CN205275494U - Automatic system takes place for methyl nitrite - Google Patents
Automatic system takes place for methyl nitrite Download PDFInfo
- Publication number
- CN205275494U CN205275494U CN201521084388.4U CN201521084388U CN205275494U CN 205275494 U CN205275494 U CN 205275494U CN 201521084388 U CN201521084388 U CN 201521084388U CN 205275494 U CN205275494 U CN 205275494U
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- CN
- China
- Prior art keywords
- methyl nitrite
- storage device
- reaction vessel
- generation systems
- automatic
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- BLLFVUPNHCTMSV-UHFFFAOYSA-N methyl nitrite Chemical compound CON=O BLLFVUPNHCTMSV-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000831 Steel Inorganic materials 0.000 claims description 21
- 239000010959 steel Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 5
- 235000011149 sulphuric acid Nutrition 0.000 abstract description 10
- 239000001117 sulphuric acid Substances 0.000 abstract description 10
- 238000004590 computer program Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 230000008878 coupling Effects 0.000 abstract description 3
- 238000010168 coupling process Methods 0.000 abstract description 3
- 238000005859 coupling reaction Methods 0.000 abstract description 3
- 238000007598 dipping method Methods 0.000 abstract 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 21
- 239000007789 gas Substances 0.000 description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- 235000010288 sodium nitrite Nutrition 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003245 coal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002341 toxic gas Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010020852 Hypertonia Diseases 0.000 description 1
- LOMVENUNSWAXEN-UHFFFAOYSA-N Methyl oxalate Chemical compound COC(=O)C(=O)OC LOMVENUNSWAXEN-UHFFFAOYSA-N 0.000 description 1
- 239000007832 Na2SO4 Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000003287 bathing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 235000003642 hunger Nutrition 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 230000037351 starvation Effects 0.000 description 1
Abstract
The utility model provides an automatic system takes place for methyl nitrite, include: reaction vessel, in the bottom dipping in thermostatted water bath cabinet liquid, a pressure sensor is connected to reaction vessel's a port, and a peristaltic pump is connected to another port, connects a sulphuric acid storage tank at the other end of this peristaltic pump, the cold -trap pipe, with reaction vessel connects, in the dipping in low -temperature constant -temperature bath cabinet liquid, methyl nitrite storage device is with the cold -trap union coupling, in the dipping in low -temperature constant -temperature bath cabinet liquid, vacuum cylinder, one end are connected in methyl nitrite storage device, and a vacuum pump is connected to the other end, are connected a pressure sensor on the pipeline between vacuum cylinder and the methyl nitrite storage device. This system can improve the methyl nitrite's of formation productivity and purity, improves the stability and the security of reaction system, combines computer program automatic control, and the operating personnel of being convenient for observes, reduces intensity of labour.
Description
Technical field
This utility model relates to chemical research technical field, is specifically related to a kind of methyl nitrite generation systems automatically.
Background technology
The oxidized coupling synthesis of oxalate of carbon monoxide, and then Hydrogenation is that C1 chemical heavy wants one of research direction for ethylene glycol, and oxalate is as the intermediate products of the many kinds of substances such as dyestuff, medicine, extractant, owing to having structure and the performance of uniqueness, receive extensive concern. The few natural gas of China's oil starvation, coal relative abundance, by producing synthesis gas from coal then through oxalate preparing ethylene glycol, is a more economic ethylene glycol synthetic route.
Oxalate synthetic reaction process is:
2CH3ONO+2CO��(COOCH3)2+2NO
Current lot of domestic and international colleges and universities and scientific research institutions are all at the research work carrying out CO coupling generation dimethyl oxalate. catalyst, reactor feed gas methyl nitrite is owing to having bought being difficult on the market, need to configure at laboratory voluntarily, shown in traditional collocation method and flow chart accompanying drawing 1: a certain amount of methanol and sodium nitrite are placed in there-necked flask, then being added dropwise over sulphuric acid, product methyl nitrite becomes liquid through cryosel or liquid nitrogen; After methyl nitrite steel cylinder is pumped into negative pressure, the methyl nitrite of liquid is pumped in methyl nitrite steel cylinder together.
