CN103480247B - Gas-drying system in a kind of synthesis gas preparing ethylene glycol technique and drying means - Google Patents
Gas-drying system in a kind of synthesis gas preparing ethylene glycol technique and drying means Download PDFInfo
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- CN103480247B CN103480247B CN201310429057.9A CN201310429057A CN103480247B CN 103480247 B CN103480247 B CN 103480247B CN 201310429057 A CN201310429057 A CN 201310429057A CN 103480247 B CN103480247 B CN 103480247B
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Abstract
The invention discloses the gas-drying system in a kind of synthesis gas preparing ethylene glycol technique, comprise the oxidative esterification tower (1), condenser (2), drying device and the cooler (5) that are connected successively by pipeline, the bottom of described drying device is connected with heater (6) and circulator (7) in turn, described cooler (5) top has gas vent, it is connected with described circulator (7), and described drying device is connected with oxonation unit; Wherein, the pipeline between described drying device and described cooler (5) is connected with storage tank (8), alkali lye is equipped with in its inside.There is not the emptying to air in purging displacement in device regenerative process of the present invention, stopped the discharge of pernicious gas like this, protected environment; Decrease the consumption of nitrogen simultaneously, reduce production cost; Whole process control procedure is more stable in addition, is also convenient to the production operation of chemical industry personnel.
Description
Technical field
The present invention relates to a kind of gas-drying system and drying means, particularly relate to a kind of for the synthesis of the gas-drying system in gas preparing ethylene glycol technique and use described system to carry out the method for gas drying.
Background technology
Synthesis gas preparing ethylene glycol produce in esterification unit the NO circulating air, oxygen and the methyl alcohol that mainly return with carbonylation unit for raw material, by the esterification of nitrogen trioxide and methyl alcohol in oxidative esterification tower, generate methyl nitrite (MN) and water, its reaction equation is:
N
2O
3+2CH
3OH→2CH
3ONO+H
2O
After being cooled to 5 DEG C from oxidative esterification tower top outlet gas, then process through the further drying of gas, the moisture content (because the water of trace can make oxonation catalysqt deactivation) that removing is wherein micro-, the carbonylation unit of last fed downstream.
Problems existing: be illustrated in figure 1 gas-drying system of the prior art, as shown in Figure 1, comprise the oxidative esterification tower 1, condenser 2, drying device and the cooler 5 that are connected successively by pipeline, the bottom of described drying device is connected with heater 6 and circulator 7 in turn, described cooler 5 top has gas vent, it is connected with described circulator 7, and described drying device is connected with oxonation unit; Shown drying device is the adsorption tanks of two hocket absorption and reproduction operation, be respectively the first adsorption tanks 3 and the second adsorption tanks 4, described first adsorption tanks 3 are separately connected with described oxonation unit, cooler 5 with gas outlet, the top end of the second adsorption tanks 4, and bottom air intake end is separately connected with described heater with condenser 2.
The described course of work is specially: described first adsorption tanks 3 carry out absorption work, and described second adsorption tanks 4 are regenerating tank;
After cooling, enter the first adsorption tanks 3 from oxidative esterification tower 1 out reaction gas, described first adsorption tanks 3 Middle molecule sieve absorption sends into carbonylation unit after falling minor amount of water wherein, and described first adsorption tanks 3 prepare to carry out reproduction operation;
While described first adsorption tanks 3 carry out absorption work, described second adsorption tanks 4 carry out regenerative process: first introduce pure nitrogen gas and purge bed, replace; Then heater is opened, resolved the water of described second adsorption tanks 4 Middle molecule sieve absorption with hot nitrogen by circulator 7, the water deviate from is taken out of with gas, after the water condensation taken out of in gas is got off outer row by cooler 5, gas is got back in circulator 7 and is continued to utilize, close heater, adopt and lowered the temperature by described second adsorption tanks 4 through the cooled nitrogen of described cooler 5, described second adsorption tanks 4 prepare to carry out absorption work;
(2) described second adsorption tanks 4 carry out absorption work, and described first adsorption tanks 3 carry out reproduction operation for regenerating tank, and detailed process is the same;
Certainly, what first work also can be described second adsorption tanks 4, and described first adsorption tanks 3 are regenerating tank.
Adopt in the described course of work valve of the prior art or other any can control flow check to device change gas flow and always complete the change of gas flow.
