gaseous phase formaldehyde preparation facilities, and the product gaseous phase formaldehyde of gaseous phase formaldehyde preparation facilities is adopted the export and is passed through the raw materials feed inlet of pipeline connection poly methoxy dimethyl ether reaction rectification preparation facilities.
The formaldehyde preparation device and the polymethoxy dimethyl ether reaction rectification preparation device are the same as the second technical scheme.
And the gas-phase formaldehyde preparation device comprises a formaldehyde water solution evaporator and a steam permeation device which are sequentially connected, wherein the formaldehyde water solution evaporator is provided with a formaldehyde water 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 the polymethoxy dimethyl ether reaction rectifying tower through a gas-phase formaldehyde extraction pipeline.
Part of formaldehyde aqueous solution generated by an absorption tower in the formaldehyde preparation device enters a gas-phase formaldehyde preparation device, is changed into a gas phase through an evaporator, and then enters a steam permeation device to remove water vapor in the mixed gas phase, so that gas-phase formaldehyde is obtained.
The utility model has the advantages and beneficial effect:
1. the utility model discloses a methyl alcohol and synthetic DMMn's of high concentration formaldehyde reaction rectification process units, its advantage lies in selecting for use methyl alcohol and have the water chain to increase the reactant for the reaction raw materials, the low price has higher market competition, gather methoxy dimethyl ether reaction rectification tower top of the tower component and rely on vapor permeation equipment to get rid of moisture, eliminate the azeotropic composition in the system, the equipment investment has both been saved, subsequent operating expenses has been reduced again, greatly reduced DMM3 ~ 5's manufacturing cost, annual economic benefits improves greatly.
2. The process device of the utility model takes industrial methanol as a single raw material, and the raw material has low price. The device gives full play to the advantages of the reactive distillation tower and the steam permeation equipment, breaks the restriction of reaction balance, prevents the reaction from going to the direction of larger polymerization degree, and improves the reaction conversion rate of each section and the yield and selectivity of the target product DMM 3-5.
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 device provided by the present invention is further described with reference to the accompanying drawings.
Example 1
As shown in fig. 1, a reactive distillation process device for synthesizing DMMn from methanol and high-concentration formaldehyde comprises: a polymethoxy dimethyl ether reaction rectifying tower 1, two product refining towers, a vapor permeation device 2, related feeding pipelines and pipelines for connecting the devices. The polymethoxy dimethyl ether reaction rectifying tower is provided with a tower kettle reboiler 6, and a tower top complete condenser 5 is arranged behind the steam penetration equipment. The polymethoxy dimethyl ether reaction rectifying tower is characterized in that a raw material feeding port and a circulating material feeding port are arranged on a reaction section of the polymethoxy dimethyl ether reaction rectifying tower, a liquid phase extraction port is arranged behind a tower kettle reboiler, a gas phase extraction port is arranged at the top of the tower, and the raw material feeding port is connected with a raw material feeding pipeline. The primary product refining tower 3 and the secondary product refining tower 4 are both provided with a tower kettle reboiler and a tower top complete condenser, a tower body is provided with a raw material feed inlet, a tower kettle is provided with a liquid phase extraction outlet, and a tower top is provided with a liquid phase extraction outlet, 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; the raw material feeding port of the secondary product refining tower is connected with the liquid phase extraction port of the primary product refining tower through a pipeline, the liquid phase extraction port of the tower kettle is connected with the circulating material feeding port through a pipeline, and the liquid phase extraction port of the tower top is connected with the target product extraction pipeline. The vapor permeation equipment is provided with a gas phase feed inlet, a permeation 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 through a pipeline, the permeation side extraction outlet is connected with a water extraction pipeline, the interception side extraction outlet is connected with a feed inlet of a top complete condenser, and a discharge outlet of the top complete condenser is connected with a reflux port at the top of the polymethoxy dimethyl ether reaction rectifying tower and an extraction pipeline at the top of the tower.