Reaction equation is as follows:
2NaNO2+H2SO4+2CH3OH=Na2SO4+2CH3ONO+2H2O
Current laboratory is prepared methyl nitrite gas link and is substantially all adopted this manual mode, detailed step is as follows: with vacuum pump 102, methyl nitrite steel cylinder 101 is evacuated to vacuum, there-necked flask 109 adds a certain proportion of sodium nitrite solution and absolute methanol, Dropping funnel 110 adds concentrated sulphuric acid. It is slowly added dropwise concentrated sulphuric acid in there-necked flask 109. Evacuated methyl nitrite steel cylinder 101 is connected after starting by reaction with gas generating unit. Under the effect of pressure reduction, react the gas of generation run through the Drexel bottle 106 of cryosel bath 105, water in condensation separation gas and entering in methyl nitrite steel cylinder 101 after methanol. When in methyl nitrite steel cylinder 101, pressure reaches stopped reaction after absolute pressure, it is filled with steel cylinder with High Purity Nitrogen and is configured to the gaseous mixture that reaction is required. Preparation notes at any time following some: one is make response system maintenance normal pressure, it is to avoid operate under vacuo; Two is prevent the methanol in solution from volatilizing, and produces NO gas, causes product gas purity to decline; Three is the drop rate that need to control concentrated sulphuric acid at any time, it is to avoid reaction is excessively fierce, causes glass container blast or release of toxic gas.
In course of reaction, the change of system pressure generally indicates with balloon, therefore experimenter must observe in the moment in course of reaction, it is prevented that gas produces too fast, causes system pressure too high, it is impossible to collect gas. This reaction process suffers from the drawback that one is the sulphuric acid dripping high concentration with Dropping funnel, can gradually decrease because of acid amount, its flow velocity is continually changing in course of reaction, causes whole system unstable so that amount and the purity of the methyl nitrite gas of generation all have larger fluctuation; Two is reaction system pressure using balloon as instruction, it is difficult to strictly monitors reaction process, can reduce productivity and the purity of reaction, also easily cause danger; Three is that reaction adopts non-close system, it is often necessary to carries out in fume hood, can discharge substantial amounts of nitrogen oxides, bring great pollution to environment in course of reaction. In a word, the gas procedure of preparing adopted at present is wasted time and energy, and there is substantial amounts of potential safety hazard, is badly in need of freeing operator from " gas-making process " frequently, experiment progress can be accelerated on the one hand, also ensure that on the other hand and prepare highly purified methyl nitrite gas.
Utility model content
For overcoming above-mentioned deficiency, this utility model provides a kind of methyl nitrite generation systems automatically, improves productivity and the purity of the methyl nitrite generated, improve stability and the safety of response system, automatically control in conjunction with computer program, it is simple to operator observe, reduce labor intensity.
For solving above-mentioned technical problem, this utility model be the technical scheme is that
A kind of methyl nitrite generation systems automatically, including:
Reaction vessel, bottom is dipped in a constant water bath box liquid, and the Single port of reaction vessel connects a pressure transducer, and another port connects a peristaltic pump, and the other end at this peristaltic pump connects a sulfuric acid storage tank;
Cold-trap pipe, is connected with described reaction vessel, is dipped in a cryogenic thermostat bath cabinet liquid;
Methyl nitrite storage device, is connected with cold-trap pipe, is dipped in a cryogenic thermostat bath cabinet liquid;
Dewar bottle, one end is connected to methyl nitrite storage device, and the other end connects a vacuum pump, and the pipeline between Dewar bottle with methyl nitrite storage device is connected a pressure transducer.
Further, described reaction vessel is there-necked flask, and described pressure transducer and peristaltic pump are individually fixed in two ports of there-necked flask; Described methyl nitrite storage device is methyl nitrite steel cylinder.
Further, the outlet side of described reaction vessel connects a drying tower.
Further, the access port of described cold-trap pipe, described Dewar bottle access port connect pinch valve respectively.
Further, described pinch valve is wiredly connected to computer.
Further, described cold-trap pipe and methyl nitrite storage device are dipped in same cryogenic thermostat bath cabinet liquid.
Further, it is designed with temperature sensor in described constant water bath box and cryogenic thermostat bath cabinet.
Further, described peristaltic pump, pressure transducer, temperature sensor are all wiredly connected to computer.