After oxidative esterification tower 1 reaction out, gas (mainly: N
2, CO, methyl nitrite, NO, methyl alcohol and trace water) be cooled to about 5 DEG C through condenser, enter the drying system of gas, the first adsorption tanks 3 in this system and the second adsorption tanks 4 respectively alternate cycles carry out absorption and reproduction operation.Esterification gas sends into carbonylation unit after falling minor amount of water wherein by the first adsorption tanks 3 Middle molecule sieve absorption; Meanwhile the second adsorption tanks 4 regenerate.Pure nitrogen gas first will be introduced or pure CO gas purges bed, replaces, (object is that methyl nitrite contained in gas is blown out the second adsorption tanks 4 in emptying during regeneration, because violent decomposition reaction can be there is in methyl nitrite 140 DEG C time, and regeneration temperature is more than 180 DEG C, can be very dangerous so there is methyl nitrite gas in adsorption tanks, must replace); Then resolved the water of described second adsorption tanks 4 Middle molecule sieve absorption with hot nitrogen (now heater is opened) by circulator 7, the water removed is taken out of with gas, outer row after cooler 5 condensation; Under finally using nitrogen (now heater pass) that the temperature of described second adsorption tanks 4 is dropped to its duty again, prepare the absorption work carrying out next circulation.Just have a large amount of pernicious gases in this process and enter air, very unfavorable to environmental protection.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of for the synthesis of the gas-drying system in gas preparing ethylene glycol technique, purges the problem of replacement process to discharge of noxious gases in air when solving adsorption tanks regeneration.
Present invention also offers a kind of method using described device to carry out gas drying.
Gas-drying system in a kind of synthesis gas preparing ethylene glycol technique, comprise the oxidative esterification tower, condenser, drying device and the cooler that are connected successively by pipeline, the bottom of described drying device is connected with heater and circulator in turn, described cooler top has gas vent, it is connected with described circulator, and described drying device is connected with oxonation unit;
Wherein, the pipeline between described drying device and described cooler is connected with storage tank, alkali lye is equipped with in its inside.
Gas-drying system in synthesis gas preparing ethylene glycol technique of the present invention, wherein said alkali lye is be the alkali lye of 10% by the concentration that methyl alcohol is formulated.
Gas-drying system in synthesis gas preparing ethylene glycol technique of the present invention, wherein said storage tank is also connected with esterification unit.
Gas-drying system in synthesis gas preparing ethylene glycol technique of the present invention, wherein said described drying device is hocket absorption and two adsorption tanks of reproduction operation, is respectively the first adsorption tanks and the second adsorption tanks.
Use the gas-drying system in described synthesis gas preparing ethylene glycol technique to carry out a method for gas drying, comprise the steps:
(1) described first adsorption tanks carry out absorption work, and described second adsorption tanks are regenerating tank;
After cooling, enter the first adsorption tanks from esterification column out reaction gas, described first adsorption tanks Middle molecule sieve absorption sends into carbonylation unit after falling minor amount of water wherein, and described first adsorption tanks prepare to carry out reproduction operation;
While described first adsorption tanks carry out absorption work, described second adsorption tanks carry out regenerative process: first introduce pure nitrogen gas and purge bed, replace; Then heater is opened, the water of described second adsorption tanks Middle molecule sieve absorption is resolved by circulator hot nitrogen, the water deviate from is taken out of with gas, enter in storage tank, easily there is the methyl nitrite decomposed in alkali liquor absorption gas in storage tank, then get back to circulator after cooler cooling from described storage tank gas out and continue to utilize, close heater, adopt through the cooled nitrogen of described cooler by described second adsorption tanks cooling, described second adsorption tanks prepare to carry out absorption work;
(2) described second adsorption tanks carry out absorption work, and described first adsorption tanks are that regenerating tank carries out reproduction operation, the same step of detailed process (1); Iterative cycles like this;
Wherein, the alkali lye in described storage tank is be the alkali lye of 10% by the concentration that methyl alcohol is formulated.
