CN106883127B - A kind of device continuously generating methyl nitrite - Google Patents
A kind of device continuously generating methyl nitrite Download PDFInfo
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- CN106883127B CN106883127B CN201710245118.4A CN201710245118A CN106883127B CN 106883127 B CN106883127 B CN 106883127B CN 201710245118 A CN201710245118 A CN 201710245118A CN 106883127 B CN106883127 B CN 106883127B
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- methyl nitrite
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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 discloses a kind of devices for continuously generating methyl nitrite, including tubular reactor, the heating device set on tubular reactor tube wall, the liquid tank set on tubular reactor bottom, the cooling coil set on tubular reactor upper end, methanol tank, NO tank and O2Tank, methanol tank are connected to tubular reactor top, NO tank and O by pipeline2Tank is connected to tubular reactor bottom by pipeline, and tubular reactor top is connected to four-way valve by pipeline, and four-way valve is respectively communicated in reaction unit, gas analyzer and N2Blow device.A kind of device continuously generating methyl nitrite provided by the present invention, structure is simple, and reaction is convenient；Different function is realized in the upper, middle and lower segment of a tubular reactor, is reduced the risk of leakage, is avoided storage bring quality uncertainty and security risk.
Description
Technical field
The present invention relates to chemical equipment technical fields, and in particular to a kind of device for continuously generating methyl nitrite.
Background technique
Methyl nitrite gas is O2Gaseous oxidation is coupled the unstripped gas of synthesizing dimethyl oxalate reaction, is studying the technique
Or when evaluation catalyst, it due to the property unstability of methyl nitrite gas, can not buy on the market, need voluntarily to make
It is standby.
Existing method is all to produce methyl nitrite gas by liquid-phase chemical reaction, is collected after storing with various methods
Slow release, which comes out, to be 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
Other than main reaction, nitric acid and nitrogen oxides for being formed there are also the decomposition of nitrous acid, disproportionation etc., the nitrous acid of synthesis
Methyl esters dissolution below freezing in methyl alcohol, methyl nitrite gas is released to 30-100 DEG C by heating reaction kettle when use
It is put into surge tank, it is clear that is released at this time is the mixing gas of methyl nitrite and methanol, wherein the content of methyl nitrite
It is influenced by factors such as original concentration, release temperature and pressure, and does not refer to this point in the patent.
It is higher to the accuracy and precision requirement of data due in evaluating catalyst and technical study, it is therefore desirable to
There is stable methyl nitrite raw material that is constant and knowing content.
And the reaction of the generation methyl nitrite of existing patented technology is all interval, to the methyl nitrite of offer
Purity does not also control effectively means, therefore has the following deficiencies:
1. reaction is complicated, by-product is more；
2. having the container or device of storage methyl nitrite, there are security risks；
3. methyl nitrite placement causes to decompose and other complicated side reactions cause raw material impurity content high；
4. constant and known content methyl nitrite cannot be provided.
Summary of the invention
It is an object of the invention to provide a kind of devices for continuously generating methyl nitrite, solve in above-mentioned prior art problem
One or more.
A kind of device continuously generating methyl nitrite according to the present invention, including tubular reactor, be set to the tubular type
The heating device of reactor tube walls, set on the liquid tank of the tubular reactor bottom, set on the tubular reactor upper end
Cooling coil, methanol tank, NO tank and O2Tank, the methanol tank are connected to the tubular reactor top, the NO by pipeline
Tank and the O2Tank is connected to the tubular reactor bottom by pipeline, and the tubular reactor top is connected to by pipeline
Four-way valve, the four-way valve are respectively communicated in reaction unit, gas analyzer and N2Blow device.
A kind of device continuously generating methyl nitrite provided by the present invention, structure is simple, and reaction is convenient；
Realize different function in the upper, middle and lower segment of tubular reactor, between connectionless part, reduce leakage
Risk, reaction front and back carry out the purging of nitrogen, eliminate safe hidden trouble, plunger metering pump, mass flowmenter are all by passing through computer
Digitized adjusting and accurate recording are realized in control；
It realizes methyl nitrite gas and generates instant consumption immediately, avoid storage bring quality uncertainty and peace
Full hidden danger；
Liquid feedstock is accurately controlled by plunger metering pump, gas by mass flowmenter, is carried out in tubular reactor anti-
It answers temperature control accurate, realizes the stability and reproducibility of gas supply；
The methyl nitrite gas of concentration accurate stable can according to actual needs, be provided for CO synthesizing dimethyl oxalate
Catalyst developmental research, obtain extraordinary effect.
