CN110818568A - Device for continuously producing methyl nitrite gas and application thereof - Google Patents
Device for continuously producing methyl nitrite gas and application thereof Download PDFInfo
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- CN110818568A CN110818568A CN201810891957.8A CN201810891957A CN110818568A CN 110818568 A CN110818568 A CN 110818568A CN 201810891957 A CN201810891957 A CN 201810891957A CN 110818568 A CN110818568 A CN 110818568A
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- BLLFVUPNHCTMSV-UHFFFAOYSA-N methyl nitrite Chemical compound CON=O BLLFVUPNHCTMSV-UHFFFAOYSA-N 0.000 title claims abstract description 239
- 239000002994 raw material Substances 0.000 claims abstract description 89
- 238000011156 evaluation Methods 0.000 claims abstract description 83
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 81
- 239000012530 fluid Substances 0.000 claims abstract description 74
- 238000004868 gas analysis Methods 0.000 claims abstract description 59
- 238000002360 preparation method Methods 0.000 claims abstract description 37
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 17
- 230000005540 biological transmission Effects 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 98
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 37
- 230000003197 catalytic effect Effects 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 22
- 238000003860 storage Methods 0.000 claims description 12
- 238000004891 communication Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000010924 continuous production Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 2
- 238000006722 reduction reaction Methods 0.000 abstract description 6
- 239000007789 gas Substances 0.000 description 236
- 239000003054 catalyst Substances 0.000 description 37
- 238000006243 chemical reaction Methods 0.000 description 26
- 239000012071 phase Substances 0.000 description 22
- 239000007791 liquid phase Substances 0.000 description 15
- 239000000203 mixture Substances 0.000 description 15
- 238000000034 method Methods 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- 238000011160 research Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LOMVENUNSWAXEN-UHFFFAOYSA-N Methyl oxalate Chemical compound COC(=O)C(=O)OC LOMVENUNSWAXEN-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- JRLTTZUODKEYDH-UHFFFAOYSA-N 8-methylquinoline Chemical group C1=CN=C2C(C)=CC=CC2=C1 JRLTTZUODKEYDH-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- -1 firstly Substances 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 238000012332 laboratory investigation Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Molecular Biology (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a device for continuously producing methyl nitrite gas and application thereof, comprising: a methyl nitrite gas production system for continuously producing methyl nitrite gas; a gas analysis system for obtaining a methyl nitrite gas concentration, the methyl nitrite gas being from a methyl nitrite gas production system; and the first fluid transmission control unit is connected with the methyl nitrite gas preparation system and the gas analysis system, and is used for communicating the methyl nitrite gas preparation system with the gas analysis system to provide a gas sample to be analyzed for the gas analysis system and controlling the product output of the methyl nitrite gas preparation system. The invention realizes the stable supply of methyl nitrite gas, and further connects a methyl nitrite gas preparation system with a catalytic reaction evaluation system which takes methyl nitrite as raw material in series, thereby realizing the stability and service life evaluation of the nitric acid reduction reaction for preparing the methyl nitrite gas and the supply of a stable gas source for the catalytic reaction.
Description
Technical Field
The invention relates to the technical field of continuous production of methyl nitrite, in particular to a device for continuously producing methyl nitrite gas and application thereof.
Background
Methyl nitrite gas is a raw material gas for catalytic reaction such as synthesis of dimethyl oxalate by CO gas phase coupling, and is industrially regenerated by reaction cycle, so that there is no problem of continuous supply of methyl nitrite gas, but in laboratory tests, methyl nitrite is consumed, and in the study of the process or evaluation of a catalyst, methyl nitrite gas is not commercially available and needs to be self-made in a laboratory due to its instability. Therefore, the design of a set of methyl nitrite gas continuous supply device is of great significance for laboratory investigation of the service life of the catalyst for the reaction of CO and methyl nitrite.
The existing method for continuously producing methyl nitrite gas has some defects, and methyl nitrite gas generated by reaction is influenced by factors such as original concentration, environmental temperature, pressure and the like, namely, the concentration of the generated methyl nitrite gas is unstable, so that the subsequent process or catalyst evaluation is influenced. Since the requirement for the accuracy of data is high in catalyst evaluation and process research, a device for continuously supplying methyl nitrite gas with a stable and known concentration is required to realize the process research of catalytic reaction or the life test of the catalyst to stably operate for a long period.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide an apparatus for continuously producing methyl nitrite gas and use thereof, comprising: a methyl nitrite gas production system for continuously producing methyl nitrite gas; a gas analysis system for obtaining a methyl nitrite gas concentration, the methyl nitrite gas being from a methyl nitrite gas production system; and the first fluid transmission control unit is connected with the methyl nitrite gas preparation system and the gas analysis system, and is used for communicating the methyl nitrite gas preparation system with the gas analysis system to provide a gas sample to be analyzed for the gas analysis system and controlling the product output of the methyl nitrite gas preparation system. The invention realizes the stable supply of methyl nitrite gas, and further connects a methyl nitrite gas preparation system and a catalytic reaction evaluation system which takes methyl nitrite as raw material in series, thereby realizing the stability and service life evaluation of the nitric acid reduction reaction prepared by the methyl nitrite gas, the supply of a stable gas source of the catalytic reaction, the process research of the catalytic reaction which takes the methyl nitrite as the raw material, such as CO and methyl nitrite, and the like, or the service life evaluation of the catalyst.
To achieve the above and other related objects, a first aspect of the present invention provides an apparatus for continuously producing methyl nitrite gas, comprising:
a methyl nitrite gas production system for continuously producing methyl nitrite gas;
a gas analysis system for obtaining a methyl nitrite gas concentration, the methyl nitrite gas being from a methyl nitrite gas production system;
and the first fluid transmission control unit is connected with the methyl nitrite gas preparation system and the gas analysis system, and is used for communicating the methyl nitrite gas preparation system with the gas analysis system to provide a gas sample to be analyzed for the gas analysis system and controlling the product output of the methyl nitrite gas preparation system.
