CN108328583B - A kind of production technology of refined sulfuric acid reagent - Google Patents
A kind of production technology of refined sulfuric acid reagent Download PDFInfo
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- CN108328583B CN108328583B CN201810289300.4A CN201810289300A CN108328583B CN 108328583 B CN108328583 B CN 108328583B CN 201810289300 A CN201810289300 A CN 201810289300A CN 108328583 B CN108328583 B CN 108328583B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of production technologies of refined sulfuric acid reagent, belong to sulphate reagent production field.A kind of production technology of refined sulfuric acid reagent, the following steps are included: S1, choose petroleum refinery's gas, natural gas, the unpurified low-grade sulfur waste sulphur relatively low containing sulfur grade is made in oven gas recycling, raw material may be implemented using petroleum refinery's gas in it, natural gas, the sulfur waste sulphur of oven gas recycling is as raw material, mode is mixed using slag and low-grade sulfur waste sulphur, realize the reasonable utilization of more low-grade sulfur-bearing waste, it is simple that coking number cleaning operation is effectively reduced, operating cost is lower, quartz sand and pyrite cinder can be realized recycling as carrier, reduce energy consumption, pure air preparation system, save drying equipment investment, avoid the consumption of the drying process concentrated sulfuric acid, reduce energy consumption, SO in production process3It is handled by desorption tower, then utilizes evaporator rectification and purification SO3, reagent of sulfuric acid purity is high obtained.
Description
Technical field
The present invention relates to sulphate reagent production fields, more specifically to a kind of production technology of refined sulfuric acid reagent.
Background technique
Refined sulfuric acid reagent is highly important reagent on chemical industry, at present in extracting sulfuric acid, for high sulfur-bearing
The sulfur-bearing waste of amount mostly uses the mode for directly entering the pure burning of furnace to generate SO at present2Gas is consequently facilitating relieving haperacidity, and this mode is to low
The waste of sulfur content will cause in this way coking number increase with cleaning operation difficulty, and at present Sulphuric acid technique
In drying tower apparatus be mostly it is dry by the concentrated sulfuric acid, the consumption of the concentrated sulfuric acid is big, and investment is high, at high cost, in addition current work
Skill energy consumption is higher, and operating cost is high, and sulfuric acid product purity is low.
Summary of the invention
1. technical problems to be solved
Aiming at the problems existing in the prior art, the purpose of the present invention is to provide a kind of production works of refined sulfuric acid reagent
Skill, it may be implemented, and cleaning operation is simple, and low energy consumption is at low cost, and product purity is high.
2. technical solution
To solve the above problems, the present invention adopts the following technical scheme that.
A kind of production technology of refined sulfuric acid reagent, comprising the following steps:
S1, choose petroleum refinery's gas, natural gas, oven gas recycling are made unpurified containing relatively low low-grade of sulfur grade
Sulfur waste sulphur, main component accounting are respectively as follows:
Sulphur: 56-62%
Moisture: 28-32%
Organic matter: 3-6%
Oxide impurity: 4-7%
Choose petroleum refinery's gas, natural gas, the obtained height relatively high containing sulfur grade by processing purification of oven gas recycling
Grade sulfur waste sulphur, main component accounting are respectively as follows:
Sulphur: 78-82%
Moisture: 6-10%
Organic matter: 4-8%
Oxide impurity: 4-8%
Slag is chosen, the slag is made of quartz sand and pyrite cinder, and the silica of quartz sand main component
Accounting >=98.5%, silica accounting >=70% of pyrite cinder main component；
S2, the low-grade sulfur waste sulphur by step S1, high-grade sulfur waste sulphur, slag carry out break process respectively, and respectively
Sieve the low-grade sulfur waste sulphur of feeding granularity≤6mm, high-grade sulfur waste sulphur, slag；
S3, it the low-grade sulfur waste sulphur and slag that sieve in step S2 mix is mixed and made into mixed raw material, the two is matched
Material accounting is respectively 48-52% and 48-52%, so that the furnace sulfur content that enters of mixed raw material is 38-42%, enters furnace moisture content≤8%；
S4, the mixed raw material in step S2 sieve the high-grade sulfur waste sulphur and step S3 that take is entered into boiling roaster；
S5, the gas that step S4 roasting is formed later is introduced into cyclone dust collectors, main component has SO in gas2, it is a small amount of
CO2, a small amount of solid particulate matter, the solid particulate matter after first and second grade of cyclone dust removal of cyclone dust collectors in gas is through whirlwind
The slag discharge drum of deduster is discharged；
S6, will by cyclone dust collectors, treated that gas is passed through SO in step S52Analytic Tower is handled, the SO2Solution
It analyses dry air used in tower to be made using pure air preparation system, CO2With air emptying, SO after purified, conversion, tail gas2
Gas is purified, it is dry after enter converter by SO2It is converted into SO3, convert the SO of formation3It is passed through desorption tower removal SO2, pass through
The SO that desorption tower desorption is completed3Into evaporator rectification and purification SO3, it is passed through in water and reagent of sulfuric acid is made.
