CN1244534C - Technological process for producing sodium oxalate by liquid-spraying type sodium formate dehydrogenation and use equipment - Google Patents
Technological process for producing sodium oxalate by liquid-spraying type sodium formate dehydrogenation and use equipment Download PDFInfo
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- CN1244534C CN1244534C CN 02148873 CN02148873A CN1244534C CN 1244534 C CN1244534 C CN 1244534C CN 02148873 CN02148873 CN 02148873 CN 02148873 A CN02148873 A CN 02148873A CN 1244534 C CN1244534 C CN 1244534C
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Abstract
The present invention relates to a technology and a device thereof for producing sodium oxalate by the liquid spray type dehydrogenation of sodium formate. The technology comprises the steps that a sodium formate solution is mixed with thermal airflow for sufficient heat exchange, and the sodium oxalate can be obtained by dewatering, melting and a dehydrogenation reaction of the sodium formate solution. The device for the technology mainly comprises a hot air furnace, a heat exchanger, a dehydrogenation reactor and a separator, wherein a shrinking pipe arranged in the dehydrogenation reactor is used for realizing the sufficient heat exchange of the sodium formate solution and the thermal airflow. The technology overcomes the defects of the prior art. The device has the advantages of little equipment investment, simple and convenient technological operation, steam consumption saving, low cost and high conversion rate and heat efficiency.
Description
Technical field
The present invention relates to the preparation method of sodium oxalate.Particularly a kind of liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology and equipment used thereof.
Background technology
Existing process by sodium formiate production sodium oxalate at first is that aqueous sodium formate solution is condensed into supersaturated solution with double-effect evaporator; separate out the crystal of band crystal water; utilize centrifuge dewatering to make exsiccant sodium formiate crystal; and then exsiccant sodium formiate crystal is put into the dehydrogenation pot of handwarmer; with the flame direct heating the bottom of a pan, be heated through fusion until dehydrogenation reaction takes place, cease fire immediately and water; take sodium oxalate suspension away with vacuum then, circulation is so again and again gone down.Its shortcoming is: 1, its production process is to be interrupted; 2, its production process is used the more so power consumption height of rotating machinery; 3, the thermo-efficiency of its handwarmer dehydrogenation pot is lower, only has 16～18%; 4, heating process temperature control is observed by the workman and is finished, so poor stability, be prone to sticking pot and be burned phenomenon, sometimes the part also can occurring, to rest on a certain temperature-time longer, the side reaction of part takes place, influence the transformation efficiency that sodium formiate generates sodium oxalate, at present generally 78～84%; 5, need to use the post personnel more; 6, aqueous sodium formate solution is condensed into supersaturation and separates out a large amount of crystal, use steam heating, so steam consumption is higher; 7, owing to be handwarmer, smoke prevention and dust control are difficult for reaching ideal effect, and environment is had pollution.
Summary of the invention
The objective of the invention is to overcome the defective of prior art and provide that a kind of facility investment is little, technological operation is simple and convenient, can save steam consumption, cost is low, transformation efficiency and all higher liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology of thermo-efficiency.
Another object of the present invention provides a kind of above-mentioned liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology equipment used.
Liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology of the present invention comprises certain density sodium formate solution is heated to 180-205 ℃ earlier, mix with 900-1050 ℃ hot gas flow again and carry out sufficient heat exchange, make sodium formate solution through dehydration, fusion until dehydrogenation reaction takes place; Isolate hydrogen then, can obtain the resultant sodium oxalate.
Wherein, the concentration of described sodium formate solution can be 45-50%.
The blending ratio of described sodium formate solution and hot gas flow can be 1: 2-5.
In the reaction process of the dehydration of described sodium formate solution, fusion and dehydrogenation, the mixture velocity of itself and hot gas flow is increased to 50-80m/s by 15-25m/s in the scope of 8-10 rice, be contracted to 15-25m/s again.
Liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology equipment used of the present invention mainly comprise hotblast stove, interchanger, dehydrogenation reactor and separator; Wherein said dehydrogenation reactor comprises reactor shell, and an end of cylindrical shell links to each other with the air outlet of hotblast stove, is provided with the atomizer nozzle identical with the hot blast wind direction near this air outlet place; Be provided with the convergent-divergent pipe that contraction gradually enlarges gradually again at the reactor middle part, the other end of cylindrical shell communicates with the separator inlet place.
Wherein, the effect of described convergent-divergent pipe be make the dry sodium formiate of the fine particle shape that forms behind the sodium formiate transpiring moisture once more with the hot blast intense mixing, accelerate its mixture heat exchange velocity and fully heating, make the dehydrogenation reaction of sodium formiate comparatively thorough, help improving transformation efficiency.
Described cylindrical shell length can be 8-10 rice; Barrel diameter can be the 280-320 millimeter; Distance in the described cylindrical shell between nozzle and the convergent-divergent pipe can be 3-5 rice.
Gas flow rate can be 15-20m/s in the described reactor; The gas flow rate of described convergent-divergent pipe at the minimum diameter place can be 50-80m/s.
Liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology equipment used of the present invention can also comprise high-pressure pump.
Liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology equipment used of the present invention can also comprise with the alternative above-mentioned dehydrogenation reactor of venturi nozzle reactor.Using the core of venturi nozzle reactor is the Venturi de Laval noz(zle), the elevated temperature heat air-flow that produces by the hotblast stove shrinking zone compression of flowing through, the speed during by throat is very high, can reach 80-120m/s, spray into aqueous sodium formate solution in throat this moment, and the flow velocity in the squit hole is 11-15m/s.Its drips of solution will be impacted into the very big tiny vaporific drop of surface-area (ratio of unit weight) by the kinetic energy of high velocity air, and turbulent flow goes in the hot gas flow to be mixed into the higher heat exchange of line efficiency with it consumingly, moisture in the drop promptly is evaporated, sodium formiate forms than bigger, the more tiny dry sodium formiate particle of the specific surface area of drop, and be suspended in and continue in the hot gas flow to be heated, through being molten to the generation dehydrogenation reaction, generate sodium oxalate and hydrogen.Hydrogen and waste gas are discharged from through tripping device then, and meanwhile sodium oxalate but is collected.Because the discharge that sprays into waste gas of aqueous sodium formate solution all is a successive, so its reaction also is a successive.
The characteristics of liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology of the present invention are that to produce the exsiccant sodium formiate be that different positions in same well heater is finished with continuing heating until dehydrogenation reaction takes place, and its advantage is:
1, equipment is few, invests for a short time, and technological operation is simple and convenient.
2, can save the steam consumption of producing dried sodium formiate with the sodium formate solution dehydrogenation, save about 1 ton of steam/(ton sodium oxalate).
3, a hotblast stove can be banned whole dehydrogenation cooking stoves, and a sparge pipe well heater can be banned whole dehydrogenation pots; Also can cancel simultaneously and make a fire and see personnel such as pipe boiler post, reduce cost, suit measures to local conditions, be about 9 yuan of/ton sodium oxalates.
4, at short notice, just can make sodium formiate be heated to 400 ℃ and dehydrogenation reaction takes place, this is very favourable to improving its transformation efficiency that changes into sodium oxalate; As long as the blending ratio of sodium formate solution and hot gas flow is appropriate, the outlet temperature of its reaction just can obtain good control, and its transformation efficiency is reached more than 90%; Save the consumption of sodium formiate, be about 0.12 ton/sodium oxalate.
5, the thermo-efficiency of technological process is higher, can reach more than 60%, economizes on coal to be about 0.13 ton/oxalic acid.
Description of drawings
Further describe the present invention below in conjunction with drawings and Examples.