The first fluid delivery control unit is used for controlling the flow direction of the methyl nitrite gas mixture.
Preferably, at least one of the following technical features is also included:
1) the methyl nitrite gas preparation system comprises a methyl nitrite generation reactor and a first gas-liquid separator which are connected, and the first gas-liquid separator is connected with a gas analysis system through the first fluid conveying control unit;
the first gas-liquid separator is provided with a gas-phase outlet and a liquid-phase outlet, the gas-phase outlet of the first gas-liquid separator is connected with the first fluid conveying control unit, and the liquid-phase outlet of the first gas-liquid separator is provided with a liquid discharge valve;
2) the gas analysis system comprises a first gas analyzer, a first emptying pipeline and a pipeline for connecting the first gas analyzer, the first fluid conveying control unit is connected with the first emptying pipeline and the pipeline for connecting the first gas analyzer in parallel through pipelines, and the pipeline for connecting the first gas analyzer is connected with the first gas analyzer; the first gas analyzer may be a gas chromatograph;
3) a first pressure gauge is arranged on a pipeline connecting the first fluid conveying control unit and the gas analysis system;
4) a first backpressure valve is arranged on a pipeline connecting the first fluid conveying control unit and the gas analysis system;
5) the first fluid conveying control unit comprises a first three-way valve, a first end of the first three-way valve is connected with the methyl nitrite gas preparation system, a second end of the first three-way valve is connected with the gas analysis system, and a third end of the first three-way valve is used for outputting methyl nitrite gas outwards.
More preferably, in feature 5), the first fluid delivery control unit further includes a first three-way valve control block, the first three-way valve control block is in communication connection with the gas analysis system and the first three-way valve, and is configured to control the first three-way valve to switch on the gas analysis system, control the first three-way valve to stop outputting the methyl nitrite gas to the outside when the methyl nitrite gas concentration measured by the gas analysis system does not reach the target, and control the first three-way valve to output the methyl nitrite gas to the outside when the methyl nitrite gas concentration measured by the gas analysis system reaches the target.
More preferably, in the feature 1), the methyl nitrite gas production system further comprises a first raw material supply unit for producing methyl nitrite gas, the first raw material supply unit being connected to the methyl nitrite generation reactor.
Still more preferably, a second pressure gauge is provided on a pipe connecting the first raw material supply part and the methyl nitrite generation reactor.
Still more preferably, the first raw material supply part includes a supply unit for an aqueous solution containing methanol and nitric acidElement, supply NO unit and supply N2And (4) units.
Still further more preferably, at least one of the following technical features is also included:
a1) the unit for supplying the aqueous solution containing the methanol and the nitric acid comprises a liquid storage tank, a weighing device and a metering pump, wherein the weighing device and the metering pump are arranged below the liquid storage tank;
a2) the NO supply unit comprises an NO supply pipeline and a first flowmeter arranged on the NO supply pipeline, and the NO supply pipeline is connected with the methyl nitrite generation reactor;
a3) supply N2The unit includes a supply N2Pipe and supply N2Second flow meters on pipes, supply N2The pipeline is connected with the methyl nitrite generating reactor;
a4) the first raw material supply part further comprises a first mixing tank, the NO supply unit and the N supply2The unit is connected with a methyl nitrite generation reactor through a first mixing tank.
The methyl nitrite gas production system includes, but is not limited to, a production system in which a gaseous phase raw material containing nitric oxide and a nitric acid waste water solution containing methanol are reacted in a methyl nitrite generation reactor to obtain methyl nitrite. Using a gas phase raw material containing nitric oxide to react with a nitric acid wastewater solution containing methanol to obtain methyl nitrite: the reaction temperature is 40-120 ℃, the pressure is 0.1-1.0MPaG, and the liquid hourly space velocity is 1-4m3/mcat 3H, liquid retention time of 20-60min, gas hourly space velocity of 200-3/mcat 3H, gas residence time 0.1-0.4s, molar ratio of NO to nitric acid 2-8. In volume percentage, the content of NO in the gas phase raw material is 5-20 percent, and N is2The content of (A) is 80-95%; in the liquid phase raw material, the content of nitric acid is 1-10%, the content of water is 0-40%, and the content of methanol is 55-99% by mass percentage.
Preparing liquid raw materials according to requirements, storing the prepared liquid raw materials in a liquid storage tank, placing the liquid raw materials on a weighing device, conveying the liquid raw materials into a methyl nitrite generation reactor through a metering pump, and preparing raw material gas NO and N2Respectively fed into the second tank through a first flowmeter and a second flowmeterA mixing tank and then a methyl nitrite generation reactor, wherein after the gas-liquid mixture such as methyl nitrite generated by the reaction is separated by a first gas-liquid separator, the liquid phase is discharged periodically, and the pH value can be measured by sampling and the liquid phase is analyzed by liquid chromatography; and the separated gas phase is introduced into a first gas analyzer through a first fluid conveying control unit to analyze the concentration of methyl nitrite gas, and when the concentration of the methyl nitrite gas in the analysis and test gas phase reaches the standard, the gas is introduced into a subsequent catalytic reaction evaluation device taking methyl nitrite as a raw material.
The second aspect of the present invention provides use of the above apparatus for continuously producing methyl nitrite gas for supplying methyl nitrite to a catalytic reaction using methyl nitrite as a raw material.
A third aspect of the present invention provides a catalytic reaction evaluation apparatus using methyl nitrite as a raw material, including:
the above-mentioned apparatus for continuously producing methyl nitrite gas;
a catalytic reaction evaluation system using methyl nitrite as a raw material is connected with a product output end of a first fluid delivery control unit in a device for continuously producing methyl nitrite gas.