The sulfur waste sulphur that raw material is recycled using petroleum refinery's gas, natural gas, oven gas reduces energy consumption as raw material, at
This is low, before entering furnace and being roasted, mixes mode using slag and low-grade sulfur waste sulphur, realizes more low-grade sulfur-bearing waste
Reasonable utilization, be effectively reduced that coking number cleaning operation is simple, and operating cost is lower, slag uses quartz sand and pyrite
Cost is relatively low for slag, and quartz sand and pyrite cinder can be realized recycling as carrier, reduce energy consumption, pure air
Preparation system saves drying equipment investment, avoids the consumption of the drying process concentrated sulfuric acid, reduce energy consumption, produced
SO in journey3It is handled by desorption tower, then utilizes evaporator rectification and purification SO3, reagent of sulfuric acid purity is high obtained.
Preferably, fluidized bed furnace used in the step S4, boiling furnace gas pipeline in the middle part of and first group of steaming of waste heat boiler
Hair device corresponding position installs one group of shock wave generator respectively.
Preferably, the waste heat that evaporator is generated using converter work conversion in the step S6 is as evaporation heat source.
Preferably, 800~900 DEG C of furnace temperature are controlled when fluidized bed furnace is roasted in the step S4, furnace bottom pressure is 1240-
1260mmH2O column.
Preferably, evaporator is made of stainless steel in the step S6, and heating temperature is 130-134 when evaporation
℃。
Preferably, the pure air preparation system include screw air compressor, it is air accumulator, oil water separator, cold dry
Machine, first filter and the second filter, air pass sequentially through screw air compressor, air accumulator, oil water separator, cold dry
Enter SO after machine, first filter and the processing of the second filter purge2Analytic Tower.
Preferably, desorption tower uses bubbler desorption tower in the step S6, and bubbler desorption tower is generally void tower, in order to
Increase gas liquid interfacial area and reduce back-mixing, the addition filler in tower, using tetrafluoro silk filler, tetrafluoro silk filler is thermopnore.
3. beneficial effect
Compared with the prior art, the present invention has the advantages that
(1) the sulfur waste sulphur that the raw material of this programme is recycled using petroleum refinery's gas, natural gas, oven gas is reduced as raw material
Energy consumption, it is at low cost, before entering furnace and being roasted, mode is mixed using slag and low-grade sulfur waste sulphur, is realized lower
The reasonable utilization of grade sulfur-bearing waste, is effectively reduced that coking number cleaning operation is simple, and operating cost is lower, and slag is using quartz
Cost is relatively low for sand and pyrite cinder, and quartz sand and pyrite cinder can be realized recycling as carrier, reduce the energy
Consumption, pure air preparation system save drying equipment investment, avoid the consumption of the drying process concentrated sulfuric acid, reduce energy
Source consumes, the SO in production process3It is handled by desorption tower, then utilizes evaporator rectification and purification SO3, reagent of sulfuric acid obtained
Purity is high.
Specific embodiment
Below in conjunction in the embodiment of the present invention；Technical solution in the embodiment of the present invention is clearly and completely retouched
It states；Obviously；Described embodiments are only a part of the embodiments of the present invention；Instead of all the embodiments.Based on the present invention
In embodiment；Every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example；It shall fall within the protection scope of the present invention.