In some embodiments, the NO tank and the O2The pipeline that tank is connected to the tubular reactor is equipped with matter
Measure flowmeter, the mass flowmenter and the NO tank and the O2N blow device is respectively equipped between tank.Pass through mass flow
Meter can calculate NO and O well2Mass ratio, N blow device can purge whole device and carry out pressure maintaining leak detection.
In some embodiments, the pipeline that the methanol tank is connected to the tubular reactor is measured equipped with plunger
Pump, the heating device are 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 equipped with tapping valve.Tapping valve can be passed through 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 substance is 4 to 1, and methanol is excessive, it is ensured that gas reacts completely, and methanol is in addition to conduct
Outside reactant, also as the diluent of methyl nitrite.
Using gas phase synthesis method, reaction is simple, and by-product is few, and methyl nitrite is produced and used, and no security risk obtains
Methyl nitrite purity is high, and the methyl nitrite of constant level can be provided.
In some embodiments, such as following steps: N2 blow device is first opened before reaction, to tubular reactor and first
Alcohol tank, NO tank, O2Tank and entire pipeline carry out nitrogen purging, and carry out pressure maintaining detection, it is ensured that system it is safe and reliable；Use plunger
Metering pump sets methanol flow rate, enters in tubular reactor above heating furnace, NO and O2After setting flow with mass flowmenter
Enter after mixing from tubular reactor bottom, is entered by the liquid tank of bottom and contacted instead in tubular reactor and upwards with methanol
It answers, the methanol to gasify in the middle part of tubular reactor and mixed gas reaction generate methyl nitrite and water, then pass through cooling coil
It is cooled down to obtain product.Production process is simple and convenient, pollution-free.
In some embodiments, the methanol of the plunger metering pump sets flow velocity as 0.5-2mL/min, the quality stream
Setting NO:40-160mL/min, O of meter2:10-40mL/min；The heating temperature of the heating furnace: 30-120 DEG C, described cold
But the cooling temperature of coil pipe: 0-10 DEG C.Facilitate production methyl nitrite raw material that is constant and knowing content.
In some embodiments, enter four-way from pipeline in the cooling gas of the cooling coil through 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 stablizing
Set use；Use N2Blow device nitrogen purging removes remaining methyl nitrite, water and other higher boiling pairs in gas analyzer
Product flows into liquid tank, and is periodically discharged to liquid tank；Valve transfer is to " detection " state, termination of pumping and pass when out of service
It holds one's breath road main valve, opens the N on air pipe2Blow device carries out being purged through gas analyzer.The state of four-way valve has " inspection
Survey " and " uses " two kinds of positions, correspondence detects methyl nitrite concentration and regular supply methyl nitrite, four-way valve when shutdown
It is maintained at " detection " position.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of device for continuously generating methyl nitrite of one embodiment of the present invention.
Specific embodiment
With reference to the accompanying drawings of the specification, the present invention is described in more detail.
As shown in fig. 1, a kind of device continuously generating methyl nitrite, including tubular reactor 1, be set to pipe reaction
The heating device 11 of 1 tube wall of device, the liquid tank 12 set on 1 bottom of tubular reactor, the cooler pan set on 1 upper end of tubular reactor
Pipe 13, methanol tank 2, NO tank 3 and O2Tank 4, liquid tank 12 leads to cooling water or freezing liquid is cooled down, and heating device 11 is heating
Furnace, heating furnace are wrapped on the tube wall at 1 middle part of tubular reactor, and methanol tank 2 is connected to 1 top of tubular reactor by pipeline,
The pipeline that methanol tank 2 is connected to tubular reactor 1 is equipped with plunger metering pump 92, and plunger metering pump 92 can calculate methanol flow rate,
Convenient for controlling the flow velocity of methanol；NO tank 3 and O2Tank 4 is connected to 1 bottom of tubular reactor, NO tank 3 and O by pipeline2Tank 4 and pipe
The pipeline that formula reactor 1 is connected to is equipped with mass flowmenter 91, mass flowmenter 91 and NO tank 3 and O2N is respectively equipped between tank 42
Blow device 8 can calculate NO and O by mass flowmenter 912Mass ratio, the mass ratio of the material of reaction is 4:1, N2 purging dress
Whole device can be purged and carry out pressure maintaining leak detection by setting 8.