Accompanying drawing 1 is a liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate process flow sheet of the present invention;
Accompanying drawing 2 is the one-piece construction synoptic diagram of dehydrogenation reactor described in the liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology equipment used of the present invention.
Wherein, label 1 sodium formate solution groove in the described accompanying drawing; 2 is high-pressure pump; 3 is hotblast stove; 4 is interchanger; 5 is dehydrogenation reactor; 6 is separator; 7 is waste gas outlet; 8 are the sodium oxalate outlet; 9 is hot-wind inlet; 10 is atomizer nozzle; 11 is the convergent-divergent pipe; 12 are the reaction gas outlet.
Embodiment
Liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology as shown in the figure comprises: the sodium formate solution of 48% concentration is passed through high-pressure pump 2, pumping hole pressure is 40kgf/cm, enter the surface-type heat exchanger 4 of hotblast stove top, make its temperature be increased to 200 ℃, directly be injected to by in the about 1000 ℃ hot gas flow that produces in the hotblast stove 3 by the nozzle 10 that is arranged on the spraying gun at hot gas flow center in the dehydrogenation reactor 5 again, sodium formate solution and hot gas flow are directly mixed, carry out heat exchange; Sodium formate solution ejection back diffusion is atomized into tiny drop (particle diameter is about 0.1mm), portion of water is evaporated by flash distillation, and mix with hot gas flow, at short notice, hot gas flow is cooled, sodium formate solution is heated, and makes sodium formate solution form the sodium formiate that exsiccant is the fine particle shape; Pass through convergent-divergent pipe 11 again, make itself and hot blast intense mixing once more, make the sodium formiate particle fully be heated to fusion, when temperature last and air-flow reached 400-500 ℃ simultaneously, sodium formiate generation dehydrogenation reaction generated sodium oxalate and hydrogen; Arrive air outlet 12 places and directly enter separator 6, hydrogen is discharged through separator with waste gas 7, and meanwhile, the resultant sodium oxalate is collected 8.Whole technological process is finished in continuous flow.
Wherein, the wind speed of hot gas flow ingress is 25m/s; The pressure at atomizer nozzle place is 30kgf/cm
2The wind speed at convergent-divergent pipe minimum diameter place is 70m/s; The wind speed in exit is 20m/s; Whole reactor cylindrical shell length is 8 meters; Barrel diameter is 300 millimeters; Distance between nozzle and the convergent-divergent pipe is 4 meters; The convergent-divergent pipe near nozzle one side's tube wall and drum shaft between angle be the 40-60 degree; Convergent-divergent pipe rear portion tube wall and drum shaft between angle be 30 the degree.
Claims (7)
1. liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology, it is characterized in that comprising sodium formate solution is heated to 180-205 ℃ earlier under condition of high voltage, again with 900-1050 ℃ hot gas flow by 1: the mixed of 2-5 is carried out sufficient heat exchange, make sodium formate solution through dehydration, fusion until dehydrogenation reaction takes place; Isolate hydrogen then, can obtain the resultant sodium oxalate.
2. liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology as claimed in claim 1, the concentration that it is characterized in that described sodium formate solution is 45-50%.
3. liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology as claimed in claim 1, it is characterized in that in the reaction process of dehydration, fusion and dehydrogenation of described sodium formate solution, the mixture velocity of itself and hot gas flow is increased to 50-80m/s by 15-25m/s in the scope of 8-10 rice, be contracted to 15-25m/s again.
4. one kind as arbitrary described liquid-spraying type sodium formiate dehydrogenating and producing sodium oxalate technology equipment used among the claim 1-3, it is characterized in that comprising hotblast stove, interchanger, dehydrogenation reactor, separator and high-pressure pump; Wherein said dehydrogenation reactor comprises reactor shell, and an end of cylindrical shell links to each other with the air outlet of hotblast stove, is provided with the atomizer nozzle identical with the hot blast wind direction near this air outlet place; Be provided with the convergent-divergent pipe that contraction gradually enlarges gradually again at the reactor middle part, the other end of cylindrical shell communicates with the separator inlet place.