Embodiment 1:
A kind of production technology of refined sulfuric acid reagent, comprising the following steps:
S1, choose petroleum refinery's gas, natural gas, oven gas recycling are made unpurified containing relatively low low-grade of sulfur grade
Sulfur waste sulphur, main component accounting are respectively as follows:
Sulphur: 59%
Moisture: 30%
Organic matter: 5%
Oxide impurity: 6%
Choose petroleum refinery's gas, natural gas, the obtained height relatively high containing sulfur grade by processing purification of oven gas recycling
Grade sulfur waste sulphur, main component accounting are respectively as follows:
Sulphur: 80%
Moisture: 8%
Organic matter: 6%
Oxide impurity: 6%
Slag is chosen, slag is made of quartz sand and pyrite cinder, and the silica accounting of quartz sand main component
It is 99%, the silica accounting of pyrite cinder main component is 75%；
S2, the low-grade sulfur waste sulphur by step S1, high-grade sulfur waste sulphur, slag carry out break process respectively, and respectively
Sieve the low-grade sulfur waste sulphur of feeding granularity≤6mm, high-grade sulfur waste sulphur, slag；
S3, it the low-grade sulfur waste sulphur and slag that sieve in step S2 mix is mixed and made into mixed raw material, the two is matched
Material accounting is respectively 50% and 50%, so that the furnace sulfur content that enters of mixed raw material is 40%, entering furnace moisture content is 7%；
S4, the mixed raw material in step S2 sieve the high-grade sulfur waste sulphur and step S3 that take is entered into boiling roaster, boiled
In the middle part of furnace gas pipeline and first group of evaporator corresponding position of waste heat boiler installs one group of shock wave generator respectively；Due to sulfur-bearing waste
There are many powder, some meticulous powder are when entering furnace, there are no having enough time falling on boiling bed burning, just by air-flow
Entrainment moves up, and burns in upper furnace, is easy to be adhered in inner wall of the pipe under conditions of having fusion temperature and forms coking,
If taking manual cleaning, it will cause and stop for a long time, operating environment is also very poor, interferes shock-wave ash-clearing principle using same frequency, real
The not parking deashing of present line, per tour cleaning is primary, preferably solves lime-ash cleaning problem, creates item for production stable operation
Part；800~900 DEG C of furnace temperature are controlled when fluidized bed furnace is roasted, furnace bottom pressure is 1240-1260mmH2O column realizes sulfur-bearing waste
Full combustion.
S5, the gas that step S4 roasting is formed later is introduced into cyclone dust collectors, main component has SO in gas2, it is a small amount of
CO2, a small amount of solid particulate matter, the solid particulate matter after first and second grade of cyclone dust removal of cyclone dust collectors in gas is through whirlwind
The slag discharge drum of deduster is discharged；
S6, will by cyclone dust collectors, treated that gas is passed through SO in step S52Analytic Tower is handled, SO2Analytic Tower
Dry air used is made using pure air preparation system, CO2With air emptying, SO after purified, conversion, tail gas2Gas
Enter converter after purified, dry by SO2It is converted into SO3, convert the SO of formation3It is passed through desorption tower removal SO2, by desorption
The SO that tower desorption is completed3Into evaporator rectification and purification SO3, it is passed through in water and reagent of sulfuric acid is made, evaporator is worked using converter
The waste heat that conversion generates has saved the energy as evaporation heat source；
Desorption tower uses bubbler desorption tower in step S6, and bubbler desorption tower is generally void tower, connects to increase gas-liquid
Contacting surface product and reduction back-mixing, the addition filler in tower, using tetrafluoro silk filler, tetrafluoro silk filler is thermopnore, be may be implemented more
High air velocity and mass-transfer efficiency is full of sulfuric acid in bubbler desorption tower, does not need acid separating device, air from tower bottom into
Enter, be dispersed into bubble and rise along liquid, both contacted with liquid phase, while stirring liquid to increase mass-transfer efficiency, this desorption tower
Structure is simple, low cost, easy to control, easy-maintaining, anticorrosion are easy to solve, and effectively absorbs SO3Present in SO2, it is ensured that
SO3Purity.
