CN215102940U - Regeneration system for esterification of ethylene glycol and methyl nitrite prepared from coal - Google Patents
Regeneration system for esterification of ethylene glycol and methyl nitrite prepared from coal Download PDFInfo
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- CN215102940U CN215102940U CN202120239226.2U CN202120239226U CN215102940U CN 215102940 U CN215102940 U CN 215102940U CN 202120239226 U CN202120239226 U CN 202120239226U CN 215102940 U CN215102940 U CN 215102940U
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Abstract
The utility model discloses a regeneration system that is used for coal system ethylene glycol methyl nitrite to esterify, include: the regeneration tower is used for the synthesis reaction of methyl nitrite; the methanol circulating pipeline is used for circularly spraying the methanol in the regeneration tower; a methanol circulation pump disposed on the methanol circulation line and configured to generate a shutdown signal when the methanol circulation pump is shut down; the methanol storage tank is used for storing the methanol for standby spraying; the methanol pipeline is used for communicating the methanol storage tank with the regeneration tower; and the valve is arranged on the methanol pipeline and is configured to respond to the stop operation signal and conduct the methanol pipeline to feed methanol from the methanol storage tank to the regeneration tower. The utility model discloses a regeneration system meets when unusual operating mode such as methyl alcohol circulating pump jump car, and the valve can receive the signal that the methyl alcohol circulating pump sent, and the valve is opened in the linkage, and the methyl alcohol of methyl alcohol storage tank provides promptly to spray, makes the heat shift out fast, ensures regeneration system's operation safety.
Description
Technical Field
The utility model relates to a chemical industry equipment field, more specifically relate to a regeneration system that is used for coal system ethylene glycol methyl nitrite to esterify.
Background
The existing technical process route for preparing ethylene glycol from coal mainly adopts a raw material route for synthesizing ethylene glycol by a carbonylation and hydrogenation two-step method, and the total reaction equation is as follows: 2CO +4H2+1/2O2=(CH2OH)2+H2O；
The first step, preparation and regeneration of Methyl Nitrite (MN), the reaction equation is as follows:
2CH3OH+2NO+1/2O2=2CH3ONO+H20；
the second step, the synthesis of dimethyl oxalate (DMO), the reaction equation is:
2CH3ONO+2CO=(COOCH3)2+H2O；
step three, preparing ethylene glycol by hydrogenating dimethyl oxalate, wherein the reaction equation is as follows:
(COOCH3)2+4H2=(CH2OH)2+2CH3OH；
the methyl nitrite esterification regeneration is one of important steps of preparing ethylene glycol from coal, synthetic recycle gas is introduced into an esterification regeneration tower, methanol recycle solution is sprayed on the tower top, oxygen with accurate proportion is added, and NO, gasified methanol and oxygen in the synthetic recycle gas react at 65-70 ℃ and 0.35MPa to generate methyl nitrite. In the operation process, the reaction temperature must be strictly controlled, the reaction rate will be greatly increased after the temperature is increased, a large amount of reaction heat is generated, and the overtemperature is caused, so that the safe operation of equipment and a system is damaged.
Methyl nitrite is a substance which is very easy to decompose, abbreviated as MN, and can be decomposed thermally and catalytically in the presence of a catalyst. The thermal decomposition products of MN are methanol, formaldehyde, NO and water, and the catalytic decomposition products of MN are methyl formate, methanol, NO and water. Methyl nitrite decomposition generates a large amount of decomposition heat, resulting in rapid increase in temperature and pressure, resulting in reaction runaway.
Excessive oxygen proportion can also cause violent reaction in the esterification regeneration tower, and the reaction is intensified along with the rise of temperature and pressure, thereby causing over-temperature and over-pressure of equipment.
In the esterification regeneration step of the methyl nitrite in the coal-to-ethylene glycol, the main measure for removing the reaction heat is to take away the heat through a large amount of circulating gas, and on the other hand, the sufficient spraying methanol is utilized for gasification to take away the heat, and the two are mutually supplemented, but the shortage is not necessary. When the esterification regeneration system encounters abnormal working conditions such as power failure, steam stop, water stop and the like, which cause the stop of a synthesis cycle gas compressor, the jump of a methanol cycle methanol pump of an esterification regeneration tower and the like, process gas in the system does not flow in a short time, the supply of the cycle methanol is stopped, the reaction continues in the two towers in a short time, the concentration of MN exceeds the standard, the explosion limit is reached, and the over-temperature, over-pressure and even explosion accidents are likely to happen. In recent years, domestic coal-to-ethylene glycol enterprises have been subjected to esterification tower explosion accidents because reaction heat in an accident state cannot be rapidly removed, and the accidents cause overtemperature, overpressure and explosion.
