CN111530407B - Esterification reactor and esterification reaction method - Google Patents
Esterification reactor and esterification reaction method Download PDFInfo
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- CN111530407B CN111530407B CN202010367863.8A CN202010367863A CN111530407B CN 111530407 B CN111530407 B CN 111530407B CN 202010367863 A CN202010367863 A CN 202010367863A CN 111530407 B CN111530407 B CN 111530407B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/04—Preparation of esters of nitrous acid
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Abstract
The invention relates to the technical field of coal-to-ethylene glycol, in particular to an esterification reactor and an esterification reaction method. An esterification reactor comprises a shell, an oxidation device and an esterification device arranged above the oxidation device, wherein the oxidation device and the esterification device are both arranged inside the shell, so that the oxidation device and the esterification device are integrally arranged in a vertical direction. The esterification reactor integrates the oxidation device and the esterification device, so that a large amount of heat carried by gas in the oxidation device is introduced into the esterification device, a heating device at the bottom of the original esterification device is removed, the manufacturing cost of the esterification reactor is reduced, the effective utilization of the heat is realized, the heat loss is reduced, and the cost of the esterification reaction is reduced; meanwhile, the integrated esterification reactor reduces the floor area and further reduces the production cost.
Description
Technical Field
The invention relates to the technical field of coal-to-ethylene glycol, in particular to an esterification reactor and an esterification reaction method.
Background
At present, the esterification reactor of ethylene glycol basically adopts a combination mode of an oxidation reactor and an esterification reactor. In the oxidation reactor, nitrogen monoxide and oxygen gas generate nitrogen dioxide, and the nitrogen dioxide and methanol are introduced into the esterification reactor to generate methyl nitrite. The esterification reactor generally adopts a mode of a rectifying tower, and a heating device is arranged at the bottom of the esterification reactor to increase the temperature inside the rectifying tower, so that the methyl nitrite is conveniently separated from the mixed gas and is discharged from an upper gas phase outlet. In the esterification process, energy waste is easily caused by overhigh reaction temperature in the oxidizer, and a heating device at the bottom of the esterification reactor also needs to consume a large amount of energy. Meanwhile, in the prior art, the reaction efficiency is low due to insufficient mixing of oxygen and nitric oxide.
Disclosure of Invention
The invention aims to solve the problem that energy is wasted due to low energy utilization rate in the prior art.
In order to achieve the above object, an aspect of the present invention provides an esterification reactor, including a housing, an oxidation device, and an esterification device disposed above the oxidation device, wherein the oxidation device and the esterification device are both disposed inside the housing, such that the oxidation device and the esterification device are integrally disposed in a vertical direction.
Preferably, the oxidation device comprises an oxidation reaction unit and a cooling unit; the cooling unit comprises a first section with the lower part corresponding to the oxidation reaction unit and a second section with the upper part extending out of the oxidation reaction unit, and the first section is communicated with the second section.
Preferably, the oxidation reaction unit includes the first inlet pipe that is used for letting in oxygen and the second inlet pipe that is used for letting in nitric oxide, first inlet pipe with the second inlet pipe is in inside interior pipe and the excircle pipe that overlaps mutually and establish outside circling the formation of oxidation unit, interior outside of pipe is provided with a plurality of first jets, the outer pipe inboard is provided with a plurality of second jets, so that oxygen with nitric oxide sprays relatively.
Preferably, the cooling unit includes a radiating pipe spirally arranged inside the housing, and two ends of the radiating pipe are respectively provided with a circulating cooling water outlet and a circulating cooling water inlet.
Preferably, the esterification device comprises a plurality of esterification reaction modules arranged in the vertical direction, each esterification reaction module comprises a filler and a redistributor arranged above the filler, and a third feed port for introducing methanol is arranged on the side surface of the shell.
Preferably, the upper end of the shell is provided with a gas phase outlet for discharging reaction mixed gas in the esterification reactor, and the bottom of the shell is provided with a liquid outlet for discharging reaction mixed liquid in the esterification reactor.
Preferably, a liquid level gauge is arranged at the lower part of the shell.
