CN207525169U - A kind of reactor of continuous production nitromethane - Google Patents
A kind of reactor of continuous production nitromethane Download PDFInfo
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- CN207525169U CN207525169U CN201721183480.5U CN201721183480U CN207525169U CN 207525169 U CN207525169 U CN 207525169U CN 201721183480 U CN201721183480 U CN 201721183480U CN 207525169 U CN207525169 U CN 207525169U
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Abstract
The utility model provides a kind of reactor of continuous production nitromethane, includes the reaction zone of n series connection, wherein, reaction zone one includes：Housing, the mixing chamber being arranged in the housing and the reaction tube being connect with the mixing chamber, the reacting product outlet for the sodium nitrite import being connect with the mixing chamber and dimethyl suflfate import are provided on the housing, connecting with the reaction tube and move thermal medium inlet and outlet；Each reaction zone of reaction zone two to reaction zone n each include：Housing, the mixing chamber being arranged in the housing and the reaction tube being connect with the mixing chamber are provided with the import for the upper reaction zone reaction product being connect with the mixing chamber on the housing and dimethyl suflfate import, the reacting product outlet that is connect with the reaction tube and move thermal medium inlet and outlet；The reacting product outlet of other reaction zones in addition to the last one reaction zone is connected with the reaction product import of next reaction zone by pipeline.
Description
Technical field
The utility model is related to a kind of reactors of continuous production nitromethane.
Background technology
Nitromethane is simplest aliphatic nitro compound.Hydrogen on methyl is quite living due to being influenced by nitro
It sprinkles, therefore has a wide range of applications in field of fine chemical.In recent years, market demand increases, and export volume increases year by year.At present
There are mainly two types of the methods of domestic production nitromethane：One kind is methane gas phase nitrification process, nitric acid is gasified and (natural with methane
Gas) it mixes in proportion, it is directly nitrified under the conditions of 450~550 DEG C of normal pressure in the reactor.It is condensed again, absorb, slightly evaporate, rectifying
Obtain finished product；Another method is dimethyl suflfate nitroso method of substitution：Replace by dimethyl suflfate and sodium nitrite, slightly evaporate,
Rectifying is made.
The raw materials used methane of first method (natural gas) is inflammable and explosive, is unfavorable for keeping the safety in production, and side reaction is more, and product is pure
Low, high energy consumption is spent, it is of high cost.The second way is simple with technological operation, and raw material is easy to get, and production cost is low, is easy to industrialize
The features such as production, belongs to nitromethane production technology commonly used at present.But the reaction belongs to strongly exothermic reversible reaction：
The progress that temperature is conducive to synthetic reaction is reduced, but temperature is low, reaction rate is small, and the reaction time is long；Reaction temperature is improved, again
Back reaction is promoted to increase, raw material is also decomposed.So the current mode of production is mostly used in batch reactor, to nitrous
The method that dimethyl suflfate is slowly added dropwise in sour sodium prepares nitromethane, with heat-flash effect caused by control reaction.The preparation
Method yield is low, generally 50%~55%；Easily generation by-product-methyl nitrite；Batch Process can not realize scale
Industrial production.
Utility model content
The utility model, which is directed to strongly exothermic effect in dimethyl suflfate method of substitution, to be caused side reaction, product purity easily occurs
Technical disadvantages low, yield is low provide a kind of reactor and method of continuous production nitromethane.The reactor and method
While continuous production nitromethane is realized, the generation of side reaction can be effectively controlled, promotes the effecting reaction of product, is improved
Product yield and product purity.