SUMMERY OF THE UTILITY MODEL
In order to solve the technical problem, the utility model provides a regeneration system for coal system ethylene glycol methyl nitrite esterifies, include: the regeneration tower is used for the synthesis reaction of methyl nitrite; the methanol circulating pipeline is used for circularly spraying the methanol in the regeneration tower; a methanol circulation pump disposed on the methanol circulation line and configured to generate a shutdown signal when the methanol circulation pump is shut down; the methanol storage tank is used for storing the methanol for standby spraying; the methanol pipeline is used for communicating the methanol storage tank with the regeneration tower; and the valve is arranged on the methanol pipeline and is configured to respond to the stop operation signal and conduct the methanol pipeline to feed methanol from the methanol storage tank to the regeneration tower.
In some embodiments, the method further comprises: the circulating gas pipeline is used for introducing synthetic circulating gas into the regeneration tower; the gas flow sensing device is arranged on the circulating gas pipeline and used for detecting whether gas in the circulating synthesis gas pipeline flows or not and generating a flow stopping signal when no gas flows; wherein the valve is further configured to respond to the flow stopping signal and conduct a methanol pipeline to feed methanol from the methanol storage tank to the regeneration tower.
In some embodiments, the regeneration tower further comprises an accumulator communicated with the methanol storage tank, wherein the accumulator internally controls a predetermined pressure value for providing power for methanol in the methanol storage tank to enter the regeneration tower.
In some embodiments, the predetermined pressure value is between 0.6 MPa and 1.0 MPa.
In some embodiments, the valve is a quick-open valve or an air-close valve.
In some embodiments, the valve has a delayed opening function.
In some embodiments, the delay is between 1 and 4 seconds.
In some embodiments, the system further comprises a methanol introducing main pipeline for introducing or supplementing methanol into the regeneration tower; the methanol is introduced into the branch pipeline, and the methanol storage tank is communicated with the methanol introduction main pipeline and is used for introducing or supplementing methanol into the methanol storage tank.
In some embodiments, the methanol pipeline is communicated with the methanol circulating pipeline, and a check valve is arranged on the pipeline at the position where the pipeline is communicated with the outlet of the methanol circulating pump and used for preventing the methanol in the methanol storage tank from being refilled into the methanol circulating pump after the valve is opened.
In some embodiments, the methanol line has a length of 5 meters or less.
The utility model discloses well methyl alcohol storage tank passes through the upper portion intercommunication of methyl alcohol pipeline and regenerator column, is provided with the valve on the methyl alcohol pipeline, runs into the methyl alcohol circulating pump when unusual operating mode such as skip car when regeneration system, and circulation methyl alcohol stops under the condition of supply, and the signal that the methyl alcohol circulating pump sent can be received to this valve, and the valve is opened in the linkage, and the methyl alcohol of methyl alcohol storage tank passes through the methyl alcohol pipeline and gets into the regenerator column for provide and promptly spray, make the heat shift out fast, ensure regeneration system's operation safety.
Drawings
Fig. 1 is a schematic structural diagram of a regeneration system according to an embodiment of the present invention.
Symbolic illustration in the drawings:
1, a regeneration tower;
2, a methanol storage tank;
3 an accumulator;
4, a valve;
5 a check valve;
6 a methanol circulating pump;
7 a methanol distributor;
101 introducing methanol into a main pipeline;
1011 methanol is introduced into a branch pipeline;
102 a methanol pipeline;
103 methanol circulation line;
104 a methanol circulation line;
105 oxygen gas inlet pipeline;
106 gas phase outlet line;
107 circulating gas lines.
Detailed Description
The technical features of the present invention are further explained by the following embodiments with reference to the accompanying drawings:
the embodiment provides a regeneration system for esterifying ethylene glycol methyl nitrite prepared from coal, as shown in fig. 1, including: the device comprises a regeneration tower 1, methanol circulating pipelines 103 and 104, a methanol circulating pump 6, a methanol storage tank 2 and a methanol pipeline 102, wherein the regeneration tower 1 is used for the synthesis reaction of methyl nitrite; the methanol circulating pipelines 103 and 104 are used for circulating spraying of methanol in the regeneration tower 1; a methanol circulation pump 6 disposed between the methanol circulation lines 103 and 104, configured to generate a stop signal when the methanol circulation pump 6 stops operating; the methanol storage tank 2 is used for storing methanol for standby spraying; the methanol pipeline 102 is used for communicating the methanol storage tank 2 with the regeneration tower 1, and preferably, the length of the methanol pipeline 102 is less than 5 meters, so that the methanol in the methanol storage tank 2 enters the regeneration tower 1 as soon as possible; a valve 4 is disposed on the methanol line 102 and configured to open the methanol line 102 in response to the stop signal to introduce methanol from the methanol storage tank 2 to the regeneration tower 1 for emergency spraying.
