CN106883127A - A kind of device for continuously generating methyl nitrite - Google Patents
A kind of device for continuously generating methyl nitrite Download PDFInfo
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- CN106883127A CN106883127A CN201710245118.4A CN201710245118A CN106883127A CN 106883127 A CN106883127 A CN 106883127A CN 201710245118 A CN201710245118 A CN 201710245118A CN 106883127 A CN106883127 A CN 106883127A
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- tubular reactor
- methyl nitrite
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- gas
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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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of device for continuously generating methyl nitrite, including tubular reactor, the heater located at tubular reactor tube wall, the liquid tank located at tubular reactor bottom, the cooling coil located at tubular reactor upper end, methanol tank, NO tanks and O2Tank, methanol tank is by pipeline communication in tubular reactor top, NO tanks and O2By pipeline communication in tubular reactor bottom, by pipeline communication in four-way valve, four-way valve is respectively communicated with reaction unit, gas analyzer and N tank on tubular reactor top2Blow device.A kind of device for continuously generating methyl nitrite provided by the present invention, simple structure, reaction is convenient；Difference in functionality is realized in the upper, middle and lower segment of a tubular reactor, reduce the risk of leakage, it is to avoid quality uncertainty and potential safety hazard that storage brings.
Description
Technical field
The present invention relates to technical field of chemical, and in particular to a kind of device for continuously generating methyl nitrite.
Background technology
Methyl nitrite gas is O2The unstripped gas of gaseous oxidation coupling synthesizing dimethyl oxalate reaction, is studying the technique
Or when evaluating catalyst, due to the property unstability of methyl nitrite gas, cannot commercially buy, it is necessary to voluntarily make
It is standby.
Existing method is all to produce methyl nitrite gas by liquid-phase chemical reaction, and various methods are used after collecting storage
Slow release is out used.
Disclosed in CN106278900A it is a kind of prepare methyl nitrite and method without interruption, nitrous acid solution and
Methanol sulphuric acid mixed solution reacts in a kettle., and reaction equation is as follows：
2NaNO2+2CH3OH+H2SO4→2CH3ONO+Na2SO4+2H2O
In addition to main reaction, nitric acid and nitrogen oxides etc. that also the decomposition of nitrous acid, disproportionation are formed, the nitrous acid of synthesis
Methyl esters in methyl alcohol, is released methyl nitrite gas to 30-100 DEG C when using in dissolving below freezing by heating response kettle
It is put into surge tank, it is clear that what is now released is the mixing gas of methyl nitrite and methyl alcohol, wherein the content of methyl nitrite
Influenceed by factors such as original concentration, release temperature and pressure, and this point is not referred in the patent.
Because in evaluating catalyst and technical study, the accuracy and precision requirement to data are higher, it is therefore desirable to
There is the methyl nitrite raw material that is constant and understanding content of stabilization.
And the reaction of the generation methyl nitrite of existing patented technology is all interval, to the methyl nitrite for providing
Purity does not also control effectively means, therefore there is following defect：
1. react complicated, accessory substance is more；
2. there are the container or device of storage methyl nitrite, there is potential safety hazard；
3. methyl nitrite place cause decomposition and other complicated side reactions cause raw material impurity content high；
4. constant and known content methyl nitrite can not be provided.
The content of the invention
It is an object of the invention to provide a kind of device for continuously generating methyl nitrite, in the above-mentioned prior art problem of solution
One or more.
A kind of device for continuously generating methyl nitrite of the invention, including tubular reactor, located at the tubular type
The heater of reactor tube walls, the liquid tank located at the tubular reactor bottom, located at the tubular reactor upper end
Cooling coil, methanol tank, NO tanks and O2Tank, the methanol tank is by pipeline communication in the tubular reactor top, the NO
Tank and the O2Tank by pipeline communication in the tubular reactor bottom, the tubular reactor top by pipeline communication in
Four-way valve, the four-way valve is respectively communicated with reaction unit, gas analyzer and N2Blow device.
A kind of device for continuously generating methyl nitrite provided by the present invention, simple structure, reaction is convenient；
Realize difference in functionality in the upper, middle and lower segment of a tubular reactor, between connectionless part, reduce leakage
Risk, carries out the purging of nitrogen before and after reaction, eliminate safe hidden trouble, and plunger metering pump, mass flowmenter are all by by computer
Control, realizes digitized regulation and accurate recording；
Realize methyl nitrite gas and produce consumption immediately immediately, it is to avoid quality uncertainty and peace that storage brings
Full hidden danger；
Liquid feedstock is accurately controlled by plunger metering pump, gas by mass flowmenter, is carried out instead in tubular reactor
Answer temperature control accurate, realize the stability and reappearance of gas supply；
Can be according to the actual requirements, there is provided the methyl nitrite gas of concentration accurate stable is used for CO synthesizing dimethyl oxalates
Catalyst developmental research, obtain extraordinary effect.