5. equipment as claimed in claim 4 is characterized in that described cylindrical shell length is 8-10 rice; Barrel diameter is the 280-320 millimeter; Distance in the described cylindrical shell between nozzle and the convergent-divergent pipe is a 3-5 rice.
6. equipment as claimed in claim 4 is characterized in that gas flow rate is 15-20m/s in the described reactor; The gas flow rate of described convergent-divergent pipe at the minimum diameter place is 50-80m/s.
7. equipment as claimed in claim 4 is characterized in that also comprising with the venturi nozzle reactor substituting deoxidation reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02148873 CN1244534C (en) | 2002-11-22 | 2002-11-22 | Technological process for producing sodium oxalate by liquid-spraying type sodium formate dehydrogenation and use equipment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02148873 CN1244534C (en) | 2002-11-22 | 2002-11-22 | Technological process for producing sodium oxalate by liquid-spraying type sodium formate dehydrogenation and use equipment |
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| CN1502599A CN1502599A (en) | 2004-06-09 |
| CN1244534C true CN1244534C (en) | 2006-03-08 |
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| CN 02148873 Expired - Fee Related CN1244534C (en) | 2002-11-22 | 2002-11-22 | Technological process for producing sodium oxalate by liquid-spraying type sodium formate dehydrogenation and use equipment |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1903821B (en) * | 2006-08-01 | 2012-05-23 | 太原理工大学 | Technology of producing sodium oxalate by continuous dehydrogenation of sodium formate and its equipment |
| US9085827B2 (en) | 2012-07-26 | 2015-07-21 | Liquid Light, Inc. | Integrated process for producing carboxylic acids from carbon dioxide |
| US10329676B2 (en) | 2012-07-26 | 2019-06-25 | Avantium Knowledge Centre B.V. | Method and system for electrochemical reduction of carbon dioxide employing a gas diffusion electrode |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1319927C (en) * | 2004-07-26 | 2007-06-06 | 电子科技大学 | Method of microwave dehydrogenation for producing sodium oxalate |
| CN101077855B (en) * | 2006-05-23 | 2011-12-07 | 太原理工大学 | Technique and device for continuously dehydrogenating and producing sodium oxalate by dehydrogenation reaction remaining heat |
| CN1927805B (en) * | 2006-09-25 | 2012-05-09 | 太原理工大学 | Process and apparatus of preparing sodium oxalate by superheated steam ejecting mixing fast heating-up continuous dehydrogenation |
| CN102391099B (en) * | 2011-09-16 | 2014-12-10 | 罗田县富阳化肥有限公司 | Method and equipment for producing sodium oxalate through continuous dehydrogenation by two-fluid spraying |
-
2002
- 2002-11-22 CN CN 02148873 patent/CN1244534C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1903821B (en) * | 2006-08-01 | 2012-05-23 | 太原理工大学 | Technology of producing sodium oxalate by continuous dehydrogenation of sodium formate and its equipment |
| US9085827B2 (en) | 2012-07-26 | 2015-07-21 | Liquid Light, Inc. | Integrated process for producing carboxylic acids from carbon dioxide |
| US9175407B2 (en) | 2012-07-26 | 2015-11-03 | Liquid Light, Inc. | Integrated process for producing carboxylic acids from carbon dioxide |
| US10329676B2 (en) | 2012-07-26 | 2019-06-25 | Avantium Knowledge Centre B.V. | Method and system for electrochemical reduction of carbon dioxide employing a gas diffusion electrode |
| US11131028B2 (en) | 2012-07-26 | 2021-09-28 | Avantium Knowledge Centre B.V. | Method and system for electrochemical reduction of carbon dioxide employing a gas diffusion electrode |
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| CN1502599A (en) | 2004-06-09 |
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