CN105197897B - A kind of high-temperature fusion salt processing method rich in CaSO4 materials - Google Patents
A kind of high-temperature fusion salt processing method rich in CaSO4 materials Download PDFInfo
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- CN105197897B CN105197897B CN201510566908.3A CN201510566908A CN105197897B CN 105197897 B CN105197897 B CN 105197897B CN 201510566908 A CN201510566908 A CN 201510566908A CN 105197897 B CN105197897 B CN 105197897B
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Abstract
The present invention relates to a kind of be rich in CaSO4The high-temperature fusion salt processing method of material, belongs to metallurgical and technical field of environmental protection in chemical industry.First melting salt system is put in molten salt reaction device, is added rich in CaSO from the top of molten salt reaction device4Material, then from molten salt reaction device bottom nitrogen, carbonaceous reducing agent nitrogen buffer gas are reacted from bottom into molten salt reaction device, prepare SO2And CO2Gaseous mixture and CaO, the SO of generation2And CO2Gaseous mixture is flowed out from the top of molten salt reaction device, obtains rich SO after condensed device condensation, purification2Tail gas finally carries out antacid；The CaO for obtaining gradually sinks to bottom, CaO and fuse salt are together imported CaO separators after the completion of reaction to obtain CaO and fuse salt, fuse salt enters first fuse salt storage tank Jing after fuse salt cleaning system is processed, then entered in heater by fuse salt blood circulation and heated, finally enter to go to second fuse salt storage tank so as to stream enters molten salt reaction device.The invention enables CaSO4The processing cost of material is reduced.
Description
Technical field
The present invention relates to a kind of be rich in CaSO4The high-temperature fusion salt processing method of material, belongs to metallurgical and chemical industry environmental protection skill
Art field.
Background technology
At present, produce in industrial processes rich in CaSO4Material ardealite, desulfurated plaster, Calx iron salt method give up
Sewage sludge etc. belongs to solid waste, and which part still falls within danger wastes.
Rich in CaSO4Material belong to greatly industrial solid castoff, metallurgical industry all produces substantial amounts of solid waste every year,
Show according to correlation report, up to 2,000,000,000 tons of the industrial solid castoff that China stores up up to now, only China's non-ferrous metal metallurgy
Industry will produce the solid waste more than 70,000,000 tons every year.
By taking cupper smelting as an example, China is Copper making big producing country, due to copper sustained production rapid growth in recent years, is led
Copper pyrometallurgy enterprise is caused to need every year to process in a large number containing heavy metal and the acid waste water containing arsenic, a large amount of spent acidics containing heavy metal
Water produces substantial amounts of solid slag, referred to as copper sludge Jing after waste water treatment process process, and copper sludge just belongs to one kind and is rich in
CaSO4Material.Further, in phosphorous chemical industry field, about 75,000,000 tons of national ardealite yield in 2014, volume of cargo in storage is up to 2.5
Hundred million tons.Country and industry put into effect market access requirements, design atlas, construction, when technical regulation, over more than 20 years entirely
Guo20Duo Ge provinces and cities all Devoting Major Efforts To Developing application ardealites.But, the utilization rate of ardealite in 2014 still only 25% or so, and
It is only used for cement retarder and plaster of Paris etc..With global industry development continuously and healthily, people anticipate to ecological environmental protection
The enhancing of knowledge, therefore, these how effectively and reasonably, are scientifically processed rich in CaSO4Material has caused relevant industries and Chinese Ministry of Environmental Protection
Its innoxious and recycling treatment will be become the metallurgical emphasis with environmental worker's research both at home and abroad by paying close attention to for door.
This patent is sought out a kind of new rich in CaSO4The method of disposal of material-high-temperature fusion salt treatment method, it is reason to believe that, this is not
Certain economic benefit can only be produced, prior is its environmental benefit for bringing and social benefit.