Preferably, at least one of the following technical features is also included:
1) the catalytic reaction evaluation equipment further comprises a dryer, and the catalytic reaction evaluation system is connected with the product output end of the first fluid conveying control unit through the dryer; the dryers can be a group of dryers, and the dryers are connected in parallel or in series;
2) the catalytic reaction evaluation equipment further comprises a third flow meter, and the third flow meter is arranged on a communication pipeline between the catalytic reaction evaluation system and the product output end of the first fluid conveying control unit;
3) the catalytic reaction evaluation system comprises a catalytic reaction component using methyl nitrite as a raw material, a second gas-liquid separator and a gas analyzer, wherein the catalytic reaction component is communicated with a product output end of the first fluid conveying control unit, and is connected with the gas analyzer through the second gas-liquid separator.
The second gas-liquid separator is provided with a gas-phase outlet and a liquid-phase outlet, the gas-phase outlet of the second gas-liquid separator is connected with the gas analyzer, and the liquid-phase outlet of the second gas-liquid separator is provided with a liquid discharge valve.
More preferably, in the feature 3), the catalytic reaction component includes a catalytic reactor.
Further more preferably, at least one of the following technical features is also included:
a1) the catalytic reaction component also comprises a third pressure gauge which is arranged on a pipeline connecting the product output end of the first fluid conveying control unit and the catalytic reactor;
a2) the catalytic reaction component also comprises a second raw material supply component for catalytic reaction, and the second raw material supply component is connected with the catalytic reactor.
Still more preferably, in the feature a2), at least one of the following technical features is further included:
b1) the catalytic reaction evaluation equipment further comprises a second mixing tank, and the second raw material supply component and the output end of the first fluid conveying control unit are connected in parallel through a pipeline and then connected with the catalytic reactor through the second mixing tank;
b2) the second raw material supply part comprises a CO supply unit and an N supply unit2And (4) units.
Still even more preferably, the feature b2) further includes at least one of the following technical features:
c1) the CO supply unit comprises a CO supply pipeline and a fourth flowmeter arranged on the CO supply pipeline, and the CO pipeline is connected with the catalytic reactor;
c2) supply N2The unit includes a supply N2Pipe and supply N2Fifth flowmeter on the pipeline, said supply N2A conduit is connected to the catalytic reactor.
The catalytic reaction evaluation system comprises but is not limited to all chemical reactions of CO and methyl nitrite which take methyl nitrite as raw material. Catalyst for evaluation of reaction of CO with methyl nitrite: one of alumina or molecular sieve is taken as a carrier, the supported subgroup metal elements include but are not limited to one or two of Pd, Pt, Ti, Fe, Co, Ni and the like, and the metal loading is between 0.01 wt% and 0.5 wt%.
More preferably, in the feature 3), at least one of the following technical features is further included:
d1) a third pressure gauge is arranged on a pipeline connecting the second gas-liquid separator and the gas analyzer;
d2) a second back pressure valve is arranged on a pipeline connecting the second gas-liquid separator and the gas analyzer;
d3) the second gas-liquid separator is connected with a second emptying pipeline and a pipeline connected with a gas analyzer in parallel through pipelines, and the second gas-liquid separator is connected with the gas analyzer through the pipeline connected with the gas analyzer;
d4) the catalytic reaction evaluation system further comprises a second fluid conveying control unit, the gas analysis system comprises a first gas analyzer, the first gas analyzer is used as the gas analyzer of the catalytic reaction evaluation system, and the second gas-liquid separator and the first fluid conveying control unit are connected with the first gas analyzer through the second fluid conveying control unit. The second fluid conveying control unit is used for controlling the tail gas analysis sources of the nitrite gas preparation system and the catalyst evaluation system.
Still more preferably, in the feature d4), the second fluid delivery control unit includes a second three-way valve, a first end of the second three-way valve is connected to the first fluid delivery control unit, a second end of the second three-way valve is connected to the first gas analyzer, and a third end of the second three-way valve is connected to the second gas-liquid separator.
Still further more preferably, the second fluid transportation control unit further includes a second three-way valve control block, the second three-way valve control block is in communication connection with the first gas analyzer and the second three-way valve, and is configured to control the second three-way valve to communicate the first fluid transportation control unit with the first gas analyzer when the methyl nitrite gas concentration measured by the first gas analyzer does not reach a target, and control the second three-way valve to communicate the second gas-liquid separator with the first gas analyzer when the methyl nitrite gas concentration measured by the first gas analyzer reaches a target.
When the concentration of methyl nitrite gas in an analysis test gas phase reaches the standard, the gas is led to a subsequent catalytic reaction evaluation device which takes methyl nitrite as a raw material, firstly, water and other impurities carried in mixed gas are removed through a dryer, the mixed gas enters a catalytic reactor of a catalytic reaction evaluation system after being measured through a mass flow meter, CO or other gases which need to be supplemented in catalytic reaction enter the catalytic reactor for reaction after being measured through a third flow meter, reaction outlet gas enters a second gas-liquid separator, liquid phase products can be stored in the second gas-liquid separator with the function of a product tank and are periodically discharged, most of tail gas is discharged after the gas phase passes through a second back pressure valve, and a small amount of part of tail gas is sent to a gas analyzer for gas chromatography analysis of tail gas composition.
