CN109970081A - A method of sodium pyrosulfite is prepared using coking sulphur cream - Google Patents
A method of sodium pyrosulfite is prepared using coking sulphur cream Download PDFInfo
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- CN109970081A CN109970081A CN201910225270.5A CN201910225270A CN109970081A CN 109970081 A CN109970081 A CN 109970081A CN 201910225270 A CN201910225270 A CN 201910225270A CN 109970081 A CN109970081 A CN 109970081A
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- Prior art keywords
- sodium pyrosulfite
- stage reactor
- level
- sulfur dioxide
- sulphur cream
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/14—Preparation of sulfites
- C01D5/145—Pyrosulfites or metabisulfites
-
- 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 methods for preparing sodium pyrosulfite using coking sulphur cream, belong to technical field of environmental protection in chemical industry.Sulfur dioxide gas and sodium carbonate liquor use counter current contacting mode, and gas is successively passed through the first order, the second level and third stage reactor, and sodium carbonate liquor is successively passed through the third level, the second level and the first stage reactor.Sulfur dioxide is in excessive state in first stage reactor, sodium pyrosulfite quality is improved significantly in first stage reactor, sodium carbonate is in excessive state in third stage reactor, absorb sulfur dioxide all in third stage reactor, there is no sulfur dioxide in the tail gas come out in third stage reactor, maximize absorption rate of sulfur dioxide, i.e., sodium pyrosulfite product yield reaches maximization.The present invention solves the problems, such as that the processing of coking sulphur cream is difficult, and obtained sodium pyrosulfite product purity >=96.5% meets national standard, directly outer can sell, solve environmental issue, increase the performance of enterprises.
Description
Technical field
The invention belongs to technical field of environmental protection in chemical industry, prepare burnt sulfurous using coking sulphur cream more specifically to a kind of
The method of sour sodium.
Background technique
Hydrogen sulfide in coke-stove gas is handled using HPF wet oxidation process, which is the wet type liquid using ammonia as alkali source
Phase catalytic oxidation desulfurization decyanation technology.H in coke-stove gas is absorbed in desulfurizing tower2The doctor solution solution circulation pump of S and HCN
Be delivered to regenerator, the regeneration of the compressed air oxidation sent in regenerator with air compression station, then desulfurization lean solution from regenerator into
Enter desulfurizing tower top spray coal gas desulfurization, is so recycled.The sulphur foam generated in regenerator at the top of regenerator then by expanding
Part is pumped into filter press filtering from inflow sulphur foam tank, then by sulphur foam, and the solid being obtained by filtration is coking sulphur cream, filtrate
Send desulfurizing tower recycling back to.
Main component in obtained coking sulphur cream is sulphur, but because product purity is low, can not sell, need to pay out of one's own pocket and send outside
Processing, had both caused the significant wastage of resource, while also adding processing cost.Part coke-oven plant is that processing coking sulphur cream has system
Sour project, but, equipment seriously corroded big because investing, technique is immature to cause the relieving haperacidity operation stop production to overhaul period long, maintenance maintenance
At high cost, the concentrated sulfuric acid price produced is lower, often in loss operating status.
It is a kind of using sulphur foam or containing that publication date is that the Chinese patent 201420043714.6 on October 1st, 2014 discloses
The device of sulphur impurity production sodium pyrosulfite comprising sequentially connected concentrate drying system, oxidation burners, dust separation system
System, sulfur dioxide absorption system and sodium pyrosulfite concentration systems, and the washing tail gas being connect with sulfur dioxide absorption system
System.The technology the problem is that its be not particularly suited for using coking sulphur cream as raw material sodium pyrosulfite prepare, it is obtained
The purity of sodium pyrosulfite is not also high.In the patent then level-one, second level, third-stage reactor can produce product sodium pyrosulfite
It send to the processing of concentrate drying system.The unstable product quality that level-one, second level, third-stage reactor obtain is produced in this way, is easy to lead
Cause product unqualified.
Summary of the invention
Goal of the invention: aiming at the above shortcomings existing in the prior art, the purpose of the present invention is to provide a kind of using burnt
Change the method that sulphur cream prepares sodium pyrosulfite.Sodium pyrosulfite product purity obtained by the present invention is high, meets national standard, can
It is directly outer to sell, turn waste into wealth, economize on resources, increases economic well-being of workers and staff, have a good application prospect.