In this embodiment, a gas flow sensing device (not shown) is disposed on the recycle gas line 107 for introducing the synthesis recycle gas into the regeneration tower 1, and is configured to detect whether gas in the recycle gas line 107 flows or not, and generate a stop flow signal when no gas flows, and the valve 4 is capable of responding to the stop flow signal and/or the stop operation signal, and conducting the methanol line 102 to introduce methanol from the methanol storage tank 2 to the regeneration tower 1 for emergency spraying.
In this embodiment, the system further comprises an accumulator 3 communicated with the methanol storage tank 2, wherein a predetermined pressure value is controlled inside the accumulator 3 for providing power for the methanol in the methanol storage tank 2 to enter the regeneration tower, and preferably, the predetermined pressure value is controlled inside the accumulator 3 to be between 0.6 MPa and 1.0 MPa.
In some embodiments, the valve 4 is a quick-opening valve and/or an air-closing valve, where the quick-opening valve is that the valve has only two regulating valve positions and is fully opened or fully closed, and the air-closing valve is that the power source is an air source, and in the case of an air source, the valve is in a closed state, and the valve automatically opens when the air source fails, so as to ensure that the methanol in the methanol storage tank 2 can rapidly enter the regeneration tower 1 in an accident state.
In some embodiments, the valve 4 has a delayed opening function, the controller of the valve 4 can set to delay the opening of the valve 4 for a predetermined time after receiving the stop flow signal and/or the stop operation signal, and the controller of the valve 4 is opened after receiving the signal for the predetermined time, so as to avoid the valve 4 being opened erroneously due to signal fluctuation, and preferably, the set predetermined time is between 1 and 4s, and is preferably set to 3 s.
In the embodiment, the methanol inlet main pipe 101 is communicated with the upper part of the regeneration tower 1 and is used for supplementing methanol into the regeneration tower so as to supplement the loss of the methanol in the circulation process; the methanol inlet branch pipeline 1011 is communicated with the methanol storage tank 2 and the methanol inlet main pipeline 101 and is used for introducing or supplementing methanol into the methanol storage tank 2, and the purity of the methanol introduced into the methanol inlet main pipeline 101 and the methanol inlet branch pipeline 1011 is higher and is different from the methanol used in circulation.
In this embodiment, the methanol pipeline 102 is communicated with the methanol circulation pipeline 104, and a check valve 5 is disposed on the methanol circulation pipeline 104 at the pipeline communication position and the outlet of the methanol circulation pump 6, so as to prevent methanol in the methanol storage tank 2 from being back-filled into the methanol circulation pump 6 after the valve 4 is opened.
In the normal operation state of the regeneration system of the embodiment, the valve on the branch 1011 for introducing the methanol in the methanol storage tank 2 is opened, the methanol storage tank 2 is filled with the methanol, and the valve is closed; the connecting valve between the accumulator 3 and the methanol storage tank 2 is opened and the valve 4 on the methanol line 102 is closed during normal production. Synthetic recycle gas (main components are CO, NO and CO)2、N2MN, etc.) enters the regeneration tower 1 through a circulating gas pipeline 107, and the middle upper part of the regeneration tower 1 is connected with an oxygen introducing pipeline 105, NO, O2、The methanol reacts in the tower to generate MN, and MN gas phase is output from a gas phase outlet pipeline 106 connected with the middle lower part of the regeneration tower 1. When the regeneration system encounters abnormal working conditions such as the shutdown of a recycle gas compressor or the shutdown of a methanol circulating pump 6, an airflow sensing device arranged on a circulating gas pipeline 107 monitors that the synthesis circulating gas airflow stops flowing to generate a flow stopping signal, or the methanol circulating pump 6 generates an operation stopping signal, a controller of a valve 4 starts the valve 4 after receiving the flow stopping signal and/or the operation stopping signal, and standby methanol in a methanol storage tank 2 can rapidly enter a methanol circulating pipeline 104 through a methanol pipeline 102 and is introduced into a methanol distributor 7 in a regeneration tower 1 for emergency spraying. A large amount of latent heat is taken away by the gasification of the methanol in the regeneration tower 1, and the heat is quickly removed, so that the safe and efficient treatment of a regeneration system is ensured.
In a preferred embodiment, the methanol storage tank is designed to have a volume of 1m3The length of the methanol pipeline 102 is less than 5m, the pipe diameter is set to DN150, the flow speed of the methanol is 2m/s, the valve 4 is an air-closed valve and a quick-open valve (has two functions) under the condition that the pressure of the energy accumulator is controlled to be 0.6-1.0 MPa, the methanol can enter the regeneration tower 1 within the time of less than 3s, and the diameter of the methanol is 1m3The methanol can continuously provide 28s of emergency spraying, and the heat can be rapidly removed in the accident state. The calculation method comprises the following steps: 1m3/(2× 3.14 × 0.15 × 0.15/4) =28 s. In practical implementation, the methanol amount of the methanol storage tank can be adjusted according to actual needs, and preferably, the methanol storage amount provides 25 s-60 s of emergency spraying to meet emergency requirements.
