CN203960093U - Produce the device of dimethyl oxalate - Google Patents
Produce the device of dimethyl oxalate Download PDFInfo
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- CN203960093U CN203960093U CN201420365403.1U CN201420365403U CN203960093U CN 203960093 U CN203960093 U CN 203960093U CN 201420365403 U CN201420365403 U CN 201420365403U CN 203960093 U CN203960093 U CN 203960093U
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- dimethyl oxalate
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Abstract
The utility model relates to a kind of device of producing dimethyl oxalate, mainly solves prior art and exists technical process complicated, the problem that occupation area of equipment is large.The utility model is by adopting described device to comprise reactor, water cooler, gas-liquid separator, recovery tower and storage tank, reactor inlet is connected with unstripped gas transport pipe, reactor outlet is connected with water cooler entrance, the outlet of water cooler gaseous phase materials is connected with gas-liquid separator entrance by pipeline 6, cooler liquid material outlet communicates with pipeline 6, the gas material outlet of gas-liquid separator is connected with recovery tower material inlet, the liquid material outlet of gas-liquid separator is connected with storage tank by pipeline 13, recovery tower absorption agent entrance is connected with absorption agent transport pipe 7, recovery tower material outlet is connected with outlet conduit 8, recovery tower tower reactor material outlet is connected with storage tank by pipeline 12, the technical scheme that storage tank outlet is connected with product conduit has solved this problem preferably, can be used in the industrial production of dimethyl oxalate.
Description
Technical field
The present invention relates to a kind of device of producing dimethyl oxalate, specifically, take the device of coal based synthetic gas as raw material production dimethyl oxalate.
Background technology
Dimethyl oxalate (DMO), as important intermediates, can be hydrolyzed oxalic acid processed, also can Hydrogenation ethylene glycol, in chemical industry, there is important purposes.Along with the continuous rise of oil price, adopting coal is that raw material production organic chemicals becomes current study hotspot analysis, with coal based synthetic gas synthesis of oxalate, ethylene glycol, is therefore the feasible commercialization industry route of synthetic organic chemistry product.The synthetic route of DMO mainly contains two: article one route is to generate by methyl alcohol and oxalic acid esterification, exists waste discharge amount large, the shortcoming that environmental pollution is serious; Another route is that linked reaction under palladium system or platinum group catalyst generates by CO and methyl nitrite.Because Developing Coal Chemical Industry is rapid in recent years, second route has caused concern widely as coal through the intermediate steps of synthetic gas preparing ethylene glycol, and CO is at loading type Pd/α-Al
2o
3under catalyst action, under normal pressure, generate DMO and NO with methyl nitrite linked reaction, main reaction equation is as follows:
2CO+2CH
3ONO→(COOCH
3)
2+2NO
Side reaction mainly contains CO and reacts generation NO and methylcarbonate with methyl nitrite, and methyl nitrite decomposes generates NO, methyl-formiate and methyl alcohol, and CO reacts with NO and generates N
2and CO
2, chemical equation is as follows:
CO+2CH
3ONO→2NO+C
3H
6O
3
4CH
3ONO→4NO+C
2H
4O
2+2CH
3OH
2CO+2NO→N
2+2CO
2
At present, in existing technique, generally first adopt methyl alcohol to absorb, after methyl alcohol, methylcarbonate is separated with DMO, technique through membrane sepn or variable-pressure rectification or separation of extractive distillation methyl alcohol and methylcarbonate obtains pure DMO product again, and the DMO that purifies need complete through the technique of alcohol wash tower, alcohol recovery tower and rectifying tower.
The patent US4453026A of Ube company discloses CO and nitrous acid (first or second) ester has been reacted under the katalysis of platinum group noble metal catalyst, and by the row condensation of reaction product limit, separation obtains phlegma and non-condensable gas.In the process of condensation, add a certain amount of methyl alcohol to avoid oxalic acid two (first or second) ester to sneak into non-condensable gas Crystallization Plugging pipeline.Phlegma enters elementary rectifying tower, obtains thick oxalic acid two (first or second) ester product.