Specifically, the utility model is related to：
(1) a kind of reactor of continuous production nitromethane, which is characterized in that the reactor is connected anti-including n
Area is answered, wherein,
Reaction zone one includes：Housing, the mixing chamber being arranged in the housing and the reaction tube being connect with the mixing chamber, it is described
It is provided with the sodium nitrite import being connect with the mixing chamber and dimethyl suflfate import on housing, connect with the reaction tube
Reacting product outlet and shifting thermal medium inlet and outlet；
Each reaction zone of reaction zone two to reaction zone n each include：Housing, the mixing chamber being arranged in the housing and with
The reaction tube of mixing chamber connection is provided with the upper reaction zone reaction product that is connect with the mixing chamber on the housing
Import and dimethyl suflfate import, the reacting product outlet being connect with the reaction tube and move thermal medium inlet and outlet；
The reacting product outlet of other reaction zones and reacting for next reaction zone in addition to the last one reaction zone
Product inlet is connected by pipeline.
(2) reactor described in above-mentioned (1), which is characterized in that the dimethyl suflfate inlet pipeline end is equipped with level
Round single layer coil tube is placed with multiple mixed flow nozzles on the coil pipe, dimethyl suflfate is sprayed into mixing chamber by the mixed flow nozzle,
The mixed flow nozzle is 200~600mm from mixing chamber distance from bottom.
(3) reactor described in above-mentioned (1) or (2), which is characterized in that n reaction zone is in integrally straight structure.
(4) reactor in above-mentioned (1) to (3) described in any one, which is characterized in that the reaction tube uses coiled
Structure, interior outer wrap number is 1~3 layer to coil pipe in the housing.
(5) reactor in above-mentioned (1) to (4) described in any one, which is characterized in that the mixing chamber is cylinder,
Ratio of height to diameter is 4~6:3.
(6) reactor in above-mentioned (1) to (5) described in any one, which is characterized in that the sodium nitrite import is with mixing
The side lower end for closing room is connected by pipeline, and dimethyl suflfate inlet pipeline is stretched into from the bottom centre of mixing chamber, mixing chamber
Outlet be 180 ° above the side of mixing chamber, and with side import horizontal direction angle.
(7) method of continuous production nitromethane, which is characterized in that use any one institute in above-mentioned (1) to (6)
Sodium nitrite solution is continuously passed through the mixing chamber of reaction zone one by the reactor stated from the sodium nitrite import of reaction zone one first
In, dimethyl suflfate import of the dimethyl suflfate respectively by each reaction zone by the way of multistage feeding continuously enters each reaction
The mixing chamber in area, the reactor are persistently kept the temperature at the reaction temperatures by moving thermal medium.
(8) method described in above-mentioned (7), wherein reactant dimethyl suflfate are fed using 5 segmentations, that is, the reactor
Include the reaction zone of 5 series connection.
(9) the combined feed molar ratio of the method described in above-mentioned (7) or (8), wherein dimethyl suflfate and sodium nitrite is 1~
5:1。
(10) method in above-mentioned (7) to (9) described in any one, wherein, the dimethyl suflfate inlet amount of reaction zone one
It is the 25%~60% of dimethyl suflfate total feed, the dimethyl suflfate inlet amount of reaction zone two is dimethyl suflfate combined feed
The 20%~50% of amount, the dimethyl suflfate inlet amount of reaction zone three are the 15%~40% of dimethyl suflfate total feed, instead
The dimethyl suflfate inlet amount for answering area four is the 10%~30% of dimethyl suflfate total feed, the dimethyl suflfate of reaction zone five
Inlet amount is the 5%~20% of dimethyl suflfate total feed.
Description of the drawings
Fig. 1 is the structural representation of one of the preferred embodiment of reactor of the utility model continuous production nitromethane
Figure.
1-reaction zone, one housing, the import of 2-sodium nitrite, the import of 3-dimethyl suflfate, 4-mixed flow nozzle, 5-mixed
Close room, 6-reaction interface tube, the reactant exit of 7-reaction zone one, the reaction-ure inlet of 8-reaction zone two, 9-reaction zone
Two reactant exit, the reaction-ure inlet of 10-reaction zone three, the reactant exit of 11-reaction zone three, 12-reaction zone four
Reaction-ure inlet, the reactant exit of 13-reaction zone four, five reaction-ure inlets of 14-reaction zone, 15-reaction product goes out
Mouthful, 16-shifting thermal medium inlet, 17-shifting thermal medium outlet, 18-blind flange.