Evaporator is made of stainless steel, the SO that rectifying obtains3Sulfuric acid concentration is 105%, and heating temperature is when evaporation
132 DEG C, 98% concentrated sulfuric acid need to be heated to 327 DEG C by the common way of distillation, evaporate the concentrated sulfuric acid, can be by sulfuric acid purification with the way of distillation；Work
The sulfate of most of impurity such as iron, arsenic (pentavalent), heavy metal formation precipitating in sulfuric acid heating distillation process in industry sulfuric acid
Stay in vinasse, and chloride, nitrate, ammonium salt decomposition release gas, distillate temperature reach sulfuric acid boiling point it
It is preceding just to escape；Therefore, when being evaporated to sulfuric acid boiling temperature, acquired condensate liquid is just the higher sulfuric acid of purity, still, this
Kind sulfuric acid is escaped at gaseous state with sulfuric acid vapor because there are also a small amount of impurity in distillation process, stays in condensation also with its condensation
In acid, so, i.e., make raw material using primes industrial sulphuric acid, the condensation acid that a full range steams is also seldom all qualified, usually
The condensation acid of only midbarrel is qualified, thus if producing reagent of sulfuric acid with the way of distillation merely it is necessary to cut off fraction end to end
Or the cold acid for obtaining fore-running in this way, just extending the activity duration, influences yield and yield, increases from second of distillation is carried out again
Cost；The absorption process that this technique uses must break the higher oleum of purity, need to only be heated to the oleum of 105% concentration
133 DEG C of free sulfur trioxides will overflow, and avoid that heavy metal and chloride, nitrate etc. are miscellaneous to be mixed into, and ensure that three oxidations
The purity of sulphur；In addition it avoids that oxidizing agent scavenging increasing is added in first 98% concentrated sulfuric acid solution of the common way of distillation of the addition of sulfuric acid purification agent
Behaviour has been added to do difficulty and cost；The sulfur trioxide purity is high of this technique, avoids the addition of cleanser, reduces costs.
Pure air preparation system includes screw air compressor, air accumulator, oil water separator, cooling driers, the first filtering
Device and the second filter, air pass sequentially through screw air compressor, air accumulator, oil water separator, cooling driers, first filter
Enter SO with after the processing of the second filter purge2Analytic Tower is dried air without concentrated sulfuric acid drying mode, reduces
The consumption of the concentrated sulfuric acid, technique realize small investment, and the completion time of project is short, reduces energy consumption.
The sulfur waste sulphur recycled using petroleum refinery's gas, natural gas, oven gas reduces energy consumption as raw material, at low cost,
Before entering furnace and being roasted, mode is mixed using slag and low-grade sulfur waste sulphur, realizes the conjunction of more low-grade sulfur-bearing waste
Reason utilizes, and is effectively reduced that coking number cleaning operation is simple, and operating cost is lower, slag using quartz sand and pyrite cinder at
This is lower, and quartz sand and pyrite cinder can be realized recycling as carrier, reduce energy consumption, and pure air is produced
System saves drying equipment investment, avoids the consumption of the drying process concentrated sulfuric acid, reduce energy consumption, in production process
SO3It is handled by desorption tower, then utilizes evaporator rectification and purification SO3, reagent of sulfuric acid purity is high obtained.
It is described above；It is merely preferred embodiments of the present invention；But scope of protection of the present invention is not limited thereto；
Anyone skilled in the art is in the technical scope disclosed by the present invention；According to the technique and scheme of the present invention and its
It improves design and is subject to equivalent substitution or change；It should be covered by the scope of protection of the present invention.