The process flow adopting the device is as follows:
step 1, respectively feeding the mixture of methanol, trioxymethylene, paraformaldehyde and formaldehyde aqueous solution or substances into a polymethoxy dimethyl ether reaction rectifying tower from two raw material liquid phase feed inlets on the polymethoxy dimethyl ether reaction rectifying tower, or feeding the methanol and gas-phase formaldehyde into the polymethoxy dimethyl ether reaction rectifying tower from a raw material liquid phase feed inlet and a gas-phase feed inlet on the polymethoxy dimethyl ether reaction rectifying tower for reaction;
step 2, separating a reaction zone from a product DMM3-10 (containing trace DMM2) with higher polymerization degree generated by the reaction through a stripping section of a polymethoxy dimethyl ether reaction rectifying tower, extracting from a liquid phase extraction outlet of the bottom of the polymethoxy dimethyl ether reaction rectifying tower, separating the methylal generated by the reaction, the product DMM2 with low polymerization degree, methanol which is not completely reacted and water in the system from a reaction zone of the polymethoxy dimethyl ether reaction rectifying tower through a rectifying section of the polymethoxy dimethyl ether reaction rectifying tower, and extracting from a gas phase extraction outlet at the top of the polymethoxy dimethyl ether reaction rectifying tower;
step 3, extracting steam extracted from the top of the polymethoxy dimethyl ether reaction rectifying tower from a gas phase outlet at the top of the tower, conveying the steam to steam permeation equipment, separating water in the steam from other light components through a pervaporation membrane to obtain penetrating fluid and dehydrated light components, extracting the penetrating fluid from a penetrating fluid extraction outlet, extracting the dehydrated light components from a trapped fluid extraction outlet, condensing the condensed penetrating fluid by a full condenser, returning part of the condensed penetrating fluid to the polymethoxy dimethyl ether reaction rectifying tower from the top of the tower, and mixing part of the condensed penetrating fluid with reactant methanol and returning the mixed gas to a reaction section of the polymethoxy dimethyl ether reaction rectifying tower;
step 4, conveying the liquid phase extracted from the tower bottom of the polymethoxy dimethyl ether reaction rectifying tower to a primary product refining tower and a secondary product refining tower for product refining, separating DMM2 from the tower top of the primary product refining tower to mix with reactant methanol, returning to the reaction section of the polymethoxy dimethyl ether reaction rectifying tower, separating a high-purity target product DMM3-5 from the tower top of the secondary product refining tower, and extracting from a tower top liquid phase extraction pipeline; and (3) extracting a product DMM 6-10 with an excessively high polymerization degree separated from the tower kettle from a liquid phase output pipeline of the tower kettle, and conveying the product DMM 6-10 to a circulating material feeding hole of a polymethoxy dimethyl ether reaction rectifying tower.
Example 2
As shown in fig. 2, a formaldehyde preparation apparatus and a trioxymethylene preparation apparatus were added to example 1.
The formaldehyde preparation device comprises a methanol evaporator 7, a gas mixer 8, a preheater 9, an oxidation reactor 10 and a water absorption tower 11. 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 delivery pipe connection gas mixer, another access connection oxygen delivery pipe of gas mixer, the export of gas mixer passes through the import of gas mixture delivery pipe connection preheater, the export of preheater passes through the top raw materials import of pipe connection oxidation reactor, the bottom feed inlet at the bottom of oxidation reactor's bottom formaldehyde gas mixture extraction mouth connection 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 extraction mouth of water absorption tower passes through the raw materials feed inlet of pipe connection trioxymethylene preparation facilities.
The trioxymethylene preparation device comprises a formaldehyde polymerization reaction rectifying tower 12 and a steam penetration device 13. 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, the collecting outlet of trioxymethylene, formaldehyde and water azeotrope at the top of the formaldehyde polymerization rectifying tower is connected with a steam penetration device, and the collecting outlet at the interception side of the steam penetration device is connected with a raw material feed inlet of the polymethoxy dimethyl ether reaction rectifying tower.
Example 3
As shown in fig. 3, a formaldehyde preparation device is added on the basis of the embodiment 1; gaseous phase formaldehyde preparation facilities.
Wherein the formaldehyde preparation apparatus was the same as in example 2.
The gas-phase formaldehyde preparation device comprises a formaldehyde aqueous solution evaporator 14 and a steam penetration device 15. 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 the steam permeation equipment through a pipeline, a permeation side extraction port of the steam permeation equipment is connected with a water extraction pipeline, and a 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 through a gas-phase formaldehyde extraction pipeline.