The invention has at least any one of the following beneficial effects:
1. the device for continuously producing the methyl nitrite gas realizes the continuous supply of the methyl nitrite gas, thereby ensuring that the research on the catalytic reaction process or the performance evaluation of the catalyst which takes the methyl nitrite as the raw material can be smoothly carried out;
2. analyzing the concentration of methyl nitrite gas continuously supplied and other gas concentrations according to a first gas analyzer (gas chromatograph), and providing calculation basis for the conversion rate, selectivity, space-time yield and the like of a subsequent catalyst evaluation system taking methyl nitrite as a raw material;
3. adjusting the liquid hourly space velocity and the gas space velocity of a methyl nitrite gas preparation system according to the actual requirements of catalytic reaction process research or catalyst performance evaluation by taking methyl nitrite as a raw material to realize stable supply of methyl nitrite gas;
4. the device for continuously producing methyl nitrite gas can be independently used as a catalyst evaluation system for the nitric acid reduction reaction;
5. when the catalyst evaluation is performed, the methyl nitrite gas production system and the catalyst evaluation system may be regarded as a whole, and the second back pressure valve in the catalytic reaction evaluation device using methyl nitrite as a raw material is adjusted to be the system pressure of the whole of the methyl nitrite gas production system and the catalyst evaluation system;
6. the tail gas of a methyl nitrite gas preparation system containing methyl nitrite gas is used as a raw material gas of a catalytic reaction evaluation system taking methyl nitrite as a raw material, the flow rate of the tail gas is read by a flowmeter of the catalyst evaluation system, and other gases required by the catalyst evaluation system can be replenished by other flowmeters of the catalyst evaluation system;
7. the tail gas of the catalyst evaluation system and the tail gas of the methyl nitrite gas preparation system share a first gas analyzer (gas chromatograph), and the analysis of the required tail gas is realized by adjusting a second three-way valve;
8. the catalyst evaluation system can be used as a catalyst evaluation system for generating dimethyl oxalate by the reaction of CO and methyl nitrite, a catalyst evaluation system for generating dimethyl carbonate by the reaction of CO and methyl nitrite and other catalyst evaluation systems using methyl nitrite as raw materials, and is realized by adjusting a catalyst formula, reaction temperature, reaction pressure and the like.
Drawings
FIG. 1 is a schematic view of an apparatus for continuously producing methyl nitrite gas and an apparatus for evaluating a catalytic reaction using methyl nitrite as a raw material connected in series according to the present invention.
1-a first flow meter;
2-a second flow meter;
3-a first mixing tank;
4-a liquid storage tank;
5-weighing device;
6-a metering pump;
7-a second pressure gauge;
8-methyl nitrite generating reactor;
9-a first gas-liquid separator;
10-a drain valve;
11-a first fluid delivery control unit;
12-a first pressure gauge;
13-a first back pressure valve;
14-a first gas analyzer;
15-a dryer;
16-a fourth flow meter;
17-a fifth flow meter;
18-a third flow meter;
19-a second mixing tank;
20-a third pressure gauge;
21-a catalytic reactor;
22-a second gas-liquid separator;
23-a second fluid delivery control unit;
24-a third pressure gauge;
25-second backpressure valve.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are intended to be illustrative only and not to limit the scope of the invention.
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
FIG. 1 is a schematic view of a methyl nitrite gas continuous production apparatus and a catalytic reaction evaluation system using methyl nitrite as a raw material connected in series according to the present invention.
As shown in fig. 1, the apparatus for continuously producing methyl nitrite gas comprises: a methyl nitrite gas production system for continuously producing methyl nitrite gas; a gas analysis system for obtaining a methyl nitrite gas concentration, the methyl nitrite gas being from a methyl nitrite gas production system; the first fluid transmission control unit 11 is connected with the methyl nitrite gas preparation system and the gas analysis system, and is used for communicating the methyl nitrite gas preparation system with the gas analysis system on one hand so as to provide a gas sample to be analyzed for the gas analysis system, and is used for controlling the product output of the methyl nitrite gas preparation system on the other hand.
The methyl nitrite gas preparation system comprises a methyl nitrite generation reactor 8 and a first gas-liquid separator 9 which are connected, wherein the first gas-liquid separator 9 is connected with a gas analysis system through a first fluid conveying control unit 11; the methyl nitrite gas production system further includes a first raw material supply unit for producing methyl nitrite gas, the first raw material supply unit being connected to the methyl nitrite generation reactor 8. And a second pressure gauge 7 is arranged on a pipeline connecting the first raw material supply component and the methyl nitrite generation reactor 8.
The first raw material supply part comprises an aqueous solution supply unit containing methanol and nitric acid, an NO supply unit and an N supply unit2A unit; the unit for supplying the aqueous solution containing the methanol and the nitric acid comprises a liquid storage tank 4, a weighing device 5 and a metering pump 6, wherein the weighing device 5 and the metering pump 6 are arranged below the liquid storage tank, and the liquid storage tank 4 is connected with the methyl nitrite generation reactor 8 through the metering pump 6; the NO supply unit comprises an NO supply pipeline and a first flowmeter 1 arranged on the NO supply pipeline, and the NO supply pipeline is connected with the methyl nitrite generation reactor 8; supply N2The unit includes a supply N2Pipe and supply N2Second flow meter 2 on the pipe for N2A pipeline is connected with the methyl nitrite generating reactor 8; the first raw material supply part further comprises a first mixing tank 3, the NO supply unit and the N supply2The unit is connected to a methyl nitrite generation reactor 8 via a first mixing tank 3.
The gas analysis system comprises a first gas analyzer 14, a first emptying pipeline and a pipeline for connecting the first gas analyzer, the first fluid conveying control unit 11 is connected with the first emptying pipeline and the pipeline for connecting the first gas analyzer in parallel through pipelines, and the pipeline for connecting the first gas analyzer is connected with the first gas analyzer 14; a first pressure gauge 12 is arranged on a pipeline connecting the first fluid transmission control unit 11 and the gas analysis system; a first backpressure valve 13 is arranged on a pipeline connecting the first fluid transmission control unit 11 and the gas analysis system; the first fluid conveying control unit 11 includes a first three-way valve, a first end of the first three-way valve is connected to the methyl nitrite gas preparation system, a second end of the first three-way valve is connected to the gas analysis system, and a third end of the first three-way valve is used for outputting methyl nitrite gas to the outside. The first fluid transportation control unit 11 further includes a first three-way valve control block, the first three-way valve control block is in communication connection with the gas analysis system and the first three-way valve, and is configured to control the first three-way valve to be connected to the gas analysis system, control the first three-way valve to stop outputting methyl nitrite gas to the outside when the concentration of methyl nitrite gas measured by the gas analysis system does not reach a target, and control the first three-way valve to output methyl nitrite gas to the outside when the concentration of methyl nitrite gas measured by the gas analysis system reaches a target.
