CN1042624C - Pure-oxygen normal pressure synthesis process of liquid sulfur trioxide - Google Patents
Pure-oxygen normal pressure synthesis process of liquid sulfur trioxide Download PDFInfo
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- CN1042624C CN1042624C CN95110962A CN95110962A CN1042624C CN 1042624 C CN1042624 C CN 1042624C CN 95110962 A CN95110962 A CN 95110962A CN 95110962 A CN95110962 A CN 95110962A CN 1042624 C CN1042624 C CN 1042624C
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- gas
- convertor
- pipeline
- temperature
- oxygen
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Abstract
The present invention relates to a new method for synthesizing liquid sulfur trioxide in pure oxygen under normal pressure, which belongs to the technical field of inorganic chemistry non-metallic elements and compounds thereof, particularly to the method for preparing the liquid sulfur trioxide in sulfur and compounds thereof. The present invention is characterized in that the liquid sulfur trioxide is prepared by circularly reacting in the environment of pure oxygen, pure sulfur dioxide, normal temperature and pressure which is less than 0.03Mpa. The present invention has the advantages of normal temperature, low pressure, no high requirement of devices, low cost and high product purity, and can be built by depending on the local conditions but does not depend on a sulphuric acid plant, polymerization stabilizer agents are needless to add for storage and transportation, and the present invention is suitable for China's national conditions and is convenient for popularization and use.
Description
The invention belongs to inorganic chemistry non-metallic element and compound technical thereof, be specifically related to the preparation method of sulphur trioxide in sulphur and the compound thereof.
In recent years, the vulcanizing agent of home and abroad organic synthesis product begins to use gas, liquid sulphur trioxide, so the sulfan suitability for industrialized production is extensively paid attention to.Sulfan is very high because of gaseous phase partial pressure under normal pressure, so common vitriol works technology is with containing SO
3The gas system sulfan of 7～10% (volume all refers to molar percentage with lower volume) is impossible.
At present, domestic industry production, all the fuming acid with vitriol works's 20～25% free sulphur trioxides is a raw material, and it is heated to 110～130 ℃ in evaporating kettle, makes SO in the fuming acid
3Evaporation, sulfan is made in cooling again.The shortcoming of this method is: the residual sour SO in evaporating kettle
3Can not be lower than 15～16%, otherwise equipment corrosion is difficult to solution, therefore, this method must have a large amount of residual acid to return vitriol works.Owing to adopt high temperature evaporation technology still to have the etching problem of high temperature strong acid, safety in production is on the hazard in addition.
The external latter stage eighties, German Patent (DT2617893A1) method of sulfan " make " reported in literature pressurization pure oxygen method, this technology is: pure oxygen combustion sulphur is produced sulfurous gas, under the vanadium catalyst effect, generate high-concentration sulfur trioxide with oxygen again, after cooling, make the neat liquid sulphur trioxide.Unreacted gas is circulated to sulfur furnace by the compressor back of boosting.This production method can make the production sulfan become independent production equipment, need not to rely on vitriol works, but the shortcoming of this technology is: equipment and device need bear pressure, the equipment manufacturing cost height, and safety features are strict.In addition, recycle compressor shoulder seal is leaked to be difficult to resolve and is determined, so that this patented technology is applied difficulty at home is bigger.
Purpose of the present invention promptly designs the pure-oxygen normal pressure synthesis process of liquid sulfur trioxide that can base on our country existing installation material and manufacturing technology level, industrial scale can be flexible and changeable at above-mentioned shortcoming.
Technical scheme of the present invention is mainly as follows: the oxygen of oxygen level 〉=99.5% (volume) and pure SO
2Gas, import the recycle system through pipeline under at normal temperature, less than 0.03MPa pressure, after the circulation gas of system mixes, boost through recirculation blower, enter interchanger, and through the reacted hot gas heat exchange of convertor, reach the catalyst activity temperature of reaction, enter convertor through pipeline, under the contact of multilayer vanadium catalyst, produce following reaction:
Go out the convertor reactant gases, enter interchanger and unreacted gas converting heat makes it reach the active reaction temperature of catalyst, enter condenser through pipeline then through pipeline, by water or air cooling, SO in the gas at this moment
3Be condensed into liquid and be stored in the basin, and the SO that is not condensed
3Gas and unreacted oxygen and sulfur dioxide gas after pipeline enters recirculation blower and boosts, are circulated back to system through pipeline again, continue to participate in reaction, because at additional O
2And SO
2The time have the trace N
2Gas enters system, needs to go into device for recovering tail gas through pipeline, reclaims SO
2, SO
3Back indifferent gas emptying.