The content of the invention
The problem existed for above-mentioned prior art and deficiency, the present invention provide a kind of rich in CaSO4The high temperature melting of material
Melt salt processing method.The present invention uses carbonaceous reducing agent under melting salt system（Coal, coke, natural gas etc.）Come as reducing agent
Reduction decomposition CaSO4Produce SO2With CaO, SO2Can be used for antacid, CaO can make industrial chemicals.Fuse salt plays reaction medium and storage
The function of heat release, both can reach energy-saving purpose, be avoided that the generation of course of reaction focus and the three wastes again, for processing richness
Containing CaSO4Material can avoid slagging scorification, be conducive to consecutive production.The system of the present invention takes full advantage of CaSO4In material, Ca is first
Element and S elements so that CaSO4The processing cost of material obtains larger reduction, and the present invention is achieved through the following technical solutions.
It is a kind of to be rich in CaSO4The high-temperature fusion salt processing method of material, which comprises the following steps that：
（1）Process rich in CaSO4The high-temperature fusion salt treatment device of material includes molten salt reaction device, CaO separators, melts
Melt salt holding vessel and fuse salt storage heating system；
（2）Melting salt system is heated to 1323K ~ 1423K first to put in molten salt reaction device, from molten salt reaction
Add at the top of device rich in CaSO4 materials, then flow is passed through for 100 ~ 800Ncm from molten salt reaction device bottom3·min-1Nitrogen
Gas, carbonaceous reducing agent nitrogen buffer gas carry out reaction 0.5 ~ 10h into molten salt reaction device from bottom, prepare SO2With
CO2Gaseous mixture and CaO, the SO of generation2And CO2Gaseous mixture is flowed out from the top of molten salt reaction device, condensed device condensation, purification
After obtain rich SO2Tail gas finally carries out antacid；
（3）Step（2）The CaO for preparing gradually sinks to bottom, after the completion of reaction together imports CaO and fuse salt
CaO separators（As both density is different, upper strata is fuse salt, and lower floor is calcium oxide, can be by by existing separator
Fuse salt is separated with calcium oxide）Obtain CaO and fuse salt, fuse salt is Jing after fuse salt cleaning system is processed（Cleaning will be floated
Float over the obvious residue above fuse salt to clean out）Into first fuse salt storage tank, then circulated by fuse salt
System is entered in heater and is heated, and finally enters to go to second fuse salt storage tank so as to stream enters molten salt reaction device（Select two
Individual fuse salt holding vessel be for the ease of control production process, improve safety coefficient, fuse salt major storage in two jars,
One high temperature, a low temperature, once there are leakage or other situations, the fuse salt of whole flow process can be stored by two jars
Get up）.
The step（1）In rich in CaSO4Material is copper sludge or ardealite.Rich in CaSO4Material accounts for fuse salt quality
Ratio be 5 ~ 40%.
The step（2）Middle melting salt system is Na2CO3、K2CO3、Li2CO3In one kind, two or three of mixing
Thing, during two kinds of mixture, mass ratio is 0.5 ~ 1.5:0.5 ~ 1.5, during three kinds of mixture, mass ratio is 0.5 ~ 1.5：0.5~1.5：
0.5~1.5。
The step（2）Middle carbonaceous reducing agent is coal, coke or natural gas, the addition of carbonaceous reducing agent be rich in
CaSO4CaSO in material4Mol ratio with carbon in carbonaceous reducing agent is 1.5 ~ 2.0：1.
The invention has the beneficial effects as follows：
（1）Reaction is carried out in melting salt system, and the dynamic conditions and thermodynamic condition of reaction is extremely superior so that anti-
Should extremely be easily controlled, leave freely measuring for engineering design and actual production link for very well-to-do；
（2）Reaction is carried out in melting salt system, makes reaction temperature field more by the superior heat-conductive characteristic of fuse salt
Uniformly, it is to avoid the generation of hot issue, reaction is made to be more easy to carry out；
（3）Using the heat storage function of fuse salt, the waste heat major part after reaction is made to be stored in fuse salt, fuse salt is followed
Ring is used, while improving the systematic heat utilization rate of gaseous mixture and CaO, reaches energy-saving purpose；
（4）The fuse salt method of disposal and traditional reduction decomposition CaSO4Material is compared, and reaction tail waste gas is extremely easily controlled
System, will not be eco-friendly rich in CaSO to the poisonous and hazardous pollutant of airborne release4The method of disposal of material；
（5）Whole technological process is short, the problems such as can avoid slagging scorification present in fixed bed or reacting in rotary kiln process.
