CN102515124B - Method for producing liquid dinitrogen trioxide - Google Patents
Method for producing liquid dinitrogen trioxide Download PDFInfo
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- CN102515124B CN102515124B CN201210002912.3A CN201210002912A CN102515124B CN 102515124 B CN102515124 B CN 102515124B CN 201210002912 A CN201210002912 A CN 201210002912A CN 102515124 B CN102515124 B CN 102515124B
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- gas
- liquid
- nitric acid
- dinitrogen trioxide
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- LZDSILRDTDCIQT-UHFFFAOYSA-N dinitrogen trioxide Chemical compound [O-][N+](=O)N=O LZDSILRDTDCIQT-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000007788 liquid Substances 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- WFPZPJSADLPSON-UHFFFAOYSA-N dinitrogen tetraoxide Chemical compound [O-][N+](=O)[N+]([O-])=O WFPZPJSADLPSON-UHFFFAOYSA-N 0.000 claims abstract description 24
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- 239000012043 crude product Substances 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 5
- 239000000945 filler Substances 0.000 claims description 5
- 239000012267 brine Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 4
- 239000002253 acid Substances 0.000 abstract description 11
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 description 5
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 4
- XZPVPNZTYPUODG-UHFFFAOYSA-M sodium;chloride;dihydrate Chemical compound O.O.[Na+].[Cl-] XZPVPNZTYPUODG-UHFFFAOYSA-M 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 3
- OMBRFUXPXNIUCZ-UHFFFAOYSA-N dioxidonitrogen(1+) Chemical compound O=[N+]=O OMBRFUXPXNIUCZ-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical group [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 229960001701 chloroform Drugs 0.000 description 2
- 238000006193 diazotization reaction Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000003507 refrigerant Substances 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 235000010288 sodium nitrite Nutrition 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229950005499 carbon tetrachloride Drugs 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000012809 cooling fluid Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method and equipment for producing liquid dinitrogen trioxide. One raw material used in the method is diluted nitric acid which is waste acid from a nitric acid device. The diluted nitric acid at the concentration is expensive to recycle and may cause environment pollution when discharged. The method disclosed by the invention can change this waste into a valuable material and is in accordance with national energy-conservation and emission-reduction policy. According to the method, liquid N2O4 serving as a raw material is reacted with NO to form dinitrogen trioxide, and the reaction which is a bubble type gas and liquid flow contact reaction is easier to operate and more complete than gas-gas flow reaction of NO and NO2.
Description
Technical field
The present invention relates to a kind of productive method of chemical engineering and equipment.
Background technology
Nitrous anhydride is a kind of acidic oxide, poisonous, dissolves in benzene, ether, chloroform (trichloromethane), tetracol phenixin (tetrachloromethane), soda acid unstable, under normal pressure, can be decomposed into nitrogen protoxide and nitrogen peroxide.
Nitrous anhydride is the acid anhydrides of nitrous acid, nitrous acid is due to unstable, be made generally in Sodium Nitrite and store, when use, adding strong acid can generate, and nitrous acid is widely used in chemical reaction, as nitrosification, diazotization reaction, needs to add water, strong acid owing to making at Sodium Nitrite in nitrous acid process, and after reaction, there is sodium ion out, so its application has certain limitation.Use nitrous anhydride to replace nitrous acid to carry out nitrosification and diazotization, can under anhydrous state, carry out, and produce without sodium ion after reaction, can also significantly reduce the total amount of discharge of wastewater, realize cleaner production, have good application prospect.But defectiveness is gone back in its production.
Summary of the invention
Technical problem solved by the invention is to provide a kind of method of producing liquid dinitrogen trioxide, and can produce and obtain liquid dinitrogen trioxide product, and product can be directly as finished product sale or use, easily preservation, equipment cost is low, and efficiency is high.