In some embodiments, the NO tanks and the O2The pipeline that tank is connected with the tubular reactor is provided with matter
Amount flowmeter, the mass flowmenter and the NO tanks and the O2N blow devices are respectively equipped between tank.By mass flow
Meter can well calculate NO and O2Mass ratio, N blow devices can be purged to whole device and be carried out pressurize leak detection.
In some embodiments, the pipeline that the methanol tank is connected with the tubular reactor is provided with plunger metering
Pump, the heater is heating furnace.Plunger metering pump can preferably calculate methanol flow rate, and the heating effect of heating furnace is more preferable.
In some embodiments, the tubular reactor bottom is provided with tapping valve.Can be by tapping valve under emergency case
Reactant in fast evacuation tubular reactor.
In some embodiments, using gas phase synthesis method, reaction equation is as follows：
4NO+O2+4CH3OH→4CH3ONO+2H2O
NO and O in reaction2The amount of material is 4 to 1, methyl alcohol excess, it is ensured that gas reacts completely, and methyl alcohol is except conduct
Reaction beyond the region of objective existence, also as the diluent of methyl nitrite.
Using gas phase synthesis method, reaction is simple, and accessory substance is few, and methyl nitrite is to produce to use, and without potential safety hazard, is obtained
Methyl nitrite purity is high, and can provide the methyl nitrite of constant level.
In some embodiments, such as following steps：N2 blow devices are first opened before reaction, to tubular reactor and first
Alcohol tank, NO tanks, O2Tank and whole pipeline carry out nitrogen purging, and carry out pressurize detection, it is ensured that system it is safe and reliable；Use plunger
Measuring pump sets methanol flow rate, in entering tubular reactor above heating furnace, NO and O2After flow being set with mass flowmenter
Enter from tubular reactor bottom after mixing, entered in tubular reactor by the liquid tank of bottom and contacted instead upwards with methyl alcohol
Should, the methyl alcohol gasified in the middle part of tubular reactor generates methyl nitrite and water with mixed gas reaction, then by cooling coil
Cool down obtaining product.Production process is simple and convenient, pollution-free.
In some embodiments, the methyl alcohol of the plunger metering pump sets flow velocity as 0.5-2mL/min, the quality stream
The setting NO of gauge：40-160mL/min、O2:10-40mL/min；The heating-up temperature of the heating furnace：It is 30-120 DEG C, described cold
But the chilling temperature of coil pipe：0-10℃.Convenient production methyl nitrite raw material that is constant and understanding content.
In some embodiments, four-way is entered from pipeline in the gas cooled down through the cooling coil on tubular reactor top
Valve, enters back into gas analyzer, and " use " state, supply response dress are switched to after concentration reaches prescribed concentration and keeps stabilization
Put and use；Use N2Blow device nitrogen purging removes the methyl nitrite remained in gas analyzer, water and other higher boiling pairs
Product flows into liquid tank, and liquid tank is periodically discharged；Valve transfer is to " detection " state, termination of pumping and pass when out of service
Hold one's breath road main valve, open the N on air pipe2Blow device carries out being purged through gas analyzer.The state of four-way valve has " inspection
Survey " and " use " two kinds of positions, correspondence detection methyl nitrite concentration and regular supply methyl nitrite, four-way valve during shutdown
It is maintained at " detection " position.
Brief description of the drawings
Fig. 1 is a kind of structural representation of device for continuously generating methyl nitrite of one embodiment of the present invention.
Specific embodiment
With reference to Figure of description, the present invention is described in more detail.