In document CN101993367A, CN101993365A, CN101993369A, CN101993361A, CN101492370A and CN101381309A, the reaction product of CO and nitrous acid ester will obtain gas phase overhead product and liquid phase overhead product through gas-liquid separation, then the liquid phase distillate containing barkite is carried out to separating-purifying again and obtains thick product.
It is cooling that the open linked reaction product of document CN202643601 first passes through interchanger, and a part of dimethyl oxalate is condensed; Gas phase in interchanger and liquid phase all enter gas-liquid separator, and gas-liquid separator bottom obtains the dimethyl oxalate that can directly utilize; Remaining dimethyl oxalate goes to absorption tower to utilize methyl alcohol to absorb with uncondensable gas phase, finally absorption liquid fractionation by distillation is obtained to dimethyl oxalate.
In a word, in prior art, the separation of dimethyl oxalate need to absorb and in distillation plant, refine two unit operations in cooling apparatus, exists technical process complicated, the problem that occupation area of equipment is large.
Summary of the invention
Technical problem to be solved in the utility model is that prior art exists technical process complicated, and the problem that occupation area of equipment is large provides a kind of device of new production dimethyl oxalate.It is simple that this device has flow process, the feature that occupation area of equipment is little.
For solving the problems of the technologies described above, the technical scheme that the utility model is taked is as follows: a kind of device of producing dimethyl oxalate, is characterized in that described device comprises coupler reactor R-101, water cooler E-104, gas-liquid separator S-101, dimethyl oxalate recovery tower C-101 and dimethyl oxalate storage tank D-101, coupler reactor material inlet is connected with unstripped gas transport pipe 5, coupler reactor material outlet is connected with water cooler material inlet, the outlet of water cooler gaseous phase materials is connected with the gas-liquid mixture entrance of gas-liquid separator by the first pipeline 6, cooler liquid material outlet communicates with the first pipeline 6, the gas material outlet of gas-liquid separator is connected with dimethyl oxalate recovery tower middle part material inlet, the liquid material outlet of gas-liquid separator is connected with dimethyl oxalate storage tank by second pipe 13, dimethyl oxalate recovery tower tower top absorption agent entrance is connected with absorption agent transport pipe 7, dimethyl oxalate recovery tower tower top material outlet is connected with outlet conduit 8, dimethyl oxalate recovery tower tower reactor material outlet is connected with dimethyl oxalate storage tank by the 3rd pipeline 12, dimethyl oxalate storage tank material outlet is connected with dimethyl oxalate product conduit, in described dimethyl oxalate recovery tower, between described tower top absorption agent entrance and described middle part material inlet, be provided with filler, between described middle part material inlet and tower reactor, be provided with valve tray.
In technique scheme, preferably, in described dimethyl oxalate recovery tower, the distance L between described tower top absorption agent entrance and described middle part material inlet
1, and the distance L between described middle part material inlet and tower reactor
2between pass be L
1: L
2=0.5～5.More preferably, L
1: L
2=1～2.
In technique scheme, preferably, in described dimethyl oxalate recovery tower, the theoretical plate number between described middle part material inlet and tower reactor is 5～40.
In technique scheme, preferably, on described unstripped gas transport pipe 5, be provided with feed preheater.
In technique scheme, preferably, described dimethyl oxalate recovery tower tower reactor is provided with reboiler.
In technique scheme, preferably, described outlet conduit 8 is connected with return tank D-102 material inlet by condenser; The outlet of return tank gaseous phase materials is connected with non-condensable gas pipeline; The outlet of return tank liquid phase material is connected with reflux line 10; Reflux line 10 communicates with absorption agent transport pipe 7.