The beneficial effects of the utility model are, one is instead of Dropping funnel with peristaltic pump, it is ensured that in course of reaction, the speed of sulphuric acid dropping is consistent; Two is adopt pinch valve, pressure transducer to instead of three-way valve, balloon, and pinch valve, pressure transducer adopt computer program to control, and run into system pressure and extremely can close down reaction at any time, improve response system stability, safety; Three is instead of traditional cryosel bath with cryogenic thermostat bath, makes condenser temperature keep consistent, is conducive to product steadily to collect; Four is that methyl nitrite generating means all adopts computer controlled automatic, vitriolic acid flux, reacting system pressure, steel cylinder negative pressure, temperature etc. all synchronize to show on computers, facilitate operator to observe, reduce the labor intensity of operator, improve work situation; Five is that whole reaction system adopts closed loop control, reduces the toxic gas harm to operator, decreases environmental pollution simultaneously.
Accompanying drawing explanation
Fig. 1 is the generating means schematic diagram of traditional methyl nitrite.
In figure: 101 is methyl nitrite steel cylinder; 102 is vacuum pump; 103 is Dewar bottle; 104 is three-way valve; 105 is cryosel bathing pool; 106 is Drexel bottle; 107 is magnetic agitation heater; 108 is constant water bath box; 109 is there-necked flask; 110 is Dropping funnel; 111 is thermometer; 112 is balloon.
Fig. 2 is a kind of full-automatic methyl nitrite generating means schematic diagram in embodiment.
In figure: 201 is sulfuric acid storage tank; 202 is peristaltic pump; 203 is constant water bath box; 204,213 is pressure transducer; 205 is there-necked flask; 206 is drying tower; 207,209,212,215 is pinch valve; 208 is cold-trap pipe; 210 is cryogenic thermostat bath cabinet; 211 is methyl nitrite steel cylinder; 214 is Dewar bottle; 216 is vacuum pump.
Detailed description of the invention
For making features described above of the present utility model and advantage to become apparent, special embodiment below, and coordinate institute's accompanying drawing to be described in detail below.
The present embodiment provides a kind of methyl nitrite generating means automatically, as shown in Figure 2, including the sulfuric acid storage tank 201 being sequentially connected with, peristaltic pump 202, there-necked flask 205, drying tower 206, cold-trap pipe 208, methyl nitrite steel cylinder 211, Dewar bottle 214 and vacuum pump 216, middle mouth at there-necked flask 205 connects a pressure transducer 204, also a pressure transducer 213 it is connected with in the middle of Dewar bottle 214 at methyl nitrite steel cylinder 211, it is respectively equipped with pinch valve 207 in the access port of cold-trap pipe 208 and the access port of Dewar bottle 214, 209, 212, 215, the bottom of there-necked flask 205 is dipped in constant water bath box 203 liquid, cold-trap pipe 208 and methyl nitrite steel cylinder 211 are placed in same cryogenic thermostat bath cabinet 210 liquid, it is equipped with temperature sensor (not shown) in constant water bath box 203 and cryogenic thermostat bath cabinet 210. the peristaltic pump 202 of this automatic methyl nitrite generating means, pinch valve 207,209,212,215, pressure transducer 204,213, temperature sensor all with computer wired connection, computer program can automatically control or monitor the parameters such as vitriolic acid flux, steel cylinder negative pressure, system pressure and temperature, and displays at computer terminal.
When experiment starts, with vacuum pump 216, steel cylinder 211 being evacuated to vacuum, now pinch valve 209,215 Guan Bi, pinch valve 212 is opened, and when pressure transducer 213 shows negative pressure less than 0.1KPa, closes methyl nitrite steel cylinder 211, closes vacuum pump 216. In advance equipped with baked 3A molecular sieve (moisture and methanol that carry in reaction can be removed) in drying tower 206, the sodium nitrite solution (420g sodium nitrite+1000ml deionized water+350ml methanol) prepared is poured in there-necked flask 205, the sulphuric acid 300ml of 1:1 is poured in sulfuric acid storage tank 201, peristaltic pump 202 computerizeds control, and input sulphuric acid drop rate is 3mL/min. It is 20 DEG C that water bath with thermostatic control controls, and cryogenic thermostat bath controls as-30 DEG C, and now pinch valve 207 is in opening, and pinch valve 209,212,215 is in closure state. Now, continuing to receive methyl nitrite liquid (methyl nitrite boiling point-12 DEG C, fusing point-17 DEG C) in cold-trap pipe 208, pressure transducer 204 reading monitored at any time by computer, such as hypertonia or too low can report to the police. After peristaltic pump 202 dropwises without flow and sulphuric acid, computer controls pinch valve 207 and closes, pinch valve 209 is opened, now methyl nitrite steel cylinder 211 is opened, when observing no liquid in cold-trap pipe 208, close methyl nitrite steel cylinder 210, closed clip pipe valve 209, now methyl nitrite is prepared complete, collects methyl nitrite liquid 150mL. Gas in steel cylinder passing into detection in gas chromatogram analyze, the methyl nitrite gas purity (mass percent) obtained is: methyl nitrite >=99%, methanol < 1%.