1 top of tubular reactor is connected to four-way valve 5 by pipeline, and four-way valve 5 is respectively communicated in reaction unit 6, gas
Analyzer 7 and N2Blow device 8 enters four-way from pipeline in the cooling gas of the cooling coil 13 through 1 top of tubular reactor
Valve 5 enters back into gas analyzer 7, switches to " use " state, supply response after concentration reaches prescribed concentration and keeps stablizing
Device 6 uses；Use N28 nitrogen of blow device purging removes remaining methyl nitrite in gas analyzer 7, water and other high boiling
Point by-product flows into liquid tank 12, and is periodically discharged to liquid tank 12；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, corresponding detection methyl nitrite concentration and regular supply methyl nitrite, stops
Four-way valve 5 is maintained at " detection " position when machine.
1 bottom of tubular reactor is equipped with tapping valve 10, can pass through tapping valve fast evacuation tubular reactor under emergency case
In reactant.
Methyl nitrite is synthesized using gas phase synthesis method, reaction equation is as follows:
4NO+O2+4CH3OH→4CH3ONO+2H2O
NO and O in reaction2The amount of substance is 4 to 1, and methanol is excessive, it is ensured that gas reacts completely, and methanol is in addition to conduct
Outside reactant, also as the diluent of methyl nitrite.
Using gas phase synthesis method, reaction is simple, and by-product is few, and methyl nitrite is produced and used, and no security risk obtains
Methyl nitrite purity is high, and the methyl nitrite of constant level can be provided.
Among the above, the methanol 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 temperature of heating furnace: 30-120 DEG C, the cooling temperature of cooling coil 13
Degree: 0-10 DEG C, facilitate production methyl nitrite raw material that is constant and knowing 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 tank 3, O2Tank 4 and entire pipeline carry out nitrogen purging, and carry out pressure maintaining detection, it is ensured that system it is safe and reliable；With
Plunger metering pump 92 sets methanol flow rate, enters in tubular reactor 1 above heating furnace, NO and O2It is set with mass flowmenter 91
Enter after being mixed after constant flow from 1 bottom of tubular reactor, is entered by the liquid tank 12 of bottom in tubular reactor 1 and upward
With methanol haptoreaction, the methanol to gasify in the middle part of tubular reactor 1 and mixed gas reaction generate methyl nitrite and water, then
It is cooled down to obtain product by cooling coil 13.Production process is simple and convenient, pollution-free.
The table comparison of embodiment 1, embodiment 2, embodiment 3 and embodiment 4:
By embodiment 1 and the comparison of embodiment 2 it is found that in methanol, NO and O2The identical situation of flow under, reaction temperature is got over
Height, cooling temperature are smaller, and the concentration of methyl nitrite is higher；
It is compared by embodiment 2, embodiment 3 and embodiment 4 it is found that in NO and O2Flow it is identical, reaction temperature is identical
In the case of, methanol flow is smaller, cooling temperature controls nitrous of the concentration > cooling temperature of the methyl nitrite at 5 DEG C at 10 DEG C
Concentration of the concentration > cooling temperature of sour methyl esters in 0 DEG C of methyl nitrite；
By embodiment 1 and the comparison of embodiment 4 it is found that NO and O2Flow it is identical, in the identical situation of cooling temperature, methanol
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 flow is in 100mL/min, O2Flow is in 25mL/min, reaction
Temperature is at 100 DEG C, and for cooling temperature at 5 DEG C, the concentration highest of methyl nitrite reaches 30%.
A kind of device continuously generating methyl nitrite provided by the present invention, structure is simple, and reaction is convenient；
Realize different function in the upper, middle and lower segment of tubular reactor, between connectionless part, reduce leakage
Risk, reaction front and back carry out the purging of nitrogen, eliminate safe hidden trouble, plunger metering pump, mass flowmenter are all by passing through computer
Digitized adjusting and accurate recording are realized in control；
It realizes methyl nitrite gas and generates instant consumption immediately, avoid storage bring quality uncertainty and peace
Full hidden danger；
Liquid feedstock is accurately controlled by plunger metering pump, gas by mass flowmenter, is carried out in tubular reactor anti-
It answers temperature control accurate, realizes the stability and reproducibility of gas supply；
The methyl nitrite gas of concentration accurate stable can according to actual needs, be provided for CO synthesizing dimethyl oxalate
Catalyst developmental research, obtain extraordinary effect.