In technique scheme, preferably, described reflux line 10 also communicates with overhead extraction pipeline 11.
In technique scheme, preferably, on described second pipe 13, be provided with valve.
When production equipment of the present utility model uses, comprise the following steps:
A) gas containing CO, methyl alcohol, methyl nitrite and carrier gas nitrogen contacts and reacts with platinum group metal catalysts in coupler reactor, obtains the logistics containing dimethyl oxalate.Coupler reactor is calandria type fixed bed reactor, and reactor adopts circulating hot water to remove heat.The residence time of vapor-phase reactant in beds is no more than at most 12 seconds, and the suitable residence time is 0.2～6 second.Reaction can be carried out at relatively low temperature, and typical temperature is 50～200 ℃, and preferably temperature is 60～280 ℃.For reaction pressure, can be 0～2MPa, be preferably 0～1MPa.In gas phase initial feed, the concentration of methyl nitrite can have a greater change scope, but in order to obtain suitable speed of reaction, and the concentration of methyl nitrite is minimum must not be lower than 3% volumetric concentration, preferably 5～30% volumetric concentrations.In gas phase initial feed, the concentration of CO also can have a greater change scope, and general control is in 10～90% volumetric concentrations.The described logistics containing dimethyl oxalate, contains dimethyl oxalate (most of is liquid phase, is gas phase on a small quantity), gas phase NO, is mixing the complete gas phase CO of unreacted, gas phase methyl nitrite, gas phase N
2.
B) the described logistics containing dimethyl oxalate is cooled to 60～70 ℃ in water cooler, and some dimethyl oxalate is condensed again.
C) gas phase in water cooler and liquid phase all enter gas-liquid separator, carry out further separation, and gas-liquid separator bottom has obtained the dimethyl oxalate of purity 99 % by weight, and this part dimethyl oxalate enters dimethyl oxalate storage tank and directly utilized.By gas-liquid separator, the dimethyl oxalate of 85 % by weight can separate with gas, also has the dimethyl oxalate of 15 % by weight to be taken away by gas, enters dimethyl oxalate recovery tower.
D) gas of separating enters dimethyl oxalate recovery tower with a small amount of dimethyl oxalate, the logistics that comprises methyl alcohol enters and the described logistics counter current contact containing a small amount of dimethyl oxalate from dimethyl oxalate recovery tower tower top, tower top obtains thick methyl alcohol and non-condensable gas, tower reactor obtains dimethyl oxalate product, leads to dimethyl oxalate storage tank.Described dimethyl oxalate recovery tower, methanol feeding and be absorber portion containing part between the logistics charging of a small amount of dimethyl oxalate, employing efficient low-resistance filler, absorber portion plays rectifying section effect simultaneously, logistics charging place containing a small amount of dimethyl oxalate is partly stripping section to tower reactor, adopts valve tray.The aspect ratio of described absorption distillation section and stripping section is 0.5～5.More preferably, the aspect ratio of described absorption distillation section and stripping section is 1～2.Dimethyl oxalate recovery tower stripping section theoretical plate number is 5～40.Dimethyl oxalate recovery tower overhead gas is through condensation, and non-condensable gas partly goes subsequent disposal, and a liquid phase part is sent subsequent disposal as thick methanol product extraction, and another part mixes with methanol feeding as dimethyl oxalate recovery tower and refluxes.Dimethyl oxalate recovery tower tower top service temperature is 20～60 ℃, and working pressure is 10～100kPaG; Tower reactor service temperature is 170～200 ℃, and working pressure is 40～150kPaG.
Production equipment of the present utility model, two unit operations of absorption by coupled product in prior art in cooling apparatus and the rectifying in distillation plant focus in a dimethyl oxalate recovery tower and complete, simplified flow process, save facility investment and floor space, obtained good technique effect.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the utility model production equipment.