Preferably, the esterification reactor is provided with a plurality of pressure gauges for measuring pressures at a plurality of locations in the esterification reactor and a plurality of temperature gauges for measuring temperatures at a plurality of locations in the esterification reactor.
Preferably, the radiating pipe is a surface-sintered high-flux heat exchange pipe.
In a second aspect of the present invention, an esterification reaction method using the esterification reactor described in any one of the above, comprises:
s1, introducing nitric oxide and oxygen into the oxidation device to mix to generate nitrogen dioxide;
s2, introducing methanol into the esterification device, and allowing the nitrogen dioxide and the nitric oxide in the oxidation device to enter the esterification device to react with the methanol to generate methyl nitrite.
The esterification reactor integrates the oxidation device and the esterification device, so that a large amount of heat carried by gas in the oxidation device is introduced into the esterification device, a heating device at the bottom of the original esterification device is removed, the manufacturing cost of the esterification reactor is reduced, the effective utilization of the heat is realized, the heat loss is reduced, and the cost of the esterification reaction is reduced; meanwhile, the integrated esterification reactor reduces the floor area and further reduces the production cost.
Drawings
FIG. 1 is a schematic diagram of the structure of an esterification reactor according to one embodiment of the present invention;
fig. 2 is a schematic diagram of the structure of the oxidation reaction unit of fig. 1 in which oxygen is mixed with a raw material gas.
Description of the reference numerals
1-esterification device, 2-oxidation device, 3-cooling unit, 4-radiating pipe, 5-recirculated cooling water outlet, 6-recirculated cooling water inlet, 7-first feeding pipe, 8-second feeding pipe, 9-liquid level device, 10-pressure detector, 11-temperature detector, 12-liquid outlet, 13-gas phase outlet, 14-third feeding port, 15-redistributor, 16-filler, 17-shell, 18-oxidation reaction unit, 19-first jet orifice and 20-second jet orifice.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The invention provides an esterification reactor, which comprises a shell 17, an oxidation device 2 and an esterification device 1 arranged above the oxidation device 2, wherein the oxidation device 2 and the esterification device 1 are both arranged inside the shell 17, so that the oxidation device 2 and the esterification device 1 are integrally arranged in the vertical direction.
The esterification reactor integrates the oxidation device and the esterification device, so that a large amount of heat carried by gas in the oxidation device is introduced into the esterification device, a heating device at the bottom of the original esterification device is removed, the manufacturing cost of the esterification reactor is reduced, the effective utilization of the heat is realized, the heat loss is reduced, and the cost of the esterification reaction is reduced; meanwhile, the integrated esterification reactor reduces the floor area and further reduces the production cost.
Preferably, the oxidation apparatus includes an oxidation reaction unit 18 and a cooling unit 3; the cooling unit 3 comprises a first section with the lower part corresponding to the oxidation reaction unit 18 and a second section with the upper part extending out of the oxidation reaction unit 18, and the first section is communicated with the second section. The gas in the oxidation device rises due to continuous aeration at the bottom, and the first section is used for taking away most heat while reacting oxygen and nitric oxide in the oxidation device; and the second section is used for further removing heat in the process of rising the reaction mixed gas.
Preferably, the oxidation reaction unit 18 includes a first feeding pipe 7 for introducing oxygen and a second feeding pipe 8 for introducing nitric oxide, the first feeding pipe 7 and the second feeding pipe 8 are in the inside spiral of the oxidation device forms an inner circular pipe and an outer circular pipe which are sleeved with each other, a plurality of first injection ports 19 are arranged on the outer side of the inner circular pipe, and a plurality of second injection ports 20 are arranged on the inner side of the outer circular pipe, so that oxygen and nitric oxide are relatively injected.
The oxygen and the nitric oxide in the original oxidation reaction unit 18 are respectively sprayed from the tubes arranged up and down, so that the mixing efficiency is low; in the oxidation reaction unit 18 of the present invention, the first feeding pipe 7 and the second feeding pipe 8 are coiled with each other, and the injection ports are arranged oppositely, so that the mixing efficiency of the reaction raw materials is increased, and the reaction rate is increased. In addition, the invention comprises an embodiment that the first feeding pipe 7 is an inner circular pipe, and the second feeding pipe 8 is an outer circular pipe; also included is an embodiment in which the first feed conduit 7 is an outer circular tube and the second feed conduit 8 is an inner circular tube.