As shown in fig. 1, the apparatus for evaluating a catalytic reaction using methyl nitrite as a raw material includes: the above-mentioned apparatus for continuously producing methyl nitrite gas; a catalytic reaction evaluation system using methyl nitrite as a raw material is connected to a product output terminal of a first fluid transport control unit 11 in a device for continuously producing methyl nitrite gas. The catalytic reaction evaluation equipment further comprises a dryer 15, and the catalytic reaction evaluation system is connected with the product output end of the first fluid conveying control unit 11 through the dryer 15; the catalytic reaction evaluation equipment further comprises a third flow meter 18, wherein the third flow meter 18 is arranged on a communication pipeline between the catalytic reaction evaluation system and a product output end of the first fluid transportation control unit 11; the catalytic reaction evaluation system comprises a catalytic reaction component using methyl nitrite as a raw material, a second gas-liquid separator 22 and a gas analyzer, wherein the catalytic reaction component is communicated with a product output end of the first fluid conveying control unit 11 and is connected with the gas analyzer through the second gas-liquid separator 22; the catalytic reaction component comprises a catalytic reactor 21, and further comprises a third pressure gauge 20 which is arranged on a pipeline connecting the product output end of the first fluid conveying control unit 11 and the catalytic reactor 21; the catalytic reaction component also comprises a second raw material supply component for catalytic reaction, and the second raw material supply component is connected with the catalytic reactor 21; the catalytic reaction evaluation apparatus further comprises a second mixing tank 19, the second supply sourceThe material component and the output end of the first fluid conveying control unit (11) are connected in parallel through a pipeline and then connected with the catalytic reactor 21 through the second mixing tank 19; the second raw material supply part comprises a CO supply unit and an N supply unit2A unit; the CO supply unit comprises a CO supply pipeline and a fourth flowmeter 16 arranged on the CO supply pipeline, and the CO pipeline is connected with the catalytic reactor 21; supply N2The unit includes a supply N2Pipe and supply N2Fifth flowmeter 17 on the pipeline, said supply N2The pipe is connected with the catalytic reactor 21; a third pressure gauge 24 is arranged on a pipeline connecting the second gas-liquid separator 22 and the gas analyzer; a second back pressure valve 25 is arranged on a pipeline connecting the second gas-liquid separator 22 and the gas analyzer; the second gas-liquid separator 22 is connected in parallel with a second emptying pipeline and a pipeline connected with a gas analyzer through pipelines, and the second gas-liquid separator 22 is connected with the gas analyzer through the pipeline connected with the gas analyzer; the catalytic reaction evaluation system further comprises a second fluid delivery control unit 23, the gas analysis system comprises a first gas analyzer 14, the first gas analyzer 14 is used as a gas analyzer of the catalytic reaction evaluation system, and the second gas-liquid separator 22 and the first fluid delivery control unit 11 are connected with the first gas analyzer 14 through the second fluid delivery control unit 23; the second fluid transportation control unit 23 includes a second three-way valve, a first end of which is connected to the first fluid transportation control unit 11, a second end of which is connected to the first gas analyzer 14, and a third end of which is connected to the second gas-liquid separator 22; the second fluid transportation control unit 23 further includes a second three-way valve control block, which is in communication connection with the first gas analyzer 14 and the second three-way valve, and is configured to control the second three-way valve to communicate the first fluid transportation control unit 11 with the first gas analyzer 14 when the concentration of the methyl nitrite gas measured by the first gas analyzer 14 does not reach a target, and to control the second three-way valve to communicate the second gas-liquid separator 22 with the first gas analyzer 14 when the concentration of the methyl nitrite gas measured by the first gas analyzer 14 reaches a target.
Preparing liquid raw materials as required, storing in a liquid storage tank 4, placing on a weighing device 5, feeding into a methyl nitrite generation reactor 8 via a metering pump such as a liquid metering pump 6, and feeding into raw material gas NO and N2The liquid raw material is sent into a first mixing tank 3 through a first flowmeter 1 such as a mass flowmeter and a second flowmeter 2 such as a mass flowmeter, and then sent into a methyl nitrite generation reactor 8, and the liquid raw material and the gas enter the methyl nitrite generation reactor 8 in a cocurrent or countercurrent mode to carry out nitric acid reduction reaction. Gas-liquid mixture such as methyl nitrite generated by the reaction enters a first gas-liquid separator 9 for gas-liquid separation, and liquid phase product is periodically discharged through a liquid discharge valve 10 at the bottom of the first gas-liquid separator 9 for sample analysis. A second pressure gauge 7 is arranged in front of the methyl nitrite generation reactor 8, and a first pressure gauge 12 is arranged behind the first gas-liquid separator 9 and is used for monitoring the pressure drop; the first backpressure valve 13 is used for adjusting the pressure of the methyl nitrite gas preparation system; the first fluid conveying control unit 11 is a first three-way valve, a first end of the first three-way valve is connected with the methyl nitrite gas preparation system, a second end of the first three-way valve is connected with the gas analysis system, a third end of the first three-way valve is used for outputting methyl nitrite gas to the outside, when the second end of the first three-way valve is connected with the gas analysis system, the first three-way valve 11 is arranged at an analysis position, and the gas is exhausted and analyzed through a first back pressure valve 13. Most of the gas behind the first back pressure valve 13 is exhausted, a small amount of gas enters a first gas analyzer 14 to analyze the gas phase composition of the tail gas, when the methyl nitrite gas is analyzed by the gas analysis system to reach the target concentration, the methyl nitrite gas preparation system provides the methyl nitrite gas with the target concentration through a first three-way valve, a feed gas is provided for a subsequent catalytic reaction evaluation system taking the methyl nitrite as a raw material, and research and evaluation of a nitric acid reduction catalyst can also be independently carried out.