In Fig. 1, E-101 is feed preheater, R-101 is coupler reactor, and E-104 is water cooler, and S-101 is gas-liquid separator, D-101 is dimethyl oxalate storage tank, C-101 is dimethyl oxalate recovery tower, and D-102 is dimethyl oxalate recovery tower return tank, and E-101 is feed preheater, E-102 is dimethyl oxalate recovery tower reboiler, and E-103 is dimethyl oxalate recovery tower overhead condenser.1 is nitrogen feed pipeline, and 2 is CO feed pipe, and 3 is methanol feeding pipeline, 4 is methyl nitrite feed pipe, 5 is unstripped gas transport pipe, and 6 is the first pipeline, and 7 is absorption agent transport pipe, 8 is dimethyl oxalate recovery tower tower top outlet pipeline, 9 is non-condensable gas pipeline, and 10 is reflux line, and 11 is extraction pipeline, 12 is the 3rd pipeline, and 13 is second pipe.
In Fig. 1, described device comprises coupler reactor R-101, E-104, gas-liquid separator S-101, dimethyl oxalate recovery tower C-101 and dimethyl oxalate storage tank D-101, coupler reactor material inlet is connected with unstripped gas transport pipe 5, coupler reactor material outlet is connected with water cooler E-104 material inlet, the outlet of E-104 gaseous phase materials is connected with the gas-liquid mixture entrance of gas-liquid separator by the first pipeline 6, the outlet of E-104 liquid material communicates with the first pipeline 6, the gas material outlet of gas-liquid separator S-101 is connected with dimethyl oxalate recovery tower middle part material inlet, the liquid material outlet of gas-liquid separator S-101 is connected with dimethyl oxalate storage tank by second pipe 13, dimethyl oxalate recovery tower tower top absorption agent entrance is connected with absorption agent transport pipe 7, dimethyl oxalate recovery tower tower top material outlet is connected with outlet conduit 8, dimethyl oxalate recovery tower tower reactor material outlet is connected with dimethyl oxalate storage tank by the 3rd pipeline 12, dimethyl oxalate storage tank material outlet is connected with dimethyl oxalate product conduit, in described dimethyl oxalate recovery tower, between described tower top absorption agent entrance and described middle part material inlet, be provided with high-efficiency low-resistance filler, between described middle part material inlet and tower reactor, be provided with valve tray.
When Fig. 1 shown device is used, nitrogen, CO, methyl alcohol and methyl nitrite are respectively from nitrogen feed pipeline 1, CO feed pipe 2, methanol feeding pipeline 3 and the incoming stock letter shoot of methyl nitrite feed pipe 4 road 5, after mixing, unstripped gas enters coupler reactor R-101 after feed preheater E-101 preheating, occur after linked reaction, reaction product enters water cooler E-104.After cooling, the gas phase in water cooler and liquid phase all enter gas-liquid separator, and gas-liquid separator bottom has obtained the dimethyl oxalate of purity 99 % by weight, and this part dimethyl oxalate enters dimethyl oxalate storage tank and directly utilized.The gaseous stream at gas-liquid separator top enters dimethyl oxalate recovery tower C-101 from middle part with a small amount of dimethyl oxalate, absorption agent methyl alcohol mixes from dimethyl oxalate recovery tower top and enters with dimethyl oxalate recovery tower phegma through absorption agent transport pipe 7, overhead gas enters dimethyl oxalate recovery tower tower top outlet pipeline 8, after dimethyl oxalate recovery tower overhead condenser E-103 condensation, non-condensable gas enters aftertreatment through non-condensable gas pipeline 9, thick methanol product is through 11 extraction of extraction pipeline, tower reactor obtains dimethyl oxalate product, leads to dimethyl oxalate storage tank.Dimethyl oxalate recovery tower tower reactor is provided with reboiler E-102.On second pipe 13, be provided with valve.
Below by embodiment, the utility model is further elaborated, but these embodiment are in no case construed as limiting scope of the present utility model.