The above is only preferred embodiment of the invention, it is noted that those skilled in the art, not
Under the premise of being detached from the invention design, some similar deformation and improvement can be made, these also should be regarded as the present invention
Protection scope within.
Claims (8)
1. a kind of device for continuously generating methyl nitrite, which is characterized in that including tubular reactor (1), be set to the tubular type
The heating device (11) of reactor (1) tube wall, is set to the pipe at the liquid tank (12) for being set to the tubular reactor (1) bottom
The cooling coil (13), methanol tank (2), NO tank (3) and O of formula reactor (1) upper end2Tank (4), the methanol tank (2) pass through pipe
Road is connected to the tubular reactor (1) top, the NO tank (3) and the O2Tank (4) is connected to the tubular type by pipeline
Reactor (1) bottom, tubular reactor (1) top are connected to four-way valve (5) by pipeline, and the four-way valve (5) is respectively
It is connected to reaction unit (6), gas analyzer (7) and N2Blow device (8).
2. a kind of device for continuously generating methyl nitrite according to claim 1, which is characterized in that the NO tank (3)
With the O2The pipeline that tank (4) is connected to the tubular reactor (1) is equipped with mass flowmenter (91), the mass flowmenter
(91) with the NO tank (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, which is characterized in that the methanol tank
(2) pipeline being connected to the tubular reactor (1) is equipped with plunger metering pump (92), and the heating device (11) is heating
Furnace.
4. a kind of device for continuously generating methyl nitrite according to claim 1, which is characterized in that the pipe reaction
Device (1) bottom is equipped with tapping valve (10).
5. continuously generating the device production synthesis methyl nitrite gas of methyl nitrite using one of claim 1-4
Method, which is characterized in that use gas phase synthesis method, reaction equation is as follows:
4NO+O2+4CH3OH→4CH3ONO+2H2O
NO and O in reaction2The amount of substance is 4 to 1, and methanol is excessive, it is ensured that gas reacts completely, and methanol is in addition to as reaction
Beyond the region of objective existence, also as the diluent of methyl nitrite.
6. a kind of utilization according to claim 5 continuously generates the device production synthesis methyl nitrite gas of methyl nitrite
Method, which is characterized in that such as following steps: N is first opened before reaction2Blow device (8), to tubular reactor (1) and methanol tank
(2), NO tank (3), O2Tank (4) and entire pipeline carry out nitrogen purging, and carry out pressure maintaining detection, it is ensured that system it is safe and reliable；
Methanol flow rate is set with plunger metering pump (92), is entered in tubular reactor (1) above heating furnace, NO and O2Use mass flow
Enter after being mixed after meter (91) setting flow from tubular reactor (1) bottom, it is anti-to enter tubular type by the liquid tank (12) of bottom
It answers in device (1) and upwards with methanol haptoreaction, the methanol and mixed gas reaction to gasify in the middle part of tubular reactor (1) generates
Methyl nitrite and water, then cooled down to obtain product by cooling coil (13).
7. a kind of utilization according to claim 6 continuously generates the device production synthesis methyl nitrite gas of methyl nitrite
Method, which is characterized in that the methanol 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 temperature of the heating furnace: 30-120 DEG C, described cold
But the cooling temperature of coil pipe (13): 0-10 DEG C.
8. a kind of utilization according to claim 7 continuously generates the device production synthesis methyl nitrite gas of methyl nitrite
Method, which is characterized in that enter four-way valve from pipeline in the cooling gas of the cooling coil (13) through tubular reactor (1) top
(5), gas analyzer (7) are entered back into, " use " state is switched to after concentration reaches prescribed concentration and keeps stablizing, supply is anti-
Device (6) are answered to use；Use N2Blow device (8) nitrogen purging remove gas analyzer (7) in remaining methyl nitrite, 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 closing gas circuit main valve open the N on air pipe2Blow device (8) carries out being purged through gas point
Analyzer (7).
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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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| 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 CN106883127A (en) | 2017-06-23 |
| CN106883127B true CN106883127B (en) | 2019-03-05 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2017
- 2017-04-14 CN CN201710245118.4A patent/CN106883127B/en active Active
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 |
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