The first gas-liquid separator 9 is provided with a gas phase outlet and a liquid phase outlet, the gas phase outlet of the first gas-liquid separator 9 is connected with a first fluid conveying control unit 11, the liquid phase outlet of the first gas-liquid separator 9 is provided with a liquid discharge valve 10, and reactants in the methyl nitrite generation reactor 8 can be rapidly emptied through the liquid discharge valve 10 in an emergency.
When the methyl nitrite gas reaches the target concentration after being analyzed by the gas analysis system, the methyl nitrite gas preparation system may first enter the dryer 15 by adjusting the first fluid transportation control unit 11 to supply the methyl nitrite gas at the target concentration to the catalytic reaction evaluation system using methyl nitrite as a raw material, remove moisture or other impurities entrained in the gas phase, and then enter the third flow meter 18, such as a mass flow meter, to meter the gas flow from the methyl nitrite gas preparation system. From the third flow meter 18 and the fourth flow meter 16 on the CO supply conduit and the N supply2The gas of the fifth flowmeter 17 on the pipeline enters a second mixing tank 19, the mixed gas enters a catalytic reactor 21, and the gas-liquid mixture after reaction enters a second gas-liquid separator 22 for gas-liquid separation. A third pressure gauge 20 is arranged in front of the catalytic reactor 21, and a third pressure gauge 24 is arranged behind the second gas-liquid separator 22 for monitoring the pressure drop; the second backpressure valve 25 is used to regulate the pressure of the catalyst evaluation system. Most of the tail gas is exhausted after passing through the second backpressure valve 25, and a small amount of gas is sent to a gas analyzer for analyzing the gas phase composition of the tail gas. The tail gas analysis of the methyl nitrite preparation system and the catalyst evaluation system can share one gas analyzer, and the tail gas analysis can be adjusted by a second fluid conveying control unit 23 such as a second three-way valve, wherein the state of the second three-way valve has two positions of 'detection 1' and 'detection 2', and the two positions respectively correspond to the tail gas analysis of the methyl nitrite preparation system and the tail gas analysis of the catalyst evaluation system.
Under the action of catalyst, HNO3、CH3OH reacts with NO and the like in the process gas in a methyl nitrite generating reactor 8 to be converted into CH3ONO (MN), leaving the liquid phase, enters the catalyst evaluation system with the process gas.
2NO+HNO3+3CH3OH＝3CH3ONO+2H2O (1)
The main process conditions are as follows: the methyl nitrite generator is a fixed bed reactor; the reaction temperature is 40-120 ℃; the pressure is 0.1-1.0 MpaG.
NO and HNO in the reaction3The amount of the substance(s) is more than 2-8, and the methanol is excessive to ensure HNO3The conversion is complete as much as possible, so that the performance evaluation of the nitric acid reduction catalyst and the subsequent catalyst evaluation system are facilitated, and the Methyl Nitrite (MN) in the raw material gas has stable and higher concentration.
In the above, the liquid phase raw material contains, by mass, 1-10% of nitric acid, 0-40% of water, and 55-99% of methanol. The flow rate of the metering pump 6 is set to be 5-100ml/h, and the content of NO in the gas phase raw material is 5-20% in percentage by volume, and N is set to be2The content of (A) is 80-95%, and the flow rates of the mass flowmeters 1 and 2 are 5-20ml and 80-95ml respectively.
Example 1
The apparatus for continuously producing methyl nitrite gas and the catalytic reaction evaluation washing system using methyl nitrite as a raw material were connected in series as shown in FIG. 1. 5kg of raw material liquid is prepared in advance before the experiment, and the liquid-phase raw material contains 8 mass percent of nitric acid, 60 mass percent of methanol and 32 mass percent of water. N is turned on before reaction2Purging, namely performing nitrogen purging on the first mixing tank 3, the methyl nitrite generation reactor 8, the first gas-liquid separator 9, the dryer 15, the second mixing tank 19, the catalytic reactor 21, the second gas-liquid separator 22 and the whole pipeline, and performing pressure maintaining leak detection to ensure the safety of the system. NO and N2Respectively setting the flow rates to be 8ml/min and 60ml/min by using a first flow meter 1 such as a mass flow meter and a second flow meter 2 such as a mass flow meter, mixing in a first mixing tank 3, and then entering a methyl nitrite generation reactor 8; meanwhile, a raw material liquid with a raw material liquid flow rate set to 15ml/h by a metering pump 6 is introduced into a methyl nitrite generation reactor 8, and is subjected to a contact reaction under the action of a catalyst. The wall temperature of the methyl nitrite generation reactor 8 was set to 60 ℃ and the reaction pressure was set to 0.40 MPa. Methyl nitrite, water and excessive gas-liquid mixture generated in the reaction are subjected to gas-liquid separation through a first gas-liquid separator 9, and a liquid phase product is periodically discharged through a liquid discharge valve 10 at the bottom of the first gas-liquid separator 9 and is reserved for analysis. The first fluid transport control unit 11, i.e. the three-way valve, is switched to the "analysis" position, the gas phase separated by the first gas-liquid separator 9 is largely emptied after passing through the first back-pressure valve 13 and a small amount is sent to the first gas analyzer 14Namely, the composition of the tail gas was analyzed by gas chromatography, and the composition of the tail gas was 1-1 in Table 1.
After the tail gas of the methyl nitrite preparation system reaches the specified concentration and is kept stable, the first fluid conveying control unit 11, namely the three-way valve, is switched to the evaluation position, the tail gas of the methyl nitrite preparation system as the raw material gas of the catalyst evaluation system enters the drier 15, the tail gas enters the third flow meter 18 for metering after moisture and other gas phase impurities carried in the gas phase are removed, the gas flow from the methyl nitrite preparation system is about 75ml/min, the CO which passes through the fourth flow meter 16 is about 15ml/min, and the CO which passes through the fifth flow meter 17 is about 10ml/min N2The mixture enters a second mixing tank 19 to be mixed and then enters a catalytic reactor 21 to be in contact reaction under the action of a catalyst, the wall temperature of the catalytic reactor 21 is set to be 140 ℃, and the reaction pressure is set to be 0.40 Mpa; the gas-liquid mixture generated by the reaction enters the second gas-liquid separator 22 for gas-liquid separation, most of the tail gas is exhausted after flowing through the second back pressure valve 25, a small amount of gas is sent to a gas analyzer for analyzing the gas phase composition of the tail gas, the gas analyzer is the first gas analyzer 14, and the analysis results of the gas phase composition are shown in 1-2 in table 1.