Preferably, the cooling unit 3 comprises a radiating pipe 4 spirally arranged inside the outer casing 17, and a circulating cooling water outlet 5 and a circulating cooling water inlet 6 are respectively arranged at two ends of the radiating pipe 4. The cooling medium is led into the radiating pipe 4 in the shell 17 in a spiral mode to exchange heat with the oxidation reaction unit 18, so that explosion caused by overheating of the oxidation reaction unit 18 is avoided, and the safety of the esterification reactor is improved.
Preferably, the esterification apparatus 1 comprises a plurality of esterification reaction modules arranged in a vertical direction, the esterification reaction modules comprise a filler 16 and a redistributor 15 arranged above the filler 16, and a third feed port 14 for introducing methanol is arranged on the side surface of the housing 17.
The redistributor 15 drips the methanol on the filler 16, and the filler 16 is used for the sufficient contact of the methanol liquid and the gas from the oxidation reaction unit 18 to accelerate the reaction rate reaction and generate methyl nitrite; the reaction mixture carrying the methyl nitrite produces a distillation effect due to the heat in the esterification reactor to produce the effect of separating the methyl nitrite.
Preferably, the upper end of the housing 17 is provided with a gas phase outlet 13 for discharging reaction mixed gas in the esterification reactor, and the bottom of the housing 17 is provided with a liquid outlet 12 for discharging reaction mixed liquid in the esterification reactor. The reaction mixture gas is continuously introduced into the bottom of the esterification reactor and generates gas, so that the reaction mixture gas is upwards discharged from the gas phase outlet 13, and the reaction mixture liquid falls downwards into the bottom of the esterification reactor under the action of gravity and is discharged from the liquid outlet 12.
Preferably, a liquid level gauge 9 is arranged at the lower part of the shell 17 at intervals. The liquid level device 9 arranged at intervals is used for controlling the water level at the bottom of the esterification reactor within a certain range, and gas is prevented from being introduced into the first feeding pipe 7 and the second feeding pipe 8 due to overhigh water level. Meanwhile, the fact that the water level is too low may mean that the reaction efficiency of the esterification reactor is not high, so that the water level at the bottom needs to be detected.
Preferably, the esterification reactor is provided with a plurality of pressure gauges 10 for measuring pressures at a plurality of locations in the esterification reactor and a plurality of temperature gauges 11 for measuring temperatures at a plurality of locations in the esterification reactor. The temperature in the esterification reactor needs to be monitored in real time by using a temperature detector 11 so as to avoid explosion caused by local overheating or influence on reaction efficiency due to too low temperature; the pressure at each part in the esterification reactor needs to be monitored in real time by using a pressure gauge 10 so as to avoid the influence of blockage in the esterification reactor on the reaction efficiency. In addition, the temperature or pressure of a plurality of places of the esterification reactor needs to be monitored in real time to ensure that the reaction is carried out smoothly.
Preferably, the heat dissipation pipe 4 is configured as a surface-sintered high-flux heat exchange pipe. The surface sintering type high-flux heat exchange tube has the advantages of quicker heat exchange, higher heat exchange efficiency and improvement on the operating efficiency of the esterification reactor.
In a second aspect of the present invention, an esterification reaction method using the esterification reactor described in any one of the above, comprises:
s1, introducing nitric oxide and oxygen into the oxidation device 2 to mix to generate nitrogen dioxide;
s2, introducing methanol into the esterification device 1, and introducing the nitrogen dioxide and the nitric oxide in the oxidation device 2 into the esterification device 1 to react with the methanol to generate methyl nitrite.
The process of the present invention will now be described with reference to the embodiment shown in FIG. 1. specifically, the esterification reactor comprises an oxidation unit and an esterification unit disposed above the oxidation unit.