The key technical indexes scope of the present invention is as follows:
A, gas composition (volume)
a
1: replenish gas mixture
SO
3 0
SO
2 55～75
O
2 25～45
N
2Trace
a
2: the convertor air inlet
SO
3 30～40
SO
2 15～25
O
2 15～25
a
3: circulation gas
SO
3 ≥40
SO
2 10～20
O
2 15～25
B, system pressure (MPa)
b
1: recirculation blower import≤0.01
b
2: recirculation blower outlet≤0.03
C, temperature (℃)
c
1: convertor import 〉=430
c
2: convertor outlet≤600
c
3: cooling temperature 30～32
Gained liquid SO
3Quality product is as follows:
1, SO
3(weight percent) 〉=98%
2, dissolved SO
2, O
2, N
2(weight percent)≤2%
Below in conjunction with Fig. 1 the embodiment of the invention is described in detail:
Fig. 1 is a process block synoptic diagram of the present invention.
From air separation technology 〉=the pure SO of the oxygen 1 of 99.5% (volume) and pure oxygen combustion sulphur
2Gas 2 is (or through vaporised liquid SO
2After pure SO
2Gas), under normal temperature, 0.005MPa pressure, import the recycle systems 11 through pipeline 3, after the circulation gas 11 of system mixes, boost after pipeline 13 enters interchanger 4 through recirculation blower 12, with through convertor 7 reacted hot gas heat exchanges, reach the catalyst activity temperature of reaction and enter convertor 7, under the contact of multilayer vanadium catalyst, produce following reaction through pipeline 6:
Go out 590 ℃ of convertor 7 reactant gases temperature, enter interchanger 4 and unreacted gas converting heat, make its active reaction temperature that reaches catalyst, enter condenser 10 through pipeline 9, be chilled to 31 ℃ by water or air, at this moment SO in the gas and itself reduce to 150 ℃ through pipeline 8
3Be condensed into liquid and be stored in the basin 15 through pipeline 5, and the SO that is not condensed
3With unreacted oxygen and sulfur dioxide gas after pipeline 11 enters recirculation blower 12 and boosts, be circulated back to system through pipeline 13 and continue reaction, because at additional O
2And SO
2The time N of 0.2% (volume) arranged
2Gas enters system, needs to enter device for recovering tail gas 16 through pipeline 14, reclaims SO
2, SO
3Back rare gas element emptying, 17 is sour pump among the figure.Present embodiment is finished under following condition:
A, gaseous fraction (volume)
a
1: replenish gas mixture
SO
3 0
SO
2 65
O
2 33
N
20.2a
2: the convertor air inlet
SO
3 34
SO
2 24
O
2 23
N
219a
3: circulation gas
SO
3 42
O
2 21
N
223B, system pressure (MPa)
b
1: recirculation blower import 0.005
b
2: recirculation blower outlet 0.025C, temperature (℃)
c
1: convertor import 410
c
2: convertor outlet 590
c
3: cooling temperature 31 gained liquid SO
3Quality product is as follows: 1, SO
3(weight percent) 〉=98%2, dissolved SO
2, O
2, N
2(weight percent)≤2% the present invention can be based on domestic existing installation, material and manufacture level owing to normal temperature, pressure are low, and general carbon steel equipment can use, and recirculation blower is domestic can be made, and can solve the shoulder seal problem.Industrial scale can be flexible and changeable, need not rely on vitriol works, can suit measures to local conditions to found the factory, and saves great amount of investment, and product is convenient to storing, and cost is suitable with the fuming acid method of evaporation.Because of raw material is sulfur dioxide liquid and pure oxygen, so raw material does not contain moisture content and sulfuric acid impurity, therefore stablize aborning with in the product storing, can SO not take place because of moisture and sulfuric acid impurity
3The polymerization modification generates the crystallization of infusible sulphur trioxide, therefore need not add anti-polymerization stabilizer in storing.Compare with the pressure oxidation method, because of the present invention produces under normal pressure, branch forces down, so liquid SO
3Middle dissolved SO
2Low, do not need redistillation with SO
2Remove, can obtain purer liquid SO
3Compare with the fuming acid method of evaporation, can avoid serious, the drawbacks such as safety in production is on the hazard, residual acid treatment inconvenience of equipment corrosion, should promote the use of.