As shown in fig. 1, a kind of device for continuously generating methyl nitrite, including tubular reactor 1, located at pipe reaction
The heater 11 of the tube wall of device 1, the liquid tank 12 located at the bottom of tubular reactor 1, the cooler pan located at the upper end of tubular reactor 1
Pipe 13, methanol tank 2, NO tanks 3 and O2Tank 4, liquid tank 12 leads to cooling water or freezing liquid is cooled down, and heater 11 is heating
Stove, heating furnace is wrapped on the tube wall at the middle part of tubular reactor 1, and methanol tank 2 passes through pipeline communication in the top of tubular reactor 1,
The pipeline that methanol tank 2 is connected with tubular reactor 1 is provided with plunger metering pump 92, and plunger metering pump 92 can calculate methanol flow rate,
It is easy to control the flow velocity of methyl alcohol；NO tanks 3 and O2Tank 4 is by pipeline communication in the bottom of tubular reactor 1, NO tanks 3 and O2Tank 4 and pipe
The pipeline of the connection of formula reactor 1 is provided with mass flowmenter 91, mass flowmenter 91 and NO tanks 3 and O2N is respectively equipped between tank 42
Blow device 8, NO and O can be calculated by mass flowmenter 912Mass ratio, the amount ratio of the material of reaction is 4:1, N2 purging dress
Putting 8 can be purged to whole device and be carried out pressurize leak detection.
By pipeline communication in four-way valve 5, four-way valve 5 is respectively communicated with reaction unit 6, gas on the top of tubular reactor 1
Analyzer 7 and N2Blow device 8, four-way is entered in the gas cooled down through the cooling coil 13 on the top of tubular reactor 1 from pipeline
Valve 5, enters back into gas analyzer 7, and " use " state, supply response are switched to after concentration reaches prescribed concentration and keeps stabilization
Device 6 is used；Use N2The nitrogen of blow device 8 purging removes the methyl nitrite remained in gas analyzer 7, water and other height boilings
Point accessory substance flows into liquid tank 12, and liquid tank 12 is periodically discharged；Valve transfer is to " detection " state when out of service,
Termination of pumping and closing gas circuit main valve, open the N on air pipe2Blow device 8 carries out being purged through gas analyzer 7, four-way valve 5
State has " detection " and " use " two kinds of positions, and correspondence detection methyl nitrite concentration and regular supply methyl nitrite stop
Four-way valve 5 is maintained at " detection " position during machine.
The bottom of tubular reactor 1 can be by tapping valve fast evacuation tubular reactor under being provided with tapping valve 10, emergency case
In reactant.
Methyl nitrite is synthesized using gas phase synthesis method, its reaction equation is as follows：
4NO+O2+4CH3OH→4CH3ONO+2H2O
NO and O in reaction2The amount of material is 4 to 1, methyl alcohol excess, it is ensured that gas reacts completely, and methyl alcohol is except conduct
Reaction beyond the region of objective existence, also as the diluent of methyl nitrite.
Using gas phase synthesis method, reaction is simple, and accessory substance is few, and methyl nitrite is to produce to use, and without potential safety hazard, is obtained
Methyl nitrite purity is high, and can provide the methyl nitrite of constant level.
In above-mentioned, the methyl alcohol of plunger metering pump 92 sets flow velocity as 0.5-2mL/min, and mass flowmenter 91 is set as
NO：40-160mL/min、O2:10-40mL/min；The heating-up temperature of heating furnace：30-120 DEG C, the cooling temperature of cooling coil 13
Degree：0-10 DEG C, convenient production methyl nitrite raw material that is constant and understanding content.
The production of methyl nitrite such as following steps：N is first opened before reaction2Blow device 8, to tubular reactor 1 and first
Alcohol tank 2, NO tanks 3, O2Tank 4 and whole pipeline carry out nitrogen purging, and carry out pressurize detection, it is ensured that system it is safe and reliable；With
Plunger metering pump 92 sets methanol flow rate, in entering tubular reactor 1 above heating furnace, NO and O2Set with mass flowmenter 91
Enter from the bottom of tubular reactor 1 after being mixed after constant flow, enter in tubular reactor 1 and upward by the liquid tank 12 of bottom
With methyl alcohol haptoreaction, methyl nitrite and water are generated in methyl alcohol and the mixed gas reaction of the gasification of the middle part of tubular reactor 1, then
By cooling coil 13 cool down obtaining product.Production process is simple and convenient, pollution-free.
The form contrast of embodiment 1, embodiment 2, embodiment 3 and embodiment 4：
Contrasted from embodiment 1 and embodiment 2, in methyl alcohol, NO and O2Flow identical in the case of, reaction temperature is got over
High, chilling temperature is smaller, and the concentration of methyl nitrite is higher；
Contrasted from embodiment 2, embodiment 3 and embodiment 4, in NO and O2Flow it is identical, reaction temperature identical
In the case of, methanol flow is smaller, nitrous of the concentration ＞ chilling temperatures of chilling temperature control methyl nitrite at 5 DEG C at 10 DEG C
Concentration of the concentration ＞ chilling temperatures of sour methyl esters in 0 DEG C of methyl nitrite；
Contrasted from embodiment 1 and embodiment 4, NO and O2Flow it is identical, in the case of chilling temperature identical, methyl alcohol
Flow is lower, and reaction temperature is higher, and the concentration of methyl nitrite is higher.