Fig. 2 is the round single layer coil tube of level of dimethyl suflfate inlet pipeline end and the partial enlargement of multiple mixed flow nozzles
A in schematic diagram, wherein Fig. 2 is vertical view, and the B in Fig. 2 is front view.
Specific embodiment
In the utility model, the reaction zone number n for forming reactor is preferably 2~6, particularly preferably 5.The n
A reaction zone is connected between more preferable adjacent reaction area preferably integrally in straight structure with flange, particularly preferably with blind flange.
Reaction zone each in this way is independently, can flexibly to locate according to the size of processing inventory come the quantity in on-off reaction area
Reason.
In the utility model reactor, horizontal round single layer coil tube is preferably housed in dimethyl suflfate inlet pipeline end,
And multiple mixed flow nozzles are set on the coil pipe.By the mixed flow nozzle, dimethyl suflfate moment in reactor uniformly disperses,
Reach Quick uniform with sodium nitrite solution to mix, achieve the effect that strengthen mass transfer.
In a preferred embodiment, the number of the mixed flow nozzle is 1~6, and mixed flow nozzle can be conventional literary mound
In nozzle or this kind of nozzle modified version.The reactor of the utility model is both provided with moving the disengaging of thermal medium in each reaction zone
Mouthful, it is possible thereby to which controlling the temperature of each reaction zone keeps flexibility.If the heat dissipation effect for moving thermal medium is good, temperature can be with
It controls well, then each reaction zone can be used in series same shifting thermal medium；If a certain reaction zone temperature is more difficult to control, rise
It is warm very fast, individually the shiftings thermal medium in the area can be passed through it is new, to realize preferable shifting thermal effect.
In a preferred embodiment, the shifting thermal medium is distributed in the space outside entire reaction tube, it is preferable to use water is made
To move thermal medium.
In the utility model, the temperature range of the reaction process is preferably 20~100 DEG C, more preferably 40~70 DEG C.
In the utility model, the synthesising reacting time ranges preferably from 1~10 h, more preferably 1~3h.
The continuous production of nitromethane can be realized by the utility model, and effectively controls the fuel factor of reaction,
Inhibit the generation of side reaction.It is highly preferred that the moment that reactant is realized by mixed flow nozzle feed inlet uniformly disperses, mixes,
So as to efficient fast reaction.Fast compared to conventional method reaction speed, the reaction time is short, good product selectivity, and yield is good, reduces
Production cost is suitble to the industrial production of scale.
The utility model is further illustrated referring to embodiment, it should be understood that these embodiments are only used for
Illustrative explanation, is not the limitation to the utility model.It is new to this practicality in the range of the utility model purport is not departed from
Any modification that type carries out is each fallen in the range of the requires of the utility model protection.
Embodiment 1
Sodium nitrite in aqueous solution is continuously passed through by injection port 2, and dimethyl suflfate is passed through by the injection port 3 of reaction zone one
It crosses mixed flow nozzle 4 and is injected into mixing chamber 5 and mixed with sodium nitrite solution (feed zone n=1), dimethyl suflfate and sodium nitrite
Molar ratio is 2:1.Two kinds of materials realize quick, uniformly mixing under the action of mixed flow nozzle in mixing chamber, subsequently into 6 phases
The reaction tube of connection carries out highly effective reaction.During reaction, cooling is realized by moving thermal medium inlet 16 and moving thermal medium outlet 17
The cycle of water removes the reaction heat that reaction generates, and reaction solution is made to continue heat preservation at 60 DEG C.After reaction, reaction product passes through
Outlet 7 is delivered continuously subsequent separation workshop and carries out refined purification, obtains nitromethane product.Product yield 56% is pure
Degree 97.5%.