The utility model provides a reaction rectification process units of methyl alcohol and high concentration formaldehyde synthetic DMMn has been 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 to 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 (10)

1. A reaction rectification process unit for synthesizing DMMn from methanol and high-concentration formaldehyde is characterized in that: the device comprises a polymethoxy dimethyl ether reaction rectifying tower, two product refining towers and a steam permeation device, wherein the polymethoxy dimethyl ether reaction rectifying tower is provided with a tower kettle reboiler, a tower top complete condenser is arranged behind the steam permeation device, two raw material feed inlets and a circulating material feed inlet are arranged on a reaction section of the polymethoxy dimethyl ether reaction rectifying tower, a liquid phase extraction outlet is arranged behind the tower kettle reboiler, a gas phase extraction outlet is arranged at the tower top, and the two raw material feed inlets are respectively a methanol feed inlet and a chain growth reactant feed inlet; a raw material feeding hole of a primary product refining tower is connected with a liquid phase extraction outlet at the bottom of the polymethoxy dimethyl ether reaction rectifying tower through a pipeline; the raw material feeding port of the secondary product refining tower is connected with the tower bottom liquid phase extraction port of the primary product refining tower through a pipeline, the tower bottom liquid phase extraction port of the secondary product refining tower is connected with the circulating material feeding port through a pipeline, the tower top liquid phase extraction port of the secondary product refining tower is connected with the target product extraction pipeline, the vapor permeation device is provided with a vapor phase feeding port, a permeation side extraction port and an interception side extraction port, the gas phase feed inlet is connected with a gas phase extraction outlet at the top of the polymethoxy dimethyl ether reaction rectifying tower through a pipeline, a permeation side extraction outlet is connected with a water extraction pipeline, a interception side extraction outlet is connected with a feed inlet of a full condenser at the top of the tower, a discharge outlet of the full condenser at the top of the tower is connected with a reflux inlet at the top of the polymethoxy dimethyl ether reaction rectifying tower and a top extraction pipeline, the extraction pipeline at the top of the tower is connected with a methanol mixer, and the methanol mixer is connected with a methanol feed inlet of the polymethoxy dimethyl ether reaction rectifying tower.
2. The process arrangement of claim 1, wherein: the device is characterized by further comprising a formaldehyde preparation device and a trioxymethylene preparation device, wherein a formaldehyde water solution extraction port of the formaldehyde preparation device is connected with a raw material feeding port of the trioxymethylene preparation device through a pipeline, and a trioxymethylene extraction port of a product of the trioxymethylene preparation device is connected with a raw material feeding port of the polymethoxy dimethyl ether reaction rectifying tower through a pipeline.
3. The process arrangement of claim 1, wherein: the device is characterized by further comprising a formaldehyde preparation device and a gas-phase formaldehyde preparation device, wherein a product formaldehyde water solution extraction port of the formaldehyde preparation device is connected with a raw material inlet of the gas-phase formaldehyde preparation device through a pipeline, and a product gas-phase formaldehyde extraction port of the gas-phase formaldehyde preparation device is connected with a raw material feeding port of the polymethoxy dimethyl ether reaction rectifying tower through a pipeline.
4. A process unit according to claim 2 or 3, characterized in that: 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 export of gas mixer passes through the import of gas mixture delivery pipe connection pre-heater, the export of pre-heater 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 water absorption tower, the top system of water absorption tower has the water import, the export is arranged to the impurity gas, the bottom formaldehyde aqueous solution of water absorption tower is adopted the export and is passed through the raw materials feed inlet of pipe connection trioxymethylene preparation facilities or gaseous phase formaldehyde preparation facilities.
5. The process arrangement of claim 2, wherein: the trioxymethylene preparation device comprises a formaldehyde polymerization reaction rectifying tower and a steam permeation device, wherein a full condenser is arranged at the top of the formaldehyde polymerization reaction rectifying tower, a reboiler is arranged at a tower kettle, a formaldehyde water solution feeding port is arranged at a reaction section of the formaldehyde polymerization reaction rectifying tower, trioxymethylene, formaldehyde and water azeotrope collecting ports at the top of the formaldehyde polymerization reaction rectifying tower are connected with the steam permeation device, and a collecting port at the interception side of the steam permeation device is connected with a raw material feeding port of the polymethoxy dimethyl ether reaction rectifying tower.
6. A process unit according to claim 3, characterized in that: the gas-phase formaldehyde preparation device comprises a formaldehyde aqueous solution evaporator and a steam permeation device which are sequentially connected, 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, the permeation side extraction port of the steam permeation device is connected with a water extraction pipeline, and the 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.
7. The process arrangement of claim 1, wherein: the polymethoxy dimethyl ether reaction rectifying tower consists of a rectifying section, a reaction section and a stripping section, wherein the internal part of the rectifying section is a filler or a tray, the reaction section is filled with an acidic solid catalyst, the internal part of the tower is a catalytic filler or a catalytic tray, and the internal part of the stripping section is a filler or a tray.
8. The process arrangement of claim 1, wherein: the inner parts of the first-stage product refining tower and the second-stage product refining tower are fillers or trays.
9. The process arrangement of claim 1, wherein: the first-stage product refining tower and the second-stage product refining tower are both provided with a total condenser at the top of the tower and a reboiler at the bottom of the tower.
10. The process arrangement of claim 1, wherein: the vapor permeation equipment is internally provided with a pervaporation membrane which is a permeable molecular sieve membrane.
CN201920520495.9U 2019-04-17 2019-04-17 Reaction rectification process unit for synthesizing DMMn from methanol and high-concentration formaldehyde Active CN210229171U (en)

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