A method of producing liquid dinitrogen trioxide, comprises the following steps:
1. by rare nitric acid hybrid reaction of the crude product nitrogen tetroxide of massfraction 92～96% and massfraction 10%～18%, reaction is carried out under 0.1MPa.G low pressure;
2. material after completion of the reaction, through separating, is drawn the NO gas of generation, and liquid phase is rare nitric acid, then continues to add the crude product nitrogen tetroxide hybrid reaction of massfraction 92～96%;
3. repeating step 2.;
4. material after completion of the reaction, through separating, is drawn the NO gas of generation, and the NO gas of 2. and 3. drawing with step converges;
5. the NO gas of step after 4. converging is down to normal temperature, separates and removes nitric acid; Obtain raw material NO gas, be compressed to 0.32MPa.G (gauge pressure), then be cooled to-25 DEG C～-30 DEG C;
6. step raw material NO gas and massfraction is 5. not less than 99.7% sterling liquid N
2o
4in reactor, react, its Raw NO gas is excessive; Reaction pressure is 0.15～0.3MPa.G, and temperature of reaction is-15 DEG C～-22 DEG C;
7. 6. step reacts the complete liquid N that obtains
2o
3, wherein containing excessive NO, the NO of dissolving is separated out in vacuum flashing, obtains liquid N
2o
3product.
The method of production liquid dinitrogen trioxide of the present invention, the reaction 1., 2., 3. of wherein said step is carried out in tubular reactor.
The method of production liquid dinitrogen trioxide of the present invention, the reactor of wherein said step in is 6. ceramic filler tower.
The method of production liquid dinitrogen trioxide of the present invention, the cooling step of wherein said step in 5. first adopts chilled brine cooling, then adopts ammonia cold.
The present invention also provides a kind of equipment of the method that is exclusively used in above-mentioned production liquid dinitrogen trioxide, comprise tubular reactor a, connect successively thereafter intermediate separator a, water cooler a, tubular reactor b, intermediate separator b, water cooler b, tubular reactor c, final separator and water cooler c; The top exit of intermediate separator a, intermediate separator b and final separator is connected water cooler d, acid separator, compressor, chilled brine water cooler, ammonia cooler, reactor after being communicated with again successively.Described reactor is ceramic filler tower.
The chemical reaction relating in the present invention has:
1.5N
2O
4+H
2O＝2HNO
3+NO-Q，
This is a thermopositive reaction, and speed of response is very fast, thus preferably adopt tubular reactor, and adopt the outer hot method of moving, tubular reactor arranges a sleeve pipe of importing and exporting with cooling fluid outward again, and heat of reaction is taken away immediately; (0.1MPa.G) under low pressure carried out in reaction;
N
2O
4+2NO＝2N
2O
3-Q，
This is a thermopositive reaction, and reactant ratio adopts the excessive scheme of NO.
The liquid dinitrogen trioxide that the present invention finally obtains adopts ammonia compressor refrigeration part to use chilled brine to store N as secondary refrigerant
2o
3, condition of storage: 0.01～0.05M Pa.G ,-21～-15 DEG C, storage in liquid and transport.
The present invention can obtain following technique effect:
(1) one of raw material of the present invention is rare nitric acid (massfraction is 10%～18%), the spent acid that rare nitric acid of this kind of concentration produces in nitric acid plant, the cost of utilization is high, discharges and contaminate environment, the present invention can be turned waste into wealth, and meets the national policy of energy-saving and emission-reduction;
(2) the present invention adopts tubular reactor, has guaranteed that resistance drop is in rational scope, and has reduced the vibration of reactor, prevents liquid hammer and causes security incident;
(3) the present invention adopts liquid N
2o
4react with NO as raw material and produce nitrous anhydride, react for the contact of bubbling style gas-liquid flow, compared to using NO and NO
2the reaction of gas-air-flow, react more easy to operate, react also more complete;
(4) be-15 DEG C～-22 DEG C from reactor nitrous anhydride product temperature out, can directly enter accumulating operation after only need flashing off the NO of dissolving;
(5) equipment cost is low, and efficiency is high.
The single devices using in the present invention all has commercially available.
Brief description of the drawings
Fig. 1 is the schematic diagram of the equipment of the embodiment of the present invention 1; Wherein:
1: tubular reactor a; 2: intermediate separator a; 3: water cooler a; 4: tubular reactor b; 5: intermediate separator b; 6: water cooler b; 7: tubular reactor c; 8: final separator; 9: water cooler c; 13: water cooler d; 14: acid separator; 15: compressor; 16: chilled brine water cooler; 17: ammonia cooler; 18: reactor; 19: adjust tank.