Embodiment 2
Sodium nitrite in aqueous solution is continuously passed through by injection port 2, and the dimethyl suflfate of 50% mass passes through reaction zone one
Injection port 3 be injected into mixing chamber 5 by mixed flow nozzle 4 and mixed with sodium nitrite solution (feed zone n=2), dimethyl suflfate
Total amount and the molar ratio of sodium nitrite are 2:1.Two kinds of materials are realized quick, uniformly mixed under the action of mixed flow nozzle in mixing chamber
It closes, highly effective reaction is carried out subsequently into the reaction tube being connected with 6.Following reaction liquid leaves reaction zone one, and lead to by outlet 7
It crosses entrance 8 and enters reaction zone two, in mixing chamber 5 and the dimethyl suflfate being injected into from import 3 and by mixed flow nozzle 4
(50% mass) is quickly mixed, and highly effective reaction is carried out subsequently into the reaction tube being connected with 6.During reaction, lead to respectively
It crosses the shifting thermal medium inlet 16 of reaction zone one and reaction zone two and moves the cycle that cooling water is realized in the series connection of thermal medium outlet 17, remove
The reaction heat generated is reacted, reaction solution is made to continue heat preservation at 60 DEG C.After reaction, reaction product is by exporting 9 by continuous defeated
It is sent to subsequent separation workshop and carries out refined purification, obtain nitromethane product.Product yield 60%, purity 97.5%.
Embodiment 3
Sodium nitrite in aqueous solution is continuously passed through by injection port 2, and the dimethyl suflfate of 30% mass passes through reaction zone one
Injection port 3 be injected into mixing chamber 5 by mixed flow nozzle 4 and mixed with sodium nitrite solution (feed zone n=3), dimethyl suflfate
Total amount and the molar ratio of sodium nitrite are 2:1.Two kinds of materials are realized quick, uniformly mixed under the action of mixed flow nozzle in mixing chamber
It closes, highly effective reaction is carried out subsequently into the reaction tube being connected with 6.Following reaction liquid leaves reaction zone one, and lead to by outlet 7
It crosses import 8 and enters reaction zone two, in mixing chamber 5 and the dimethyl suflfate being injected into from import 3 and by mixed flow nozzle 4
(30% mass) is quickly mixed, and highly effective reaction is carried out subsequently into the reaction tube being connected with 6.Following reaction liquid passes through
Reaction zone two is left in outlet 9, and passes through import 10 and enter reaction zone three, in mixing chamber 5 with coming from import 3 and by mixed flow nozzle
4 dimethyl suflfates being injected into (40% mass) are quickly mixed, and are carried out subsequently into the reaction tube being connected with 6 efficiently anti-
It should.During reaction, pass through the shifting thermal medium inlet 16 of reaction zone one, reaction zone two and reaction zone three and shifting thermal medium outlet respectively
The cycle of cooling water is realized in 17 series connection, removes the reaction heat that reaction generates, and reaction solution is made to continue heat preservation at 60 DEG C.Reaction terminates
Afterwards, reactant is delivered continuously subsequent separation workshop by outlet 11 and carries out refined purification, obtains nitromethane product.
Product yield 65%, purity 98.1%.