Embodiment
[embodiment]
Nitrogen, CO, methyl alcohol and methyl nitrite are respectively from nitrogen feed pipeline 1, CO feed pipe 2, methanol feeding pipeline 3 and the incoming stock letter shoot of methyl nitrite feed pipe 4 road 5, after mixing, unstripped gas enters coupler reactor R-101 after feed preheater E-101 preheating, occur after linked reaction, reaction product enters water cooler E-104.After cooling, the gas phase in water cooler E-104 and liquid phase all enter gas-liquid separator S-101, and gas-liquid separator bottom has obtained the dimethyl oxalate of purity 99 % by weight, and this part dimethyl oxalate enters dimethyl oxalate storage tank and directly utilized.The gaseous stream at gas-liquid separator top enters dimethyl oxalate recovery tower C-101 from middle part with a small amount of dimethyl oxalate, absorption agent methyl alcohol mixes from dimethyl oxalate recovery tower top and enters with dimethyl oxalate recovery tower phegma through absorption agent transport pipe 7, overhead gas enters dimethyl oxalate recovery tower tower top outlet pipeline 8, after dimethyl oxalate recovery tower overhead condenser E-103 condensation, non-condensable gas enters aftertreatment through non-condensable gas pipeline 9, thick methanol product is through 11 extraction of extraction pipeline, tower reactor obtains dimethyl oxalate product, lead to dimethyl oxalate storage tank D-101.Dimethyl oxalate recovery tower tower reactor is provided with reboiler E-102.On second pipe 13, be provided with valve.
Dimethyl oxalate recovery tower packed height is 10 meters, and hypomere theoretical plate number is 10, L
1: L
2=2; Tower top service temperature is 32 ℃, and working pressure is 40kPaG; Tower reactor service temperature is 185 ℃, and working pressure is 85kPaG, reboiler thermal load 4.0435MW.Dimethyl oxalate yield is 100%.
Wherein, reactor feed and main ducted logistics are composed as follows:
| Pipeline | 5 | 6 | 7 | 9 | 11 | 12 | 13 |
| Temperature, ℃ | 110 | 70 | 40 | 20 | 20 | 185 | 70 |
| Pressure, kPaG | 230 | 90 | 850 | 40 | 40 | 85 | 90 |
| Quality forms, % | ? | ? | ? | ? | ? | ? | ? |
| N 2 | 44.30 | 53.74 | - | 50.15 | 180ppm | - | 0.02 |
| CO | 19.08 | 10.51 | - | 11.51 | 171ppm | - | 40ppm |
| NO | 5.23 | 20.23 | - | 17.06 | 134ppm | - | - |
| CO 2 | 0 | 38ppm | - | 34ppm | 307ppm | - | - |
| Methyl nitrite | 29.74 | 7.78 | - | 11.01 | 1.03 | - | - |
| Methyl-formiate | 0 | 605ppm | - | 510ppm | 346ppm | - | 85ppm |
| Methyl alcohol | 1.65 | 2.43 | 99.78 | 9.59 | 94.4 | - | 0.072 |
| Methylcarbonate | 0 | 0.06 | 0.217 | 0.627 | 4.48 | 0.144 | 0.951 |
| Water | 0 | ? | 50ppm | - | 14.7ppm | 16ppm | - |
| Dimethyl oxalate | 0 | 5.21 | - | - | - | 99.85 | 98.92 |
Claims (9)
1. produce a device for dimethyl oxalate, it is characterized in that described device comprises coupler reactor (R-101), water cooler (E-104), gas-liquid separator (S-101), dimethyl oxalate recovery tower (C-101) and dimethyl oxalate storage tank (D-101), coupler reactor material inlet is connected with unstripped gas transport pipe (5), coupler reactor material outlet is connected with water cooler material inlet, the outlet of water cooler gaseous phase materials is connected with the gas-liquid mixture entrance of gas-liquid separator by the first pipeline (6), cooler liquid material outlet communicates with the first pipeline (6), the gas material outlet of gas-liquid separator is connected with dimethyl oxalate recovery tower middle part material inlet, the liquid material outlet of gas-liquid separator is connected with dimethyl oxalate storage tank by second pipe (13), dimethyl oxalate recovery tower tower top absorption agent entrance is connected with absorption agent transport pipe (7), dimethyl oxalate recovery tower tower top material outlet is connected with outlet conduit (8), dimethyl oxalate recovery tower tower reactor material outlet is connected with dimethyl oxalate storage tank by the 3rd pipeline (12), dimethyl oxalate storage tank material outlet is connected with dimethyl oxalate product conduit, in described dimethyl oxalate recovery tower, between described tower top absorption agent entrance and described middle part material inlet, be provided with filler, between described middle part material inlet and tower reactor, be provided with valve tray.