The oxidation device comprises an oxidation reaction unit 18 and a cooling unit 3; the cooling unit 3 comprises a first section with the lower part corresponding to the oxidation reaction unit 18 and a second section with the upper part extending out of the oxidation reaction unit 18, and the first section is communicated with the second section. Wherein, oxidation reaction unit 18 is including the first inlet pipe 7 that is used for letting in oxygen and the second inlet pipe 8 that is used for letting in nitric oxide, first inlet pipe 7 with second inlet pipe 8 is in inside spiral shell of oxidation unit forms inside and outside pipe and the excircle pipe of establishing of overlapping, the outside of inner circle pipe is provided with a plurality of first jet 19, the outside pipe inboard is provided with a plurality of second jet 20, so that oxygen with nitric oxide sprays relatively.
In the oxidation apparatus: introducing oxygen into a first feeding pipe 7, introducing nitric oxide into a second feeding pipe 8, wherein the first feeding pipe 7 and the second feeding pipe 8 are arranged in a mutually-coiled mode, and jet ports are arranged oppositely; the nitric oxide and the oxygen are relatively sprayed and mixed and react in the oxidation reaction unit 18 to generate nitrogen dioxide; while the oxidation reaction unit 18 is reacting, the first section of the lower part of the cooling unit 3 corresponding to the oxidation reaction unit 18 exchanges heat with the oxidation reaction unit 18; excessive temperatures of the oxidation reaction unit 18 are avoided. Wherein, the oxygen is introduced at 15-40 ℃; introducing nitric oxide at 10-50 ℃; the mixed gas in the oxidation reaction unit is 150-230 ℃.
Since the bottom oxidation reaction unit 18 is always being fed with gas, the generated nitrogen dioxide and the incompletely reacted nitrogen monoxide enter the area where the esterification apparatus 1 is located; before the mixed gas enters the esterification device 1, the second section of the upper part of the cooling unit 3 extending out of the oxidation reaction unit 18 continuously exchanges heat with the mixed gas, so that the temperature of the mixed gas is reduced. During the process of the mixed gas entering the esterification device, a large amount of heat released during the reaction of nitric oxide and oxygen also enters the esterification device 1 along with the mixed gas. Wherein the mixed gas cooled by the cooling unit is 50-90 ℃.
In the esterification apparatus 1: introducing methanol into a third feed inlet 14 to enter the tower, redistributing the methanol in the upper filler to the filler 16 by a redistributor 15, allowing the mixed gas with higher temperature from a bottom oxidation device to upwards pass through the filler 16, allowing the methanol liquid to downwards contact with the mixed gas at the filler 16 due to gravity, and reacting nitric oxide and nitrogen dioxide in the mixed gas with the methanol to generate a product containing methyl nitrite; the mixed gas from the oxidation unit has a relatively high heat content, and this heat content rectifies the mixed product carrying methyl nitrite. The temperature of rectification can be controlled by the heat exchange efficiency of the cooling unit, so that methyl nitrite with higher concentration is discharged from a gas phase outlet 13; while the mixed liquid containing the incompletely reacted methanol liquid is discharged at the liquid outlet at the bottom. Wherein the mixed gas in the esterification device is 60-90 ℃.
The esterification device of the prior esterification reactor is characterized in that nitrogen dioxide products generated by nitric oxide and oxygen and methanol are introduced into the esterification device together to generate methyl nitrite; the esterification reactor of the invention is to react the mixed gas generated in the oxidation device with methanol upwards to generate methyl nitrite because the bottom part is continuously aerated.
The esterification reactor integrates the oxidation device and the esterification device, so that a large amount of heat carried by gas in the oxidation device is introduced into the esterification device, a heating device at the bottom of the original esterification device is removed, the manufacturing cost of the esterification reactor is reduced, the effective utilization of the heat is realized, the heat loss is reduced, and the cost of the esterification reaction is reduced; meanwhile, the integrated esterification reactor reduces the floor area and further reduces the production cost.
The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention. Including each of the specific features, are combined in any suitable manner. The invention is not described in detail in order to avoid unnecessary repetition. Such simple modifications and combinations should be considered within the scope of the present disclosure as well.
Claims (10)
1. An esterification reactor, characterized by comprising a housing (17), an oxidation device (2) and an esterification device (1) arranged above the oxidation device (2), wherein the oxidation device (2) and the esterification device (1) are both arranged inside the housing (17), so that the oxidation device (2) and the esterification device (1) are integrally arranged in a vertical direction.