Use the gas-drying system in described synthesis gas preparing ethylene glycol technique to carry out a method for gas drying, comprise the steps:
(1) described second adsorption tanks carry out absorption work, and described first adsorption tanks are regenerating tank;
After cooling, enter the second adsorption tanks from esterification column out reaction gas, described second adsorption tanks Middle molecule sieve absorption sends into carbonylation unit after falling minor amount of water wherein, and described second adsorption tanks prepare to carry out reproduction operation;
While described second adsorption tanks carry out absorption work, described first adsorption tanks carry out regenerative process: first introduce pure nitrogen gas and purge bed, replace; Then heater is opened, the water of described first adsorption tanks Middle molecule sieve absorption is resolved by circulator hot nitrogen, the water deviate from is taken out of with gas, enter in storage tank, methyl nitrite in alkali liquor absorption gas in storage tank, gets back to circulator from described storage tank gas out and continues to utilize, close heater after cooler cooling, adopt through the cooled nitrogen of described cooler by described first adsorption tanks cooling, described first adsorption tanks prepare to carry out absorption work;
(2) described first adsorption tanks carry out absorption work, and described second adsorption tanks are that regenerating tank carries out reproduction operation, the same step of detailed process (1); Iterative cycles like this;
Wherein, the alkali lye in described storage tank is be the alkali lye of 10% by the concentration that methyl alcohol is formulated.
The method of the invention and device difference from prior art are:
The method of the invention and device set up a storage tank at the port of export of drying device, groove built with methyl alcohol formulated 10% alkali lye (preparation carrying out alkali lye without water is because the ester in gas and water react), such adsorption tanks are when regenerating, first by circulator, this part gas in tank body is circulated through alkali lye storage tank, the methyl nitrite gas of about 10% is contained just by alkali liquor absorption in such gas, and do not need to carry out emptying process, which reduce the pollution to air, separately can solve methyl nitrite and decompose when high temperature.After methyl nitrite gas is completely absorbed, then continue reproduction operation below as stated above; Lye tank (vat), through absorption after a while, after concentration is down to 5%, can be sent into esterification unit, continues to use after reclaiming methyl alcohol wherein.There is not emptying to air in purging displacement in device regenerative process of the present invention, contained by having stopped so about 15% CO, the discharge of the pernicious gases such as the NO of 5% and the methyl nitrite of 10%, protects environment; The purging displacement of the technical program is due to just in inner loop simultaneously, and not emptying, so also just decreases the consumption of nitrogen, reduce production cost; Whole process control procedure is more stable in addition, is also convenient to the production operation of chemical industry personnel.
Below in conjunction with accompanying drawing, device and method of the present invention is described further.
Accompanying drawing explanation
Fig. 1 is the structural representation of the gas-drying system in prior art in synthesis gas preparing ethylene glycol technique;
Fig. 2 is the structural representation of the gas-drying system in the present invention in synthesis gas preparing ethylene glycol technique;
Fig. 3 is the gas flow figure of device of the present invention under a kind of duty;
Fig. 4 is the gas flow figure of device of the present invention under another kind of duty.
Detailed description of the invention
Embodiment 1
As shown in Figure 2, gas-drying system in a kind of synthesis gas preparing ethylene glycol technique, comprise the oxidative esterification tower 1, condenser 2, drying device and the cooler 5 that are connected successively by pipeline, the bottom of described drying device is connected with heater 6 and circulator 7 in turn, described cooler 5 top has gas vent, it is connected with described circulator 7, and described drying device is connected with oxonation unit;
Wherein, the pipeline between described drying device and described cooler 5 is connected with storage tank 8, alkali lye is equipped with in its inside.Described alkali lye is be the alkali lye of 10% by the concentration that methyl alcohol is formulated.
Described storage tank 8 is also connected with esterification unit.
Described drying device is hocket absorption and two adsorption tanks of reproduction operation, is respectively the first adsorption tanks 3 and the second adsorption tanks 4.
Embodiment 2
A kind of method using the gas-drying system in described synthesis gas preparing ethylene glycol technique to carry out gas drying, (wherein direction shown in solid arrow is the direction of motion of reaction gas as shown in Figure 3, direction shown in dotted arrow is the direction of motion of circulating nitrogen gas), comprise the steps:
1) described first adsorption tanks 3 carry out absorption work, and described second adsorption tanks 4 are regenerating tank;
After cooling, enter the first adsorption tanks 3 from oxidative esterification tower 1 out reaction gas, described first adsorption tanks 3 Middle molecule sieve absorption sends into carbonylation unit after falling minor amount of water wherein, and described first adsorption tanks 3 prepare to carry out reproduction operation;
While described first adsorption tanks 3 carry out absorption work, described second adsorption tanks 4 carry out regenerative process: first introduce pure nitrogen gas and purge bed, replace; Then heater 6 is opened, resolved the water of described second adsorption tanks 4 Middle molecule sieve absorption with hot nitrogen by circulator 7, the water deviate from is taken out of with gas, enter in storage tank 8, methyl nitrite in alkali liquor absorption gas in described storage tank 8, get back to after cooler 5 cools circulator 7 from described storage tank 8 gas out and continue to utilize, close described heater 6, adopt and lowered the temperature by described second adsorption tanks 4 through the cooled nitrogen of described cooler 5, described second adsorption tanks 4 prepare to carry out absorption work;
2) described second adsorption tanks 4 carry out absorption work, and described first adsorption tanks 3 carry out reproduction operation, the same step 1) of detailed process for regenerating tank; Iterative cycles like this;
Wherein, the alkali lye in described storage tank 8 is be the alkali lye of 10% by the concentration that methyl alcohol is formulated.