2. produce according to claim 1 the device of dimethyl oxalate, it is characterized in that in described dimethyl oxalate recovery tower, the distance L between described tower top absorption agent entrance and described middle part material inlet
1, and the distance L between described middle part material inlet and tower reactor
2between pass be L
1: L
2=0.5～5.
3. produce according to claim 2 the device of dimethyl oxalate, it is characterized in that L
1with L
2between pass be L
1: L
2=1～2.
4. produce according to claim 1 the device of dimethyl oxalate, it is characterized in that, in described dimethyl oxalate recovery tower, the theoretical plate number between described middle part material inlet and tower reactor is 5～40.
5. produce according to claim 1 the device of dimethyl oxalate, it is characterized in that being provided with feed preheater on described unstripped gas transport pipe (5).
6. produce according to claim 1 the device of dimethyl oxalate, it is characterized in that described dimethyl oxalate recovery tower tower reactor is provided with reboiler.
7. produce according to claim 1 the device of dimethyl oxalate, it is characterized in that described outlet conduit (8) is connected with return tank (D-102) material inlet by condenser; The outlet of return tank gaseous phase materials is connected with non-condensable gas pipeline; The outlet of return tank liquid phase material is connected with reflux line (10); Reflux line (10) communicates with absorption agent transport pipe (7).
8. produce according to claim 1 the device of dimethyl oxalate, it is characterized in that described reflux line (10) also communicates with overhead extraction pipeline (11).
9. produce according to claim 1 the device of dimethyl oxalate, it is characterized in that being provided with valve on described second pipe (13).
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|---|---|---|---|
| CN201420365403.1U CN203960093U (en) | 2014-07-03 | 2014-07-03 | Produce the device of dimethyl oxalate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420365403.1U CN203960093U (en) | 2014-07-03 | 2014-07-03 | Produce the device of dimethyl oxalate |
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| CN203960093U true CN203960093U (en) | 2014-11-26 |
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ID=51920702
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892415A (en) * | 2015-04-17 | 2015-09-09 | 中国科学院福建物质结构研究所 | Material separation apparatus during dimethyl oxalate preparation process, and process method thereof |
| CN106518675A (en) * | 2015-09-15 | 2017-03-22 | 中国石油化工股份有限公司 | Dimethyl oxalate production method with byproduct (dimethyl carbonate) |
-
2014
- 2014-07-03 CN CN201420365403.1U patent/CN203960093U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892415A (en) * | 2015-04-17 | 2015-09-09 | 中国科学院福建物质结构研究所 | Material separation apparatus during dimethyl oxalate preparation process, and process method thereof |
| CN106518675A (en) * | 2015-09-15 | 2017-03-22 | 中国石油化工股份有限公司 | Dimethyl oxalate production method with byproduct (dimethyl carbonate) |
| CN106518675B (en) * | 2015-09-15 | 2019-01-01 | 中国石油化工股份有限公司 | The method for producing dimethyl oxalate and by-product dimethyl carbonate |
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