2. Esterification reactor according to claim 1, characterized in that the oxidation device comprises an oxidation reaction unit (18) and a cooling unit (3); the cooling unit (3) comprises a first section with the lower part corresponding to the oxidation reaction unit (18) and a second section with the upper part extending out of the oxidation reaction unit (18), and the first section is communicated with the second section.
3. The esterification reactor according to claim 2, wherein the oxidation reaction unit (18) comprises a first feeding pipe (7) for feeding oxygen and a second feeding pipe (8) for feeding nitric oxide, the first feeding pipe (7) and the second feeding pipe (8) are coiled inside the oxidation device to form an inner circular pipe and an outer circular pipe which are sleeved inside and outside, the outer side of the inner circular pipe is provided with a plurality of first injection ports (19), and the inner side of the outer circular pipe is provided with a plurality of second injection ports (20) so that the oxygen and the nitric oxide are injected relatively.
4. Esterification reactor according to claim 2, characterized in that the cooling unit (3) comprises a heat pipe (4) spirally arranged inside the housing (17), and the heat pipe (4) is provided with a circulating cooling water outlet (5) and a circulating cooling water inlet (6) at two ends thereof, respectively.
5. Esterification reactor according to claim 1, characterized in that the esterification apparatus (1) comprises a plurality of esterification modules arranged in a vertical direction, the esterification modules comprise a filler (16) and a redistributor (15) arranged above the filler (16), and the side of the housing (17) is provided with a third feed opening (14) for methanol.
6. The esterification reactor according to claim 1, wherein the housing (17) is provided at an upper end thereof with a gas phase outlet (13) for discharging the reaction mixture gas in the esterification reactor, and the bottom of the housing (17) is provided with a liquid outlet (12) for discharging the reaction mixture liquid in the esterification reactor.
7. Esterification reactor according to claim 1, characterized in that a liquid level gauge (9) is provided spaced below the housing (17).
8. Esterification reactor according to claim 1, characterized in that it is provided with a plurality of pressure gauges (10) for measuring the pressure at a plurality of locations within the esterification reactor and a plurality of temperature gauges (11) for measuring the temperature at a plurality of locations within the esterification reactor.
9. Esterification reactor according to claim 4, characterized in that the heat-conducting pipes (4) are provided as surface-sintered high-flux heat-exchanging pipes.
10. An esterification reaction method using the esterification reactor according to any one of claims 1 to 9, comprising:
s1, introducing nitric oxide and oxygen into the oxidation device (2) to be mixed to generate nitrogen dioxide;
s2, introducing methanol into the esterification device (1), and introducing the nitrogen dioxide and the nitric oxide in the oxidation device (2) into the esterification device (1) to react with the methanol to generate methyl nitrite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202010367863.8A CN111530407B (en) | 2020-04-30 | 2020-04-30 | Esterification reactor and esterification reaction method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010367863.8A CN111530407B (en) | 2020-04-30 | 2020-04-30 | Esterification reactor and esterification reaction method |
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| CN111530407A CN111530407A (en) | 2020-08-14 |
| CN111530407B true CN111530407B (en) | 2022-01-28 |
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Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007842A (en) * | 2012-12-26 | 2013-04-03 | 安阳盈德气体有限公司 | Methyl nitrite synthesis reactor |
| CN105272859B (en) * | 2014-07-03 | 2018-01-09 | 中国石油化工股份有限公司 | The production method of alkyl nitrite |
| CN104945263A (en) * | 2015-06-01 | 2015-09-30 | 江苏金聚合金材料有限公司 | Synthesis method and equipment of alkyl nitrite |
| CN106565498B (en) * | 2015-10-12 | 2018-07-17 | 中国石油化工股份有限公司 | The production method of methyl nitrite |
| WO2020082194A1 (en) * | 2018-10-22 | 2020-04-30 | Pujing Chemical Industry Co., Ltd | Process and system for producing alkyl nitrites |
| CN209155805U (en) * | 2018-10-24 | 2019-07-26 | 阳泉煤业集团平定化工有限责任公司 | It is esterified pre-reactor |
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