Embodiment 4
Sodium nitrite in aqueous solution is continuously passed through by injection port 2, and the dimethyl suflfate of 20% mass passes through reaction zone one
Injection port 3 be injected into mixing chamber 5 by mixed flow nozzle 4 and mixed with sodium nitrite solution (feed zone n=4), dimethyl suflfate
Total amount and the molar ratio of sodium nitrite are 2:1.Two kinds of materials are realized quick, uniformly mixed under the action of mixed flow nozzle in mixing chamber
It closes, highly effective reaction is carried out subsequently into the reaction tube being connected with 6.Following reaction liquid leaves reaction zone one, and lead to by outlet 7
It crosses import 8 and enters reaction zone two, in mixing chamber 5 and the dimethyl suflfate being injected into from import 3 and by mixed flow nozzle 4
(20% mass) is quickly mixed, and highly effective reaction is carried out subsequently into the reaction tube being connected with 6.Then reaction solution passes through
Reaction zone two is left in outlet 9, and passes through import 10 and enter reaction zone three, in mixing chamber 5 with coming from import 3 and by mixed flow nozzle
4 dimethyl suflfates being injected into (30% mass) are quickly mixed, and are carried out subsequently into the reaction tube being connected with 6 efficiently anti-
It should.Following reaction liquid leaves reaction zone three by outlet 11, and passes through import 12 and enter reaction zone four, in mixing chamber 5 with coming from
Import 3 is simultaneously quickly mixed by the dimethyl suflfate (30% mass) that mixed flow nozzle 4 is injected into, and is connected subsequently into 6
The reaction tube connect carries out highly effective reaction.During reaction, pass through reaction zone one, reaction zone two, reaction zone three and reaction zone four respectively
Shifting thermal medium inlet 16 and move thermal medium outlet 17 series connection realize cooling water cycle, remove reaction generate reaction heat, make
Reaction solution is persistently kept the temperature at 60 DEG C.After reaction, reactant by outlet 13 be delivered continuously it is subsequent separation workshop into
The refined purification of row, obtains nitromethane product.Product yield 69%, purity 99.4%.
Embodiment 5
Sodium nitrite in aqueous solution is continuously passed through by injection port 2, and the dimethyl suflfate of 20% mass passes through reaction zone one
Injection port 3 be injected into mixing chamber 5 by mixed flow nozzle 4 and mixed with sodium nitrite solution (feed zone n=5), dimethyl suflfate
Total amount and the molar ratio of sodium nitrite are 2:1.Two kinds of materials are realized quick, uniformly mixed under the action of mixed flow nozzle in mixing chamber
It closes, highly effective reaction is carried out subsequently into the reaction tube being connected with 6.Following reaction liquid leaves reaction zone one, and lead to by outlet 7
It crosses import 8 and enters reaction zone two, in mixing chamber 5 and the dimethyl suflfate being injected into from import 3 and by mixed flow nozzle 4
(20% mass) is quickly mixed, and highly effective reaction is carried out subsequently into the reaction tube being connected with 6.Following reaction liquid passes through
Reaction zone two is left in outlet 9, and passes through import 10 and enter reaction zone three, in mixing chamber 5 with coming from import 3 and by mixed flow nozzle
4 dimethyl suflfates being injected into (20% mass) are quickly mixed, and are carried out subsequently into the reaction tube being connected with 6 efficiently anti-
It should.Following reaction liquid leaves reaction zone three by outlet 11, and passes through import 12 and enter reaction zone four, in mixing chamber 5 with coming from
Import 3 is simultaneously quickly mixed by the dimethyl suflfate (20% mass) that mixed flow nozzle 4 is injected into, and is connected subsequently into 6
The reaction tube connect carries out highly effective reaction.Following reaction liquid leaves reaction zone four by outlet 13, and passes through import 14 and enter reaction
Area five, in mixing chamber 5 with being carried out quickly from import 3 and by the dimethyl suflfate (20% mass) that mixed flow nozzle 4 is injected into
Mixing carries out highly effective reaction subsequently into the reaction tube being connected with 6.During reaction, pass through reaction zone one, reaction zone respectively
2nd, cooling water is realized in the shifting thermal medium inlet 16 of reaction zone three, reaction zone four and reaction zone five and the shifting series connection of thermal medium outlet 17
Cycle, remove reaction generate reaction heat, make reaction solution continue heat preservation at 60 DEG C.After reaction, reactant passes through outlet
15, which are delivered continuously subsequent separation workshop, carries out refined purification, obtains nitromethane product.Product yield 75%, purity
99.9%.