Embodiment 3
A kind of method using the gas-drying system in described synthesis gas preparing ethylene glycol technique to carry out gas drying, (wherein direction shown in solid arrow is the direction of motion of reaction gas as shown in Figure 4, direction shown in dotted arrow is the direction of motion of circulating nitrogen gas), comprise the steps:
1) described second adsorption tanks 4 carry out absorption work, and described first adsorption tanks 3 are regenerating tank;
After cooling, enter the second adsorption tanks 4 from oxidative esterification tower 1 out reaction gas, described second adsorption tanks 4 Middle molecule sieve absorption sends into carbonylation unit after falling minor amount of water wherein, and described second adsorption tanks 4 prepare to carry out reproduction operation;
While described second adsorption tanks 4 carry out absorption work, described first adsorption tanks 3 carry out regenerative process: first introduce pure nitrogen gas and purge bed, replace; Then heater 6 is opened, resolved the water of described first adsorption tanks 3 Middle molecule sieve absorption with hot nitrogen by circulator 7, the water deviate from is taken out of with gas, enter in storage tank 8, methyl nitrite in alkali liquor absorption gas in described storage tank 8, get back to after cooler 5 cools circulator 7 from described storage tank 8 gas out and continue to utilize, close described heater 6, adopt and lowered the temperature by described first adsorption tanks 3 through the cooled nitrogen of described cooler 5, described first adsorption tanks 3 prepare to carry out absorption work;
2) described first adsorption tanks 3 carry out absorption work, and described second adsorption tanks 4 carry out reproduction operation, the same step 1) of detailed process for regenerating tank; Iterative cycles like this;
Wherein, the alkali lye in described storage tank 8 is be the alkali lye of 10% by the concentration that methyl alcohol is formulated.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (6)
1. the gas-drying system in a synthesis gas preparing ethylene glycol technique, it is characterized in that: comprise the oxidative esterification tower (1), condenser (2), drying device and the cooler (5) that are connected successively by pipeline, the bottom of described drying device is connected with heater (6) and circulator (7) in turn, described cooler (5) top has gas vent, it is connected with described circulator (7), and described drying device is connected with oxonation unit;
Wherein, the pipeline between described drying device and described cooler (5) is connected with storage tank (8), alkali lye is equipped with in its inside.
2. the gas-drying system in synthesis gas preparing ethylene glycol technique according to claim 1, is characterized in that: described alkali lye is be the alkali lye of 10% by the concentration that methyl alcohol is formulated.
3. the gas-drying system in synthesis gas preparing ethylene glycol technique according to claim 2, is characterized in that: described storage tank (8) is also connected with esterification unit.
4. the gas-drying system in synthesis gas preparing ethylene glycol technique according to claim 3, it is characterized in that: described drying device is hocket absorption and two adsorption tanks of reproduction operation, is respectively the first adsorption tanks (3) and the second adsorption tanks (4).
5. use the gas-drying system in the synthesis gas preparing ethylene glycol technique described in claim 4 to carry out a method for gas drying, it is characterized in that: comprise the steps:
1) described first adsorption tanks (3) carry out absorption work, and described second adsorption tanks (4) are regenerating tank;
After cooling, enter the first adsorption tanks (3) from oxidative esterification tower (1) out reaction gas, the absorption of described first adsorption tanks (3) Middle molecule sieve sends into carbonylation unit after falling minor amount of water wherein, and the preparation of described first adsorption tanks (3) carries out reproduction operation;
While described first adsorption tanks (3) carry out absorption work, described second adsorption tanks (4) carry out regenerative process: first introduce pure nitrogen gas and purge bed, replace, then heater (6) is opened, resolved the water of described second adsorption tanks (4) Middle molecule sieve absorption with hot nitrogen by circulator (7), the water deviate from is taken out of with gas, enter in storage tank (8), methyl nitrite in alkali liquor absorption gas in described storage tank (8), get back to circulator (7) after cooler (5) cooling from described storage tank (8) gas out and continue utilization, close described heater (6), adopt and through described cooler (5) cooled nitrogen, described second adsorption tanks (4) are lowered the temperature, the preparation of described second adsorption tanks (4) carries out absorption work,
2) described second adsorption tanks (4) carry out absorption work, and described first adsorption tanks (3) carry out reproduction operation, the same step 1) of detailed process for regenerating tank; Iterative cycles like this;
Wherein, the alkali lye in described storage tank (8) is be the alkali lye of 10% by the concentration that methyl alcohol is formulated.