Description of the drawings
Fig. 1 is present invention process flow chart.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
As shown in figure 1, should be rich in CaSO4The high-temperature fusion salt processing method of material, which comprises the following steps that：
（1）Process rich in CaSO4The high-temperature fusion salt treatment device of material includes molten salt reaction device, CaO separators, melts
Melt salt holding vessel and fuse salt storage heating system；CaSO is rich in wherein4Material is ardealite, its mass percent composition such as table
Shown in 1；
Table 1
（2）Melting salt system is heated to 1323K first to put in molten salt reaction device, from the top of molten salt reaction device
Add rich in CaSO4Material, is then passed through flow for 100Ncm from molten salt reaction device bottom3·min-1Nitrogen, carbonaceous is also
Former agent nitrogen buffer gas carry out reaction 2h into molten salt reaction device from bottom, prepare SO2And CO2Gaseous mixture and
CaO, the SO of generation2And CO2Gaseous mixture is flowed out from the top of molten salt reaction device, obtains rich SO after condensed device condensation, purification2Tail
Gas finally carries out antacid；CaSO is rich in wherein4Material is 2 with the mass ratio of melting salt system：5；Melting salt system is mass ratio
For 1:1 Na2CO3And K2CO3；Carbonaceous reducing agent is coal, and the addition of carbonaceous reducing agent is rich in CaSO4CaSO in material4With
In carbonaceous reducing agent, the mol ratio of carbon is 1.5：1；
（3）Step（2）The CaO for preparing gradually sinks to bottom, after the completion of reaction together imports CaO and fuse salt
CaO separators are obtained CaO and fuse salt, and fuse salt enters first fuse salt storage tank Jing after fuse salt cleaning system is processed,
Then entered in heater by fuse salt blood circulation and heated, finally enter to go to second fuse salt storage tank molten so as to stream enters
Melt salt reactor（In order to safety and be easy to control production procedure）.
The SO of above-mentioned generation2And CO2SO in gaseous mixture2Percent by volume is 10% ~ 25%, CO2Percentage ratio 5% ~ 13% is big absolutely
Part element sulphur has been reduced to SO2。
Embodiment 2
As shown in figure 1, should be rich in CaSO4The high-temperature fusion salt processing method of material, which comprises the following steps that：
（1）Process rich in CaSO4The high-temperature fusion salt treatment device of material includes molten salt reaction device, CaO separators, melts
Melt salt holding vessel and fuse salt storage heating system；CaSO is rich in wherein4Material is ardealite, its mass percent composition such as table
Shown in 2；
Table 2
（2）Melting salt system is heated to 1323K first to put in molten salt reaction device, from the top of molten salt reaction device
Add rich in CaSO4Material, is then passed through flow for 100Ncm from molten salt reaction device bottom3·min-1Nitrogen, carbonaceous is also
Former agent nitrogen buffer gas carry out reaction 2h into molten salt reaction device from bottom, prepare SO2And CO2Gaseous mixture and
CaO, the SO of generation2And CO2Gaseous mixture is flowed out from the top of molten salt reaction device, obtains rich SO after condensed device condensation, purification2Tail
Gas finally carries out antacid；CaSO is rich in wherein4Material is 1 with the mass ratio of melting salt system：20；Melting salt system is mass ratio
For 1:1:1 Na2CO3、K2CO3And Li2CO3；Carbonaceous reducing agent is coke, and the addition of carbonaceous reducing agent is rich in CaSO4Thing
CaSO in material4Mol ratio with carbon in carbonaceous reducing agent is 2.0：1；
（3）Step（2）The CaO for preparing gradually sinks to bottom, after the completion of reaction together imports CaO and fuse salt
CaO separators are obtained CaO and fuse salt, and fuse salt enters first fuse salt storage tank Jing after fuse salt cleaning system is processed,
Then entered in heater by fuse salt blood circulation and heated, finally enter to go to second fuse salt storage tank molten so as to stream enters
Melt salt reactor（It is easy to safety in production, is easy to control whole production procedure）.
The SO of above-mentioned generation2And CO2SO in gaseous mixture2Percent by volume is 9% ~ 23%.