The invention provides a device for continuous methyl nitrite gas, which takes the generated methyl nitrite as the raw material gas of a subsequent catalytic reaction evaluation system taking the methyl nitrite as the raw material, realizes that the methyl nitrite gas is consumed while being generated, avoids the potential safety hazard caused by the storage of the methyl nitrite gas, generates the methyl nitrite gas with stable concentration, provides the raw material gas with stable source for the evaluation of the subsequent catalytic reaction taking the methyl nitrite as the raw material, can change the required raw material gas concentration according to the requirement of the catalyst evaluation condition, and is convenient for the comparative analysis of the data of the catalyst evaluation.
Table 1 analysis of tail gas composition of example 1
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (17)
1. An apparatus for continuously producing methyl nitrite gas, comprising:
a methyl nitrite gas production system for continuously producing methyl nitrite gas;
a gas analysis system for obtaining a methyl nitrite gas concentration, the methyl nitrite gas being from a methyl nitrite gas production system;
and the first fluid conveying control unit (11) is connected with the methyl nitrite gas preparation system and the gas analysis system and is used for communicating the methyl nitrite gas preparation system with the gas analysis system on one hand so as to provide a gas sample to be analyzed for the gas analysis system and controlling the product output of the methyl nitrite gas preparation system on the other hand.
2. An apparatus for continuously producing methyl nitrite gas as claimed in claim 1, further comprising at least one of the following technical features:
1) the methyl nitrite gas preparation system comprises a methyl nitrite generation reactor (8) and a first gas-liquid separator (9) which are connected, wherein the first gas-liquid separator (9) is connected with a gas analysis system through a first fluid conveying control unit (11);
2) the gas analysis system comprises a first gas analyzer (14), a first emptying pipeline and a pipeline for connecting the first gas analyzer, the first fluid conveying control unit (11) is connected with the first emptying pipeline and the pipeline for connecting the first gas analyzer in parallel through pipelines, and the pipeline for connecting the first gas analyzer is connected with the first gas analyzer (14);
3) a first pressure gauge (12) is arranged on a pipeline connecting the first fluid transmission control unit (11) and the gas analysis system;
4) a first backpressure valve (13) is arranged on a pipeline connecting the first fluid transmission control unit (11) and the gas analysis system;
5) the first fluid conveying control unit (11) comprises a first three-way valve, a first end of the first three-way valve is connected with the methyl nitrite gas preparation system, a second end of the first three-way valve is connected with the gas analysis system, and a third end of the first three-way valve is used for outputting methyl nitrite gas outwards.
3. An apparatus for continuously producing a methyl nitrite gas as set forth in claim 2, wherein in the feature 5), the first fluid supply control unit (11) further comprises a first three-way valve control block which is connected in communication with the gas analysis system and the first three-way valve for controlling the first three-way valve to be connected to the gas analysis system, and which controls the first three-way valve to stop the output of the methyl nitrite gas when the concentration of the methyl nitrite gas measured by the gas analysis system does not reach the target, and controls the first three-way valve to output the methyl nitrite gas when the concentration of the methyl nitrite gas measured by the gas analysis system reaches the target.
4. A plant for continuous production of methyl nitrite gas as claimed in claim 2, wherein in the feature 1), the methyl nitrite gas production system further comprises a first raw material supply section for producing methyl nitrite gas, the first raw material supply section being connected to the methyl nitrite generation reactor (8).
5. An apparatus for continuous production of methyl nitrite gas as claimed in claim 4, wherein a second pressure gauge (7) is provided on a pipe connecting the first supply material unit and the methyl nitrite generating reactor (8).
6. An apparatus for continuously producing methyl nitrite gas as set forth in claim 4, wherein the first raw material supply means comprises a supply unit for an aqueous solution containing methanol and nitric acid, a supply unit for NO, and a supply unit for N2And (4) units.
7. An apparatus for continuously producing methyl nitrite gas as claimed in claim 6, further comprising at least one of the following technical features:
a1) the unit for supplying the aqueous solution containing the methanol and the nitric acid comprises a liquid storage tank (4), a weighing device (5) and a metering pump (6) which are arranged below the liquid storage tank, wherein the liquid storage tank (4) is connected with the methyl nitrite generation reactor (8) through the metering pump (6);
a2) the NO supply unit comprises an NO supply pipeline and a first flowmeter (1) arranged on the NO supply pipeline, and the NO supply pipeline is connected with the methyl nitrite generation reactor (8);
a3) supply N2The unit includes a supply N2Pipe and supply N2A second flowmeter (2) on the pipeline for N2The pipeline is connected with the methyl nitrite generating reactor (8);
a4) the first raw material supply part further comprises a first mixing tank (3), the NO supply unit and the N supply2The unit is connected with a methyl nitrite generation reactor (8) through a first mixing tank (3).
8. An apparatus for continuously producing methyl nitrite gas as claimed in any one of claims 1 to 7, which is used for supplying methyl nitrite to a catalytic reaction in which methyl nitrite is used as a raw material.
9. A catalytic reaction evaluation apparatus using methyl nitrite as a raw material, comprising:
an apparatus for continuously producing methyl nitrite gas as claimed in any one of claims 1 to 7;
a catalytic reaction evaluation system using methyl nitrite as a raw material is connected to a product output terminal of a first fluid transport control unit (11) in a device for continuously producing methyl nitrite gas.