Embodiment
For further illustrating the present invention, illustrate with the following Examples:
Embodiment 1:
A kind of equipment of the method for the production of liquid dinitrogen trioxide, comprise tubular reactor a1, connect successively thereafter intermediate separator a2, water cooler a3, tubular reactor b4, intermediate separator b5, water cooler b6, tubular reactor c7, final separator 8 and water cooler c9; The top exit of intermediate separator a2, intermediate separator b5 and final separator 8 is connected water cooler d13, acid separator 14, compressor 15, chilled brine water cooler 16, ammonia cooler 17, reactor 18 after being communicated with again successively.Described reactor 18 is ceramic filler tower, behind its bottom, is communicated to and adjusts tank 19.
Flow process when this equipment uses is as follows:
1. after crude product nitrogen tetroxide (massfraction 92～96%) being mixed with rare nitric acid (massfraction is 10%～18%), enter tubular reactor a1;
2. in tubular reactor a1, nitrogen tetroxide reacts with the water in the rare nitric acid of rare nitric acid, obtains nitric acid and nitrogen protoxide, and equation is as follows:
1.5N2O4+H2O＝2HNO3+NO-Q
This is a thermopositive reaction, and speed of response is very fast, thus adopt tubular reactor, and adopt the outer hot method of moving, (0.1MPa.G) under low pressure carried out in reaction;
3. from tubular reactor a1 out material enter intermediate separator a2, the NO of generation is drawn, liquid phase is that rare nitric acid continues to enter tubular reactor b3;
4. in tubular reactor b4, continue to add crude product nitrogen tetroxide, reacting rear material enters intermediate separator b5, and the NO of generation draws, and liquid phase is that rare nitric acid continues to enter tubular reactor c7;
5. in tubular reactor c7, continue to add crude product nitrogen tetroxide, reacting rear material enters final stage separator 8, the NO generating is down to after normal temperature after drawing and converging with intermediate separator a and intermediate separator b NO gas out after water cooler 13, is incorporated to acid separator 14 separation and removes nitric acid;
6. be compressed to 0.32MPa.G from acid separator 14 unstripped gas out through compressor 15 one-levels, then through chilled brine water cooler 16 and ammonia cooler 17, temperature enters reactor 18 bottoms after being down to-25 DEG C～-30 DEG C;
7. in reactor 18 (being ceramic filler tower), sterling liquid N2O4 (massfraction is not less than 99.7%) enters from top, reacts with the NO in the unstripped gas of bottom, and equation is as follows:
N2O4+2NO＝2N2O3-Q，
This is a thermopositive reaction, reactant ratio adopts the excessive scheme of NO, NO gas adds from the bubbling segment of reactor bottom, reaction pressure is 0.15～0.3MPa.G, temperature of reaction is-15 DEG C～-22 DEG C, liquid N2O4 adds from top, and unabsorbed NO gas temperature is increased to-10～-8 DEG C, mixes fresh feed gas and enters acid separator 14;
8. from the liquid N2O3 out of reactor 18 bottoms, contain excessive NO, enter and adjust in tank 19, after vacuum flashing, separate out after the NO of dissolving, obtain product, enter product accumulating operation.
Adopt ammonia compressor refrigeration part to use chilled brine to store N2O3 as secondary refrigerant, condition of storage: 0.01～0.05MPa.G ,-21～-15 DEG C, storage in liquid and transport.
Above-described embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not departing from the present invention; various distortion and improvement that the common engineering technical personnel in this area make technical scheme of the present invention, all should fall in the definite protection domain of claims of the present invention.
Claims (4)
1. a method of producing liquid dinitrogen trioxide, is characterized in that: comprise the following steps:
1. by rare nitric acid hybrid reaction of the crude product nitrogen tetroxide of massfraction 92～96% and massfraction 10%～18%, reaction is carried out under 0.1MPa.G low pressure;
2. material after completion of the reaction, through separating, is drawn the NO gas of generation, and liquid phase is rare nitric acid, then continues to add the crude product nitrogen tetroxide hybrid reaction of massfraction 92～96%;
3. repeating step 2.;
4. material after completion of the reaction, through separating, is drawn the NO gas of generation, and the NO gas of 2. and 3. drawing with step converges;
5. the NO gas of step after 4. converging is down to normal temperature, separates and removes nitric acid; Obtain raw material NO gas, be compressed to 0.32MPa.G, then be cooled to-25 DEG C～-30 DEG C;
6. step raw material NO gas and massfraction is 5. not less than 99.7% sterling liquid N
2o
4in reactor, react, its Raw NO gas is excessive; Reaction pressure is 0.15～0.3MPa.G, and temperature of reaction is-15 DEG C～-22 DEG C;
7. 6. step reacts the complete liquid N that obtains
2o
3, wherein containing excessive NO, the NO of dissolving is separated out in vacuum flashing, obtains liquid N
2o
3product.