It follows that methanol flow is in 0.6mL/min, NO flows are in 100mL/min, O2Flow is in 25mL/min, reaction
At 100 DEG C, at 5 DEG C, the concentration highest of methyl nitrite reaches 30% to chilling temperature to temperature.
A kind of device for continuously generating methyl nitrite provided by the present invention, simple structure, reaction is convenient；
Realize difference in functionality in the upper, middle and lower segment of a tubular reactor, between connectionless part, reduce leakage
Risk, carries out the purging of nitrogen before and after reaction, eliminate safe hidden trouble, and plunger metering pump, mass flowmenter are all by by computer
Control, realizes digitized regulation and accurate recording；
Realize methyl nitrite gas and produce consumption immediately immediately, it is to avoid quality uncertainty and peace that storage brings
Full hidden danger；
Liquid feedstock is accurately controlled by plunger metering pump, gas by mass flowmenter, is carried out instead in tubular reactor
Answer temperature control accurate, realize the stability and reappearance of gas supply；
Can be according to the actual requirements, there is provided the methyl nitrite gas of concentration accurate stable is used for CO synthesizing dimethyl oxalates
Catalyst developmental research, obtain extraordinary effect.
The above is only preferred embodiment of the invention, it is noted that to those skilled in the art, not
On the premise of departing from the invention design, some similar deformations and improvement can also be made, these also should be regarded as the present invention
Protection domain within.
Claims (8)
1. a kind of device for continuously generating methyl nitrite, it is characterised in that including tubular reactor (1), located at the tubular type
The heater (11) of reactor (1) tube wall, the liquid tank (12) located at the tubular reactor (1) bottom, located at the pipe
The cooling coil (13) of formula reactor (1) upper end, methanol tank (2), NO tanks (3) and O2Tank (4), the methanol tank (2) is by pipe
Road is communicated in the tubular reactor (1) top, the NO tanks (3) and the O2Tank (4) is by pipeline communication in the tubular type
Reactor (1) bottom, by pipeline communication in four-way valve (5), the four-way valve (5) is respectively on tubular reactor (1) top
It is communicated in reaction unit (6), gas analyzer (7) and N2Blow device (8).
2. a kind of device for continuously generating methyl nitrite according to claim 1, it is characterised in that the NO tanks (3)
With the O2The pipeline that tank (4) is connected with the tubular reactor (1) is provided with mass flowmenter (91), the mass flowmenter
(91) with the NO tanks (3) and the O2Tank is respectively equipped with N between (4)2Blow device (8).
3. a kind of device for continuously generating methyl nitrite according to claim 1, it is characterised in that the methanol tank
(2) pipeline connected with the tubular reactor (1) is provided with plunger metering pump (92), and the heater (11) is heating
Stove.
4. a kind of device for continuously generating methyl nitrite according to claim 1, it is characterised in that the pipe reaction
Device (1) bottom is provided with tapping valve (10).
5. using a kind of device production synthesis methyl nitrite gas for continuously generating methyl nitrite in claim 1-4
Method, it is characterised in that use gas phase synthesis method, reaction equation is as follows：
4NO+O2+4CH3OH→4CH3ONO+2H2O
NO and O in reaction2The amount of material is 4 to 1, methyl alcohol excess, it is ensured that gas reacts completely, and methyl alcohol is except as reaction
Beyond the region of objective existence, also as the diluent of methyl nitrite.
6. a kind of production using the device for continuously generating methyl nitrite according to claim 5 synthesizes methyl nitrite gas
Method, it is characterised in that such as following steps：N is first opened before reaction2Blow device (8), to tubular reactor (1) and methanol tank
(2), NO tanks (3), O2Tank (4) and whole pipeline carry out nitrogen purging, and carry out pressurize detection, it is ensured that system it is safe and reliable；
Methanol flow rate is set with plunger metering pump (92), in entering tubular reactor (1) above heating furnace, NO and O2Use mass flow
Enter from tubular reactor (1) bottom after being mixed after meter (91) setting flow, it is anti-to enter tubular type by the liquid tank (12) of bottom
Answer in device (1) and upwards with methyl alcohol haptoreaction, generated in methyl alcohol and the mixed gas reaction of the gasification of tubular reactor (1) middle part
Methyl nitrite and water, then cool down obtaining product by cooling coil (13).