In the regeneration system of this embodiment, methanol storage tank 2 passes through the upper portion intercommunication of methanol pipeline 102 with regenerator column 1, be provided with valve 4 on the methanol pipeline 102, run into the recycle gas compressor when regeneration system runs into abnormal conditions such as trip, methanol circulating pump 6 trips, the gaseous nonmobility of circulation in the system, or under the condition that circulation methyl alcohol stopped to supply, the signal that air current sensing device or methanol circulating pump sent can be received to valve 4's controller, valve 4 is opened in the linkage, methanol storage tank 2's methyl alcohol passes through methanol pipeline 102 and gets into regenerator column 1, be used for providing emergency spray, make the heat shift out fast, ensure regeneration system's operation safety.
While the embodiments of the present invention have been described with reference to the accompanying drawings, the present invention is not limited to the above-described embodiments, which are merely illustrative and not restrictive, and many modifications may be made by one skilled in the art without departing from the spirit and scope of the present invention as defined in the appended claims.
Claims (10)
1. A regeneration system for coal-based ethylene glycol methyl nitrite esterification is characterized by comprising:
the regeneration tower is used for the synthesis reaction of methyl nitrite;
the methanol circulating pipeline is used for circularly spraying the methanol in the regeneration tower;
a methanol circulation pump disposed on the methanol circulation line and configured to generate a stop signal when the methanol circulation pump stops operating;
the methanol storage tank is used for storing the methanol for standby spraying;
the methanol pipeline is used for communicating the methanol storage tank with the regeneration tower;
and the valve is arranged on the methanol pipeline and is configured to respond to the stop operation signal and conduct the methanol pipeline to feed methanol from the methanol storage tank to the regeneration tower.
2. The regeneration system for the esterification of methyl nitrite in ethylene glycol prepared from coal as claimed in claim 1, further comprising:
the circulating gas pipeline is used for introducing synthetic circulating gas into the regeneration tower;
the gas flow sensing device is arranged on the circulating gas pipeline and used for detecting whether gas in the circulating gas pipeline flows or not and generating a flow stopping signal when no gas flows;
wherein the valve is further configured to, in response to the stop flow signal, open the methanol line to pass methanol from the methanol storage tank to the regeneration column.
3. The regeneration system for the esterification of methyl nitrite in ethylene glycol prepared from coal as claimed in claim 1 or 2, further comprising an accumulator communicated with the methanol storage tank, wherein a predetermined pressure value is controlled inside the accumulator for providing power for the methanol in the methanol storage tank to enter the regeneration tower.
4. The regeneration system for the esterification of methyl nitrite in ethylene glycol prepared from coal as claimed in claim 3, wherein the predetermined pressure value is between 0.6 MPa and 1.0 MPa.
5. The regeneration system for the esterification of methyl nitrite in ethylene glycol prepared from coal as claimed in claim 1 or 2, wherein the valve is a quick-opening valve or a gas-closing valve.
6. The regeneration system for the esterification of methyl nitrite in ethylene glycol prepared from coal as claimed in claim 1 or 2, wherein the valve has a delayed opening function.
7. The regeneration system for the esterification of methyl nitrite in ethylene glycol prepared from coal as claimed in claim 6, wherein the predetermined delay time is between 1 and 4 seconds.
8. The regeneration system for the esterification of methyl nitrite in ethylene glycol prepared from coal as claimed in claim 1 or 2, further comprising a main methanol introduction pipeline for introducing or supplementing methanol to the regeneration tower;
and the methanol inlet branch pipeline is communicated with the methanol storage tank and the methanol inlet main pipeline and is used for introducing or supplementing methanol into the methanol storage tank.
9. The regeneration system for the esterification of methyl nitrite in ethylene glycol prepared from coal as claimed in claim 1 or 2, wherein the methanol pipeline is communicated with the methanol circulation pipeline, and a check valve is arranged on the pipeline at the position where the pipeline is communicated with the outlet of the methanol circulation pump, and is used for preventing the methanol in the methanol storage tank from being back-filled into the methanol circulation pump after the valve is opened.
10. The regeneration system for the esterification of methyl nitrite in ethylene glycol prepared from coal as claimed in claim 1 or 2, wherein the length of the methanol pipeline is less than 5 m.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120239226.2U CN215102940U (en) | 2021-01-28 | 2021-01-28 | Regeneration system for esterification of ethylene glycol and methyl nitrite prepared from coal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120239226.2U CN215102940U (en) | 2021-01-28 | 2021-01-28 | Regeneration system for esterification of ethylene glycol and methyl nitrite prepared from coal |
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