2. the method for production liquid dinitrogen trioxide according to claim 1, is characterized in that: the reaction 1., 2., 3. of described step is carried out in tubular reactor.
3. the method for production liquid dinitrogen trioxide according to claim 1, is characterized in that: the reactor of described step in is 6. ceramic filler tower.
4. the method for production liquid dinitrogen trioxide according to claim 1, is characterized in that: the cooling step of described step in 5. first adopts chilled brine cooling, then adopts ammonia cold.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210002912.3A CN102515124B (en) | 2012-01-06 | 2012-01-06 | Method for producing liquid dinitrogen trioxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210002912.3A CN102515124B (en) | 2012-01-06 | 2012-01-06 | Method for producing liquid dinitrogen trioxide |
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| Publication Number | Publication Date |
|---|---|
| CN102515124A CN102515124A (en) | 2012-06-27 |
| CN102515124B true CN102515124B (en) | 2014-07-02 |
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|---|---|---|---|
| CN201210002912.3A Expired - Fee Related CN102515124B (en) | 2012-01-06 | 2012-01-06 | Method for producing liquid dinitrogen trioxide |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3428540A (en) * | 1962-03-09 | 1969-02-18 | Allied Chem | Process for making trifluoroamine oxide |
| CN101885479A (en) * | 2010-06-13 | 2010-11-17 | 上海浦景化工技术有限公司 | Preparation method of dinitrogen trioxide and reaction equipment thereof |
| CN202482065U (en) * | 2012-01-06 | 2012-10-10 | 安徽淮化股份有限公司 | Equipment for producing liquid dinitrogen trioxide |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51143593A (en) * | 1975-06-06 | 1976-12-09 | Mitsubishi Heavy Ind Ltd | A procedure of converting the nitric dioxide to the nitric oxide |
| JP3325434B2 (en) * | 1995-08-22 | 2002-09-17 | 株式会社日立製作所 | Reference clock supply device and mobile terminal device using the same |
-
2012
- 2012-01-06 CN CN201210002912.3A patent/CN102515124B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3428540A (en) * | 1962-03-09 | 1969-02-18 | Allied Chem | Process for making trifluoroamine oxide |
| CN101885479A (en) * | 2010-06-13 | 2010-11-17 | 上海浦景化工技术有限公司 | Preparation method of dinitrogen trioxide and reaction equipment thereof |
| CN202482065U (en) * | 2012-01-06 | 2012-10-10 | 安徽淮化股份有限公司 | Equipment for producing liquid dinitrogen trioxide |
Non-Patent Citations (8)
| Title |
|---|
| A. VESELÁ |
| A. VESEL& * |
| Aacute * |
| et al..The Role of Carbon Dioxide in Free Radical Reactions of the Organism.《Physiol. Res.》.2002,第51卷335-339. * |
| JP特開昭49-62396A 1974.06.17 |
| JP特開昭51-143593B2 1976.12.09 |
| 梁肃臣等.氮氧化物的制备、性质和应用.《低温与特气》.1996,(第4期),18-21、29. |
| 氮氧化物的制备、性质和应用;梁肃臣等;《低温与特气》;19961231(第4期);18-21、29 * |
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Effective date of registration: 20210508 Address after: 234000 No. 157, Xichang Road, Suzhou, Anhui Patentee after: WANBEI COAL-ELECTRICITY GROUP Co.,Ltd. Address before: 232038 Anhui Huainan Tian Jia An District Quanshan Anhui Huaihua Limited by Share Ltd technology research and Development Center Patentee before: ANHUI HUAIHUA Co.,Ltd. |
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