Embodiment 3
As shown in figure 1, should be rich in CaSO4The high-temperature fusion salt processing method of material, which comprises the following steps that：
（1）Process rich in CaSO4The high-temperature fusion salt treatment device of material includes molten salt reaction device, CaO separators, melts
Melt salt holding vessel and fuse salt storage heating system；CaSO is rich in wherein4Material be Calx iron salt method waste water copper sludge, its quality
Percent composition is as shown in table 3；
Table 3
（2）Melting salt system is heated to 1323K first to put in molten salt reaction device, from the top of molten salt reaction device
Add rich in CaSO4Material, is then passed through flow for 100Ncm from molten salt reaction device bottom3·min-1Nitrogen, carbonaceous is also
Former agent nitrogen buffer gas carry out reaction 2h into molten salt reaction device from bottom, prepare SO2And CO2Gaseous mixture and
CaO, the SO of generation2And CO2Gaseous mixture is flowed out from the top of molten salt reaction device, obtains rich SO after condensed device condensation, purification2Tail
Gas finally carries out antacid；CaSO is rich in wherein4Material is 23 with the mass ratio of melting salt system：100；Melting salt system is quality
Than for 0.5:1.5 Na2CO3And Li2CO3；Carbonaceous reducing agent is natural gas, and the addition of carbonaceous reducing agent is rich in CaSO4Thing
CaSO in material4Mol ratio with carbon in carbonaceous reducing agent is 1.8：1；
（3）Step（2）The CaO for preparing gradually sinks to bottom, after the completion of reaction together imports CaO and fuse salt
CaO separators（Density contrast）Obtain CaO and fuse salt, fuse salt is Jing after fuse salt cleaning system is processed（Density contrast）Into
One fuse salt storage tank, is then entered in heater by fuse salt blood circulation and is heated, finally enter to go to second melting
Salt storage tank enters molten salt reaction device so as to stream（Consider for safety and to the control of production process）.
The SO of above-mentioned generation2And CO2SO in gaseous mixture2Percent by volume is 7% ~ 18%.
Embodiment 4
As shown in figure 1, should be rich in CaSO4The high-temperature fusion salt processing method of material, which comprises the following steps that：
（1）Process rich in CaSO4The high-temperature fusion salt treatment device of material includes molten salt reaction device, CaO separators, melts
Melt salt holding vessel and fuse salt storage heating system；CaSO is rich in wherein4Material be Calx iron salt method waste water copper sludge, its quality
Percent composition is as shown in table 3；
（2）Melting salt system is heated to 1423K first to put in molten salt reaction device, from the top of molten salt reaction device
Add rich in CaSO4Material, is then passed through flow for 800Ncm from molten salt reaction device bottom3·min-1Nitrogen, carbonaceous is also
Former agent nitrogen buffer gas carry out reaction 10h into molten salt reaction device from bottom, prepare SO2And CO2Gaseous mixture and
CaO, the SO of generation2And CO2Gaseous mixture is flowed out from the top of molten salt reaction device, obtains rich SO after condensed device condensation, purification2Tail
Gas finally carries out antacid；CaSO is rich in wherein4Material is 1 with the mass ratio of melting salt system：5；Melting salt system is mass ratio
For 1.5:0.5 Na2CO3And Li2CO3；Carbonaceous reducing agent is natural gas, and the addition of carbonaceous reducing agent is rich in CaSO4Material
Middle CaSO4Mol ratio with carbon in carbonaceous reducing agent is 1.7：1；
（3）Step（2）The CaO for preparing gradually sinks to bottom, after the completion of reaction together imports CaO and fuse salt
CaO separators（Density contrast）Obtain CaO and fuse salt, fuse salt is Jing after fuse salt cleaning system is processed（Density contrast）Into
One fuse salt storage tank, is then entered in heater by fuse salt blood circulation and is heated, finally enter to go to second melting
Salt storage tank enters molten salt reaction device so as to stream（Improve safety coefficient and be easy to flexibly control production procedure）.
The SO of above-mentioned generation2And CO2SO in gaseous mixture2Percent by volume is 10% ~ 60%.