7. a kind of production using the device for continuously generating methyl nitrite according to claim 6 synthesizes methyl nitrite gas
Method, it is characterised in that the methyl alcohol of the plunger metering pump (92) sets flow velocity as 0.5-2mL/min, the mass flowmenter
(91) setting NO：40-160mL/min、O2:10-40mL/min；The heating-up temperature of the heating furnace：It is 30-120 DEG C, described cold
But the chilling temperature of coil pipe (13)：0-10℃.
8. a kind of production using the device for continuously generating methyl nitrite according to claim 7 synthesizes methyl nitrite gas
Method, it is characterised in that enter four-way valve from pipeline in the gas cooled down through the cooling coil (13) on tubular reactor (1) top
(5) gas analyzer (7), is entered back into, " use " state is switched to after concentration reaches prescribed concentration and keeps stabilization, supply is anti-
Device (6) is answered to use；Use N2Blow device (8) nitrogen purging removes the methyl nitrite of residual in gas analyzer (7), water and
Other high boiling point by-products produced influent tanks (12), and liquid tank (12) is periodically discharged；Valve transfer when out of service
To " detection " state, termination of pumping and gas circuit main valve is closed, open the N on air pipe2Blow device (8) carries out being purged through gas point
Analyzer (7).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710245118.4A CN106883127B (en) | 2017-04-14 | 2017-04-14 | A kind of device continuously generating methyl nitrite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710245118.4A CN106883127B (en) | 2017-04-14 | 2017-04-14 | A kind of device continuously generating methyl nitrite |
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| CN106883127A true CN106883127A (en) | 2017-06-23 |
| CN106883127B CN106883127B (en) | 2019-03-05 |
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| CN201710245118.4A Active CN106883127B (en) | 2017-04-14 | 2017-04-14 | A kind of device continuously generating methyl nitrite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107793316A (en) * | 2017-12-05 | 2018-03-13 | 中国科学院大连化学物理研究所 | A kind of method of microreactor synthesis methyl nitrite |
| CN110818568A (en) * | 2018-08-07 | 2020-02-21 | 上海华谊能源化工有限公司 | Device for continuously producing methyl nitrite gas and application thereof |
| CN111377819A (en) * | 2018-12-28 | 2020-07-07 | 上海浦景化工技术股份有限公司 | Alkyl nitrite synthesis process and reactor |
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| CN102807492A (en) * | 2012-08-30 | 2012-12-05 | 安徽淮化股份有限公司 | Process device for producing methyl nitrite |
| CN103242166A (en) * | 2012-02-09 | 2013-08-14 | 中国科学院福建物质结构研究所 | Method for preparing methyl nitrite gas |
| CN105272859A (en) * | 2014-07-03 | 2016-01-27 | 中国石油化工股份有限公司 | Production method for alkyl nitrite |
| CN205347278U (en) * | 2015-12-30 | 2016-06-29 | 宁波金远东石化工程技术有限公司 | Synthetic methyl nitrite's device |
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2017
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242166A (en) * | 2012-02-09 | 2013-08-14 | 中国科学院福建物质结构研究所 | Method for preparing methyl nitrite gas |
| CN102807492A (en) * | 2012-08-30 | 2012-12-05 | 安徽淮化股份有限公司 | Process device for producing methyl nitrite |
| CN105272859A (en) * | 2014-07-03 | 2016-01-27 | 中国石油化工股份有限公司 | Production method for alkyl nitrite |
| CN205347278U (en) * | 2015-12-30 | 2016-06-29 | 宁波金远东石化工程技术有限公司 | Synthetic methyl nitrite's device |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107793316A (en) * | 2017-12-05 | 2018-03-13 | 中国科学院大连化学物理研究所 | A kind of method of microreactor synthesis methyl nitrite |
| CN107793316B (en) * | 2017-12-05 | 2020-04-07 | 中国科学院大连化学物理研究所 | Method for synthesizing methyl nitrite by microreactor |
| CN110818568A (en) * | 2018-08-07 | 2020-02-21 | 上海华谊能源化工有限公司 | Device for continuously producing methyl nitrite gas and application thereof |
| CN111377819A (en) * | 2018-12-28 | 2020-07-07 | 上海浦景化工技术股份有限公司 | Alkyl nitrite synthesis process and reactor |
| CN111377819B (en) * | 2018-12-28 | 2024-02-09 | 上海浦景化工技术股份有限公司 | Alkyl nitrite synthesis process and reactor |
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| CN106883127B (en) | 2019-03-05 |
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