Claims (2)
1. pure-oxygen normal pressure synthesis process of liquid sulfur trioxide, it is characterized in that: the oxygen of oxygen level 〉=99.5% and pure sulfur dioxide gas, under at normal temperature, less than 0.03MPa pressure, after pipeline is imported the recycle system and the circulation gas of system is mixed, boost through recirculation blower, enter interchanger, with through the reacted hot gas heat exchange of convertor, reach the catalyst activity temperature of reaction, enter convertor, under the effect of multilayer vanadium catalyst, produce following reaction through pipeline:
Go out the convertor reactant gases, enter interchanger and unreacted gas converting heat makes it reach the active reaction temperature of catalyst, enter condenser through pipeline then through pipeline, by water or air cooling, SO in the gas
3Be condensed into liquid, be stored in the basin, and the sulfur trioxide gas that is not condensed and unreacted oxygen and sulfur dioxide gas, after pipeline enters recirculation blower and boosts, be circulated back to system through pipeline again, continue to participate in reaction, in supplemental oxygen and sulfur dioxide gas, there is micro-nitrogen to enter system, need manage line and enter device for recovering tail gas, with micro-nitrogen purge, above-mentioned technology is finished under following condition: A, gaseous fraction (volume) a behind recovery sulfurous gas, the sulphur trioxide
1: replenish gas mixture
SO
3 0
SO
3 55～75
O
2 25～45
N
2Trace a
2: the convertor air inlet
SO
3 30～40
SO
2 15～25
O
2 15～25
N
210～20a
3: circulation gas
SO
3 ≥40
SO
2 10～20
O
2 15～25
N
210～25B, system pressure (MPa)
b
1: recirculation blower import≤0.01
b
2: recirculation blower outlet≤0.03C, temperature (℃)
c
1: convertor import 〉=430
c
2: convertor outlet≤600
c
3: cooling temperature 30～32
2, novel process according to claim 1 is characterized in that technic index is as follows:
A, gaseous fraction (volume)
a
1: replenish gas mixture
SO
3 0
SO
2 65
O
2 33
N
2 0.2
a
2: the convertor air inlet
SO
3 34
SO
2 24
O
2 23
N
2 19
a
3: circulation gas
SO
3 42
SO
2 14
O
2 21
N
2 23
B, system pressure (MPa)
b
1: recirculation blower import 0.005
b
2: recirculation blower outlet 0.025
C, temperature (℃)
c
1: convertor import 410
c
2: convertor outlet 590
c
3: cooling temperature 31
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95110962A CN1042624C (en) | 1995-03-09 | 1995-03-09 | Pure-oxygen normal pressure synthesis process of liquid sulfur trioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95110962A CN1042624C (en) | 1995-03-09 | 1995-03-09 | Pure-oxygen normal pressure synthesis process of liquid sulfur trioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1134396A CN1134396A (en) | 1996-10-30 |
| CN1042624C true CN1042624C (en) | 1999-03-24 |
Family
ID=5078288
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95110962A Expired - Fee Related CN1042624C (en) | 1995-03-09 | 1995-03-09 | Pure-oxygen normal pressure synthesis process of liquid sulfur trioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1042624C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030059363A1 (en) * | 2001-09-26 | 2003-03-27 | Shah Chetan K. | Oxygen enrichment of a sulfuric acid plant furnace |
| DE102004022506B4 (en) * | 2004-05-05 | 2012-06-21 | Outokumpu Oyj | Process and plant for the production of sulfuric acid from sulfur dioxide-rich gases |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2814437A1 (en) * | 1977-04-05 | 1978-10-19 | Boc Ltd | METHOD OF CATALYTIC OXADATION OF SULFUR DIOXIDE |
-
1995
- 1995-03-09 CN CN95110962A patent/CN1042624C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2814437A1 (en) * | 1977-04-05 | 1978-10-19 | Boc Ltd | METHOD OF CATALYTIC OXADATION OF SULFUR DIOXIDE |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1134396A (en) | 1996-10-30 |
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