Embodiment 5
As shown in figure 1, should be rich in CaSO4The high-temperature fusion salt processing method of material, which comprises the following steps that：
（1）Process rich in CaSO4The high-temperature fusion salt treatment device of material includes molten salt reaction device, CaO separators, melts
Melt salt holding vessel and fuse salt storage heating system；CaSO is rich in wherein4Material be Calx iron salt method waste water copper sludge, its quality
Percent composition is as shown in table 3；
（2）Melting salt system is heated to 1373K first to put in molten salt reaction device, from the top of molten salt reaction device
Add rich in CaSO4Material, is then passed through flow for 500Ncm from molten salt reaction device bottom3·min-1Nitrogen, carbonaceous is also
Former agent nitrogen buffer gas carry out reaction 10h into molten salt reaction device from bottom, prepare SO2And CO2Gaseous mixture and
CaO, the SO of generation2And CO2Gaseous mixture is flowed out from the top of molten salt reaction device, obtains rich SO after condensed device condensation, purification2Tail
Gas finally carries out antacid；CaSO is rich in wherein4Material is 1.5 with the mass ratio of melting salt system：5；Melting salt system is quality
Than for 1:2 Na2CO3And Li2CO3；Carbonaceous reducing agent is coal, and the addition of carbonaceous reducing agent is rich in CaSO4CaSO in material4
Mol ratio with carbon in carbonaceous reducing agent is 1.6：1；
（3）Step（2）The CaO for preparing gradually sinks to bottom, after the completion of reaction together imports CaO and fuse salt
CaO separators（Density contrast）Obtain CaO and fuse salt, fuse salt is Jing after fuse salt cleaning system is processed（Density contrast）Into
One fuse salt storage tank, is then entered in heater by fuse salt blood circulation and is heated, finally enter to go to second melting
Salt storage tank enters molten salt reaction device so as to stream（Safety and flexibly production）.
The SO of above-mentioned generation2And CO2SO in gaseous mixture2Percent by volume is 10% ~ 60%.
Embodiment 6
As shown in figure 1, should be rich in CaSO4The high-temperature fusion salt processing method of material, which comprises the following steps that：
（1）Process rich in CaSO4The high-temperature fusion salt treatment device of material includes molten salt reaction device, CaO separators, melts
Melt salt holding vessel and fuse salt storage heating system；CaSO is rich in wherein4Material is ardealite, its mass percent composition such as table
Shown in 2；
（2）Melting salt system is heated to 1373K first to put in molten salt reaction device, from the top of molten salt reaction device
Add rich in CaSO4Material, is then passed through flow for 700Ncm from molten salt reaction device bottom3·min-1Nitrogen, carbonaceous is also
Former agent nitrogen buffer gas carry out reaction 0.5h into molten salt reaction device from bottom, prepare SO2And CO2Gaseous mixture and
CaO, the SO of generation2And CO2Gaseous mixture is flowed out from the top of molten salt reaction device, obtains rich SO after condensed device condensation, purification2Tail
Gas finally carries out antacid；CaSO is rich in wherein4Material is 0.9 with the mass ratio of melting salt system：5；Melting salt system is quality
Than for 0.5:0.5:1.5 Na2CO3、K2CO3And Li2CO3；Carbonaceous reducing agent is coal, the addition of carbonaceous reducing agent be rich in
CaSO4CaSO in material4Mol ratio with carbon in carbonaceous reducing agent is 1.5：1；
（3）Step（2）The CaO for preparing gradually sinks to bottom, after the completion of reaction together imports CaO and fuse salt
CaO separators（Density contrast）Obtain CaO and fuse salt, fuse salt is Jing after fuse salt cleaning system is processed（Density contrast）Into
One fuse salt storage tank, is then entered in heater by fuse salt blood circulation and is heated, finally enter to go to second melting
Salt storage tank enters molten salt reaction device so as to stream（Flexibly, safety, relatively control flow）.
The SO of above-mentioned generation2And CO2SO in gaseous mixture2Percent by volume is 10% ~ 60%.