Claims (9)
1. a kind of reactor of continuous production nitromethane, which is characterized in that the reactor includes the reaction zone of n series connection,
Wherein,
Reaction zone one includes：Housing, the mixing chamber being arranged in the housing and the reaction tube being connect with the mixing chamber, the housing
On the reaction that is provided with the sodium nitrite import being connect with the mixing chamber and dimethyl suflfate import, is connect with the reaction tube
Product exit and shifting thermal medium inlet and outlet；
Each reaction zone of reaction zone two to reaction zone n each include：Housing, the mixing chamber being arranged in the housing and mixed with this
The reaction tube of room connection is closed, the import of a upper reaction zone reaction product being connect with the mixing chamber is provided on the housing
The reacting product outlet and shifting thermal medium inlet that are connect with dimethyl suflfate import, with the reaction tube and outlet；
The reacting product outlet of other reaction zones in addition to the last one reaction zone and the reaction product of next reaction zone
Import is connected by pipeline；
N is 2~6.
2. reactor according to claim 1, which is characterized in that the dimethyl suflfate inlet pipeline end is equipped with level
Round single layer coil tube is placed with multiple mixed flow nozzles on the coil pipe, dimethyl suflfate is sprayed into mixing chamber by the mixed flow nozzle,
The mixed flow nozzle is 200~600m from mixing chamber distance from bottom.
3. reactor according to claim 1 or 2, which is characterized in that n reaction zone is adjacent integrally in straight structure
Flanged joint is used between reaction zone.
4. reactor according to claim 1 or 2, which is characterized in that the reaction tube uses coiled structure, and coil pipe exists
Interior outer wrap number is 1~3 layer in housing.
5. reactor according to claim 1 or 2, which is characterized in that the mixing chamber is cylinder, ratio of height to diameter for 4~
6:3。
6. reactor according to claim 1 or claim 2, which is characterized in that under the side of the sodium nitrite import and mixing chamber
End is connected by pipeline, and dimethyl suflfate inlet pipeline is stretched into from the bottom centre of mixing chamber, and the outlet of mixing chamber is mixing
Above the side of room, and it is 180 ° with side import horizontal direction angle.
7. reactor according to claim 2, the number of mixed flow nozzle described in a reaction zone is 1~6.
8. reactor according to claim 2, modified version of the mixed flow nozzle for Venturi nozzle or Venturi nozzle.
9. reactor according to claim 3, the flange is blind flange.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721183480.5U CN207525169U (en) | 2017-09-14 | 2017-09-14 | A kind of reactor of continuous production nitromethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721183480.5U CN207525169U (en) | 2017-09-14 | 2017-09-14 | A kind of reactor of continuous production nitromethane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN207525169U true CN207525169U (en) | 2018-06-22 |
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ID=62568575
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201721183480.5U Active CN207525169U (en) | 2017-09-14 | 2017-09-14 | A kind of reactor of continuous production nitromethane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN207525169U (en) |
-
2017
- 2017-09-14 CN CN201721183480.5U patent/CN207525169U/en active Active
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| Date | Code | Title | Description |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20191219 Address after: 100084, room 6, building 8, building 1, Zhongguancun East Road, Haidian District, Beijing, Patentee after: Beijing Chemical Reaction Engineering Science AND Technology Co., Ltd. Address before: 100084, room 6, building 8, building 1, Zhongguancun East Road, Haidian District, Beijing, Co-patentee before: Shandong rui'ao Mstar Technology Ltd Patentee before: Beijing Chemical Reaction Engineering Science AND Technology Co., Ltd. |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: A reactor for continuous production of nitromethane Effective date of registration: 20210727 Granted publication date: 20180622 Pledgee: Haihua International Financial Leasing Co.,Ltd. Pledgor: BEIJING CHEMICAL REACTION ENGINEERING SCIENCE & TECHNOLOGY Co.,Ltd. Registration number: Y2021990000651 |