6. use the gas-drying system in the synthesis gas preparing ethylene glycol technique described in claim 4 to carry out a method for gas drying, it is characterized in that: comprise the steps:
1) described second adsorption tanks (4) carry out absorption work, and described first adsorption tanks (3) are regenerating tank;
After cooling, enter the second adsorption tanks (4) from oxidative esterification tower (1) out reaction gas, the absorption of described second adsorption tanks (4) Middle molecule sieve sends into carbonylation unit after falling minor amount of water wherein, and the preparation of described second adsorption tanks (4) carries out reproduction operation;
While described second adsorption tanks (4) carry out absorption work, described first adsorption tanks (3) carry out regenerative process: first introduce pure nitrogen gas and purge bed, replace, then heater (6) is opened, resolved the water of described first adsorption tanks (3) Middle molecule sieve absorption with hot nitrogen by circulator (7), the water deviate from is taken out of with gas, enter in storage tank (8), methyl nitrite in alkali liquor absorption gas in described storage tank (8), get back to circulator (7) after cooler (5) cooling from described storage tank (8) gas out and continue utilization, close described heater (6), adopt and through described cooler (5) cooled nitrogen, described first adsorption tanks (3) are lowered the temperature, the preparation of described first adsorption tanks (3) carries out absorption work,
2) described first adsorption tanks (3) carry out absorption work, and described second adsorption tanks (4) carry out reproduction operation, the same step 1) of detailed process for regenerating tank; Iterative cycles like this;
Wherein, the alkali lye in described storage tank (8) is be the alkali lye of 10% by the concentration that methyl alcohol is formulated.
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| CN201310429057.9A CN103480247B (en) | 2013-09-18 | 2013-09-18 | Gas-drying system in a kind of synthesis gas preparing ethylene glycol technique and drying means |
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| CN103480247B true CN103480247B (en) | 2016-01-20 |
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| CN114602302B (en) * | 2020-12-08 | 2023-08-08 | 湖北富博化工有限责任公司 | Nitromethane tail gas recycling treatment method |
| CN114602311B (en) * | 2020-12-08 | 2023-11-07 | 湖北远大富驰医药化工股份有限公司 | Method for circularly preparing nitromethane |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6251165B1 (en) * | 1998-06-02 | 2001-06-26 | Institut Francais Du Petrole | Process for adsorbing and desorbing a solvent contained in a natural gas from a dehydration process |
| FR2819426A1 (en) * | 2001-01-18 | 2002-07-19 | Fr D Etudes Et De Realisations | Gas drying comprises use of solid desiccant to remove residual water from liquid desiccant after distillation |
| CN202022868U (en) * | 2011-04-08 | 2011-11-02 | 上海焦化有限公司 | Device for producing methyl nitrite and device for producing oxalic acid dimethyl ester by continuous circulating esterification and carbonylation coupling |
| CN203178186U (en) * | 2013-03-21 | 2013-09-04 | 安徽淮化股份有限公司 | Real-time esterification and carbonylation reaction on-line analysis system for ethylene glycol production industry through synthesis gas |
-
2013
- 2013-09-18 CN CN201310429057.9A patent/CN103480247B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6251165B1 (en) * | 1998-06-02 | 2001-06-26 | Institut Francais Du Petrole | Process for adsorbing and desorbing a solvent contained in a natural gas from a dehydration process |
| FR2819426A1 (en) * | 2001-01-18 | 2002-07-19 | Fr D Etudes Et De Realisations | Gas drying comprises use of solid desiccant to remove residual water from liquid desiccant after distillation |
| CN202022868U (en) * | 2011-04-08 | 2011-11-02 | 上海焦化有限公司 | Device for producing methyl nitrite and device for producing oxalic acid dimethyl ester by continuous circulating esterification and carbonylation coupling |
| CN203178186U (en) * | 2013-03-21 | 2013-09-04 | 安徽淮化股份有限公司 | Real-time esterification and carbonylation reaction on-line analysis system for ethylene glycol production industry through synthesis gas |
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