Embodiment 7
As shown in figure 1, should be rich in CaSO4The high-temperature fusion salt processing method of material, which comprises the following steps that：
（1）Process rich in CaSO4The high-temperature fusion salt treatment device of material includes molten salt reaction device, CaO separators, melts
Melt salt holding vessel and fuse salt storage heating system；CaSO is rich in wherein4Material is ardealite, its mass percent composition such as table
Shown in 2；
（2）Melting salt system is heated to 1373K first to put in molten salt reaction device, from the top of molten salt reaction device
Add rich in CaSO4Material, is then passed through flow for 600Ncm from molten salt reaction device bottom3·min-1Nitrogen, carbonaceous is also
Former agent nitrogen buffer gas carry out reaction 10h into molten salt reaction device from bottom, prepare SO2And CO2Gaseous mixture and
CaO, the SO of generation2And CO2Gaseous mixture is flowed out from the top of molten salt reaction device, obtains rich SO after condensed device condensation, purification2Tail
Gas finally carries out antacid；CaSO is rich in wherein4Material is 1.25 with the mass ratio of melting salt system：5；Melting salt system is quality
Than for 1.5:1.5:0.5 Na2CO3、K2CO3And Li2CO3；Carbonaceous reducing agent is coke, the addition of carbonaceous reducing agent be rich in
CaSO4CaSO in material4Mol ratio with carbon in carbonaceous reducing agent is 1.8：1；
（3）Step（2）The CaO for preparing gradually sinks to bottom, after the completion of reaction together imports CaO and fuse salt
CaO separators（Density contrast）Obtain CaO and fuse salt, fuse salt is Jing after fuse salt cleaning system is processed（Density contrast）Into
One fuse salt storage tank, is then entered in heater by fuse salt blood circulation and is heated, finally enter to go to second melting
Salt storage tank enters molten salt reaction device so as to stream（Safety, flexible, convenient and reliable operation）.
The SO of above-mentioned generation2And CO2SO in gaseous mixture2Percent by volume is 10% ~ 60%.
Above in association with accompanying drawing to the present invention specific embodiment be explained in detail, but the present invention be not limited to it is above-mentioned
Embodiment, in the ken that those of ordinary skill in the art possess, can be with before without departing from present inventive concept
Put that various changes can be made.
Claims (4)
1. it is a kind of to be rich in CaSO4The high-temperature fusion salt processing method of material, it is characterised in that comprise the following steps that：
（1）Process rich in CaSO4The high-temperature fusion salt treatment device of material includes molten salt reaction device, CaO separators, fuse salt
Holding vessel and fuse salt storage heating system；
Melting salt system is heated to 1323K ~ 1423K first to put in molten salt reaction device, from the top of molten salt reaction device
Add rich in CaSO4Material, is then passed through flow for 100 ~ 800Ncm from molten salt reaction device bottom3·min-1Nitrogen, carbon
Matter reducing agent nitrogen buffer gas carry out reaction 0.5-10h into molten salt reaction device from bottom, prepare SO2And CO2Mixing
Gas and CaO, the SO of generation2And CO2Gaseous mixture is flowed out from the top of molten salt reaction device, obtains richness after condensed device condensation, purification
SO2Tail gas finally carries out antacid；
（2）Step（1）The CaO for preparing gradually sinks to bottom, and CaO and fuse salt are together imported CaO after the completion of reaction
Separator obtains CaO and fuse salt, and fuse salt enters first fuse salt holding vessel Jing after fuse salt cleaning system is processed, then
Entered in heater by fuse salt blood circulation and heated, finally entered to go to second fuse salt holding vessel so as to stream and enter melting
Salt reactor.
2. according to claim 1 rich in CaSO4The high-temperature fusion salt processing method of material, it is characterised in that：The step
（1）In rich in CaSO4Material is copper sludge or ardealite.
3. according to claim 1 rich in CaSO4The high-temperature fusion salt processing method of material, it is characterised in that：The step
（1）Middle melting salt system is Na2CO3、K2CO3、Li2CO3In one kind, two or three of mixture, Na2CO3And Li2CO3Two
When planting mixture, mass ratio is 0.5:1.5、1.5:0.5 or 1:2, during three kinds of mixture, mass ratio is 0.5 ~ 1.5:0.5~1.5:
0.5~1.5。
4. according to claim 1 rich in CaSO4The high-temperature fusion salt processing method of material, it is characterised in that：The step
（1）Middle carbonaceous reducing agent is coal, coke or natural gas, and the addition of carbonaceous reducing agent is rich in CaSO4CaSO in material4With carbon
In matter reducing agent, the mol ratio of carbon is 1.5 ~ 2.0：1.
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