Claims (7)
1. a kind of production technology of refined sulfuric acid reagent, which comprises the following steps:
The unpurified low-grade sulfur waste relatively low containing sulfur grade is made in S1, selection petroleum refinery's gas, natural gas, oven gas recycling
Sulphur, main component accounting are respectively as follows:
Sulphur: 56-62%
Moisture: 28-32%
Organic matter: 3-6%
Oxide impurity: 4-7%
Choose petroleum refinery's gas, natural gas, the obtained high-grade relatively high containing sulfur grade by processing purification of oven gas recycling
Sulfur waste sulphur, main component accounting are respectively as follows:
Sulphur: 78-82%
Moisture: 6-10%
Organic matter: 4-8%
Oxide impurity: 4-8%
Slag is chosen, the slag is made of quartz sand and pyrite cinder, and the silica accounting of quartz sand main component
>=98.5%, silica accounting >=70% of pyrite cinder main component；
S2, the low-grade sulfur waste sulphur by step S1, high-grade sulfur waste sulphur, slag carry out break process respectively, and sieve takes respectively
The low-grade sulfur waste sulphur of material granularity≤6mm, high-grade sulfur waste sulphur, slag；
S3, it the low-grade sulfur waste sulphur and slag that sieve in step S2 mix is mixed and made into mixed raw material, the two ingredient accounts for
Enter furnace moisture content≤8% so that the furnace sulfur content that enters of mixed raw material is 38-42% than being respectively 48-52% and 48-52%；
S4, the mixed raw material in step S2 sieve the high-grade sulfur waste sulphur and step S3 that take is entered into boiling roaster；
S5, the gas that step S4 roasting is formed later is introduced into cyclone dust collectors, main component has SO in gas2, a small amount of CO2, it is few
Solid particulate matter is measured, the solid particulate matter after first and second grade of cyclone dust removal of cyclone dust collectors in gas is through cyclone dust collectors
Slag discharge drum discharge；
S6, will by cyclone dust collectors, treated that gas is passed through SO in step S52Analytic Tower is handled, the SO2Analytic Tower
Dry air used is made using pure air preparation system, CO2With air emptying, SO after purified, conversion, tail gas2Gas
Enter converter after purified, dry by SO2It is converted into SO3, convert the SO of formation3It is passed through desorption tower removal SO2, by desorption
The SO that tower desorption is completed3Into evaporator rectification and purification SO3, it is passed through in water and reagent of sulfuric acid is made.
2. a kind of production technology of refined sulfuric acid reagent according to claim 1, it is characterised in that: make in the step S4
Fluidized bed furnace, in the middle part of boiling furnace gas pipeline and first group of evaporator corresponding position of waste heat boiler installs one group of shock wave hair respectively
Raw device.
3. a kind of production technology of refined sulfuric acid reagent according to claim 1, it is characterised in that: steamed in the step S6
Device is sent out using the waste heat of converter work conversion generation as evaporation heat source.
4. a kind of production technology of refined sulfuric acid reagent according to claim 1, it is characterised in that: boiled in the step S4
It rises and controls 800~900 DEG C of furnace temperature when furnace is roasted, furnace bottom pressure is 1240-1260mmH2O column.
5. a kind of production technology of refined sulfuric acid reagent according to claim 1, it is characterised in that: steamed in the step S6
Hair device is made of stainless steel, and heating temperature is 130-134 DEG C when evaporation.
6. a kind of production technology of refined sulfuric acid reagent according to claim 1, it is characterised in that: the pure air system
Taking system includes screw air compressor, air accumulator, oil water separator, cooling driers, first filter and the second filter, air
It passes sequentially through at screw air compressor, air accumulator, oil water separator, cooling driers, first filter and the second filter purge
Enter SO after reason2Analytic Tower.
7. a kind of production technology of refined sulfuric acid reagent according to claim 1, it is characterised in that: taken off in the step S6
It inhales tower and uses bubbler desorption tower, bubbler desorption tower is generally void tower, in order to increase gas liquid interfacial area and reduce back-mixing,
Addition filler in tower, using tetrafluoro silk filler, tetrafluoro silk filler is thermopnore.
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| CN1058247C (en) * | 1998-04-03 | 2000-11-08 | 云南磷肥厂 | Method for preparing sulphuric acid by baking sulphur in fluidized-bed furnace |
| CN1456494A (en) * | 2003-05-09 | 2003-11-19 | 湖北宜化化工股份有限公司 | Production of sulphuric acid by firing sulphur with mixed sulphureous iron ore |
| CN102745651A (en) * | 2012-07-17 | 2012-10-24 | 威海恒邦化工有限公司 | Energy-saving and environmental-friendly method for heating fluidized bed furnace |
| CN105293448B (en) * | 2015-10-23 | 2018-01-30 | 湖北祥云(集团)化工股份有限公司 | A kind of method of Recovered sulphur slag and pyrite-based sulfuric acid production |
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