10. A catalytic reaction evaluation apparatus using methyl nitrite as a raw material according to claim 9, further comprising at least one of the following technical features:
1) the catalytic reaction evaluation equipment further comprises a dryer (15), and the catalytic reaction evaluation system is connected with a product output end of the first fluid conveying control unit (11) through the dryer (15);
2) the catalytic reaction evaluation equipment further comprises a third flow meter (18), and the third flow meter (18) is arranged on a communication pipeline between the catalytic reaction evaluation system and a product output end of the first fluid conveying control unit (11);
3) the catalytic reaction evaluation system comprises a catalytic reaction component using methyl nitrite as a raw material, a second gas-liquid separator (22) and a gas analyzer, wherein the catalytic reaction component is communicated with a product output end of the first fluid conveying control unit (11), and the catalytic reaction component is connected with the gas analyzer through the second gas-liquid separator (22).
11. A catalytic reaction evaluation apparatus using methyl nitrite as a raw material according to claim 10, wherein in the feature 3), the catalytic reaction means includes a catalytic reactor (21).
12. A catalytic reaction evaluation apparatus in which methyl nitrite is a raw material according to claim 11, further comprising at least one of the following technical features:
a1) the catalytic reaction component also comprises a third pressure gauge (20) which is arranged on a pipeline connecting the product output end of the first fluid transmission control unit (11) with the catalytic reactor (21);
a2) the catalytic reaction component also comprises a second raw material supply component for catalytic reaction, and the second raw material supply component is connected with the catalytic reactor (21).
13. A catalytic reaction evaluation apparatus using methyl nitrite as a raw material according to claim 12, wherein the characteristic a2) further comprises at least one of the following technical characteristics:
b1) the catalytic reaction evaluation equipment further comprises a second mixing tank (19), and the second raw material supply component and the output end of the first fluid conveying control unit (11) are connected in parallel through a pipeline and then connected with the catalytic reactor (21) through the second mixing tank (19);
b2) the second raw material supply part comprises a CO supply unit and an N supply unit2And (4) units.
14. A catalytic reaction evaluation apparatus using methyl nitrite as a raw material according to claim 13, wherein the feature b2) further comprises at least one of the following technical features:
c1) the CO supply unit comprises a CO supply pipeline and a fourth flowmeter (16) arranged on the CO supply pipeline, and the CO pipeline is connected with the catalytic reactor (21);
c2) supply N2The unit includes a supply N2Pipe and supply N2A fifth flowmeter (17) on the pipeline, said supply N2The pipe is connected to the catalytic reactor (21).
15. The apparatus for evaluating a catalytic reaction using methyl nitrite as a raw material according to claim 10, characterized in that the characteristic 3) further comprises at least one of the following technical characteristics:
d1) a third pressure gauge (24) is arranged on a pipeline connecting the second gas-liquid separator (22) and the gas analyzer;
d2) a second backpressure valve (25) is arranged on a pipeline connecting the second gas-liquid separator (22) and the gas analyzer;
d3) the second gas-liquid separator (22) is connected with a second emptying pipeline and a pipeline connected with a gas analyzer in parallel through pipelines, and the second gas-liquid separator (22) is connected with the gas analyzer through the pipeline connected with the gas analyzer;
d4) the catalytic reaction evaluation system further comprises a second fluid conveying control unit (23), the gas analysis system comprises a first gas analyzer (14), the first gas analyzer (14) is used as a gas analyzer of the catalytic reaction evaluation system, and the second gas-liquid separator (22) and the first fluid conveying control unit (11) are connected with the first gas analyzer (14) through the second fluid conveying control unit (23).
16. The apparatus for evaluating a catalytic reaction using methyl nitrite as a raw material according to claim 15, characterized in that d4) the second fluid transport control unit (23) comprises a second three-way valve, a first end of the second three-way valve is connected to the first fluid transport control unit (11), a second end of the second three-way valve is connected to the first gas analyzer (14), and a third end of the second three-way valve is connected to the second gas-liquid separator (22).
17. A catalytic reaction evaluation apparatus for a methyl nitrite as a raw material according to claim 16, wherein the second fluid delivery control unit (23) further comprises a second three-way valve control block communicatively connected to the first gas analyzer (14) and the second three-way valve for controlling the second three-way valve to communicate the first fluid delivery control unit (11) with the first gas analyzer (14) when the methyl nitrite gas concentration measured by the first gas analyzer (14) does not reach a target, and to communicate the second gas-liquid separator (22) with the first gas analyzer (14) when the methyl nitrite gas concentration measured by the first gas analyzer (14) reaches a target.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805077A (en) * | 2022-04-29 | 2022-07-29 | 中国科学院福建物质结构研究所 | Full-automatic continuous production method and device for methyl nitrite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN204097372U (en) * | 2014-04-10 | 2015-01-14 | 中国科学院福建物质结构研究所 | A kind of CO vapor phase carbonylation produces the catalyst-assembly of methylcarbonate |
| CN106565494A (en) * | 2015-10-12 | 2017-04-19 | 中国石油化工股份有限公司 | Methyl nitrite preparation method by reaction of NO and nitric acid and methanol |
| CN106883127A (en) * | 2017-04-14 | 2017-06-23 | 高化学（江苏）化工新材料有限责任公司 | A kind of device for continuously generating methyl nitrite |
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- 2018-08-07 CN CN201810891957.8A patent/CN110818568A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204097372U (en) * | 2014-04-10 | 2015-01-14 | 中国科学院福建物质结构研究所 | A kind of CO vapor phase carbonylation produces the catalyst-assembly of methylcarbonate |
| CN106565494A (en) * | 2015-10-12 | 2017-04-19 | 中国石油化工股份有限公司 | Methyl nitrite preparation method by reaction of NO and nitric acid and methanol |
| CN106883127A (en) * | 2017-04-14 | 2017-06-23 | 高化学（江苏）化工新材料有限责任公司 | A kind of device for continuously generating methyl nitrite |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114805077A (en) * | 2022-04-29 | 2022-07-29 | 中国科学院福建物质结构研究所 | Full-automatic continuous production method and device for methyl nitrite |
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