By the present embodiment it can be seen that this automatic methyl nitrite generating means can improve productivity and the purity of the methyl nitrite of generation, improve stability and the safety of response system, automatically control in conjunction with computer program, it is simple to operator observe, reduce labor intensity.
Claims (8)
1. an automatic methyl nitrite generation systems, it is characterised in that including:
Reaction vessel, bottom is dipped in a constant water bath box liquid, and the Single port of reaction vessel connects a pressure transducer, and another port connects a peristaltic pump, and the other end at this peristaltic pump connects a sulfuric acid storage tank;
Cold-trap pipe, is connected with described reaction vessel, is dipped in a cryogenic thermostat bath cabinet liquid;
Methyl nitrite storage device, is connected with cold-trap pipe, is dipped in a cryogenic thermostat bath cabinet liquid;
Dewar bottle, one end is connected to methyl nitrite storage device, and the other end connects a vacuum pump, and the pipeline between Dewar bottle with methyl nitrite storage device is connected a pressure transducer.
2. automatic methyl nitrite generation systems according to claim 1, it is characterised in that described reaction vessel is there-necked flask, described pressure transducer and peristaltic pump are individually fixed in two ports of there-necked flask; Described methyl nitrite storage device is methyl nitrite steel cylinder.
3. automatic methyl nitrite generation systems according to claim 1, it is characterised in that the outlet side of described reaction vessel connects a drying tower.
4. automatic methyl nitrite generation systems according to claim 1, it is characterised in that the access port of described cold-trap pipe, described Dewar bottle access port connect pinch valve respectively.
5. automatic methyl nitrite generation systems according to claim 4, it is characterised in that described pinch valve is wiredly connected to computer.
6. automatic methyl nitrite generation systems according to claim 1, it is characterised in that described cold-trap pipe and methyl nitrite storage device are dipped in same cryogenic thermostat bath cabinet liquid.
7. automatic methyl nitrite generation systems according to claim 1, it is characterised in that described constant water bath box and be designed with temperature sensor in cryogenic thermostat bath cabinet.
8. automatic methyl nitrite generation systems according to claim 7, it is characterised in that described peristaltic pump, pressure transducer, temperature sensor are all wiredly connected to computer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201521084388.4U CN205275494U (en) | 2015-12-23 | 2015-12-23 | Automatic system takes place for methyl nitrite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201521084388.4U CN205275494U (en) | 2015-12-23 | 2015-12-23 | Automatic system takes place for methyl nitrite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN205275494U true CN205275494U (en) | 2016-06-01 |
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ID=56060087
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201521084388.4U Expired - Fee Related CN205275494U (en) | 2015-12-23 | 2015-12-23 | Automatic system takes place for methyl nitrite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN205275494U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107056619A (en) * | 2017-02-21 | 2017-08-18 | 安阳永金化工有限公司 | Regenerator safety device is esterified for coal-ethylene glycol methyl nitrite |
-
2015
- 2015-12-23 CN CN201521084388.4U patent/CN205275494U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107056619A (en) * | 2017-02-21 | 2017-08-18 | 安阳永金化工有限公司 | Regenerator safety device is esterified for coal-ethylene glycol methyl nitrite |
| CN107056619B (en) * | 2017-02-21 | 2019-08-02 | 安阳永金化工有限公司 | Regenerator safety device is esterified for coal-ethylene glycol methyl nitrite |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160601 Termination date: 20171223 |
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| CF01 | Termination of patent right due to non-payment of annual fee |