Technical solution: to solve the above-mentioned problems, the technical solution adopted in the present invention is as follows:
A method of sodium pyrosulfite, sulfur dioxide gas and sodium carbonate liquor are prepared using adverse current using coking sulphur cream
Way of contact production, sulfur dioxide gas are successively passed through the first order, the second level and third stage reactor, sodium carbonate liquor and successively lead to
Enter from the third level, the second level and the first stage reactor.This production model, sulfur dioxide is in excessive shape in the first stage reactor
State can make sodium pyrosulfite product yield and product quality in first order reactor be improved significantly, third order reaction
Sodium carbonate is in excessive state in device, so that sulfur dioxide gas is all absorbed substantially in third stage reactor, the third level
There is no sulfur dioxide ingredient substantially in the tail gas come out in reactor, maximizes absorption rate of sulfur dioxide, that is, represent coke
Sodium sulfite product yield is maximized.Calculate through us, same scale set produces product yield using present invention process
It can be improved 20~30%, product qualification rate >=99.5%.Specifically includes the following steps:
(1) it sizes mixing, the mother liquor deviate from from centrifuge, water and sodium carbonate is tuned into sodium carbonate liquor；
(2) it burns, coking sulphur cream is uniformly mixed with air, is then burnt；The high-temperature gas drop that burning is generated
Temperature, then wash removal sublimed sulfur and other impurity through water scrubber, then separates the drop that gas is carried secretly by demister, obtain to
The sulfur dioxide gas of reaction；
(3) it reacts, sodium carbonate liquor successively passes through the third level, the second level and the first stage reactor；Sulfur dioxide gas is then
It is successively to be passed through the first order, the second level and third stage reactor, then sulfur dioxide gas is discharged into tail gas washing tower；Spray
Outlet after washing recycling；
(4) it is centrifuged, step (3) reaction solution is sent into decrease temperature crystalline in crystallization kettle after reaction, is then fed into centrifuge
Middle centrifugation, the solid being centrifuged are product sodium pyrosulfite, and the mother liquor for being centrifuged abjection, which is sent back in pulping device, to be recycled；
(5) it dries, the sodium pyrosulfite that centrifugation obtains is delivered in pneumatic drier and is dried with hot dry air, dry
After dry, product separation is packaged.
Preferably, the step (1), the mass concentration of sodium carbonate liquor are 45%~48%.
Preferably, the mixing quality ratio of the step (2), coking sulphur cream and air is 1: 70~1: 100.
Preferably, the step (2), high-temperature gas by cooler cool down, the cooler be successively be arranged it is air-cooled
Device and water cooler.
Preferably, the step (2), the temperature of gas is 50~60 DEG C after cooler cools down.
Preferably, the step (2), coking sulphur cream are first crushed before mixing with air.
Preferably, the step (5), drying mode is pneumatic conveying drying.
Preferably, the step (5), the separate mode are cyclonic separation.
The utility model has the advantages that compared with the prior art, the device have the advantages that are as follows:
(1) present invention solves the problems, such as that the processing of coking sulphur cream is difficult, turns waste into wealth, economizes on resources, obtained pyrosulfurous acid
Sodium product purity meets national standard 96.5% or more, directly outer can sell, increase enterprise while solving environmental issue
Benefit has a good application prospect.
(2) sulfur dioxide and sodium carbonate liquor of the present invention are produced using counter current contacting mode, sulfur dioxide from the first order to
Third stage reactor is arrived in the second level again, and sodium carbonate liquor is from the third level to the second level again to the first stage reactor.This producer
Formula may insure that product design meets centrifuging process requirement, and quality of production stability is high, and product yield can be improved 20~30%, produce
Product qualification rate >=99.5%, greatly improves economic benefit.
Detailed description of the invention
Fig. 1 is the preparation process flow schematic diagram of the invention that sodium pyrosulfite is prepared using coking sulphur cream.
Specific embodiment
The present invention is further described below combined with specific embodiments below.
Embodiment 1
A method of sodium pyrosulfite, sulfur dioxide gas and sodium carbonate liquor are prepared using adverse current using coking sulphur cream
Way of contact production, sulfur dioxide gas is again to third stage reactor from the first order to the second level, and sodium carbonate liquor is from the third level
To the second level again to the first stage reactor.As shown in Figure 1, comprising the following steps:
(1) it sizes mixing, is tuned into being added in pulping device from the mother liquor, water and sodium carbonate deviate from centrifuge with suitable ratio
The sodium carbonate liquor that mass concentration is 45%.
(2) burn, by coking sulphur cream crush after by into sulphur machine with from air compressor air according to 1: 70
Mass ratio uniformly mixes, and is then fed into sulfur furnace and burns, and the high-temperature gas for generation of burning successively is dropped through air cooler, water cooler
Temperature washs removal sublimed sulfur and other impurity to 50 DEG C, then through water scrubber, and the drop of gas entrainment is then separated by demister,
It obtains to reaction gas.
(3) it reacts, reaction system is by thtee-stage shiplock reactor group at each other in step arrangement.Alkali slurry initially enters most
High-rise third stage reactor, then interval flows into second level reactor, enters back into the first stage reactor.Sulfur dioxide gas is then
It is continuously to be passed through the first stage reactor, enters back into the second stage reactor, is most discharged into tail after third level reactor fully absorbs afterwards
Standard discharge after spray washing recycling in gas wash tower.
In the prior art the first order, the second level and third stage reactor can produce product sodium pyrosulfite be then sent to it is dense
The processing of contracting drying system.Production will lead to the unstable product quality that the first order, the second level and third stage reactor obtain in this way,
It being easy so that product is unqualified, production technology of the present invention is material from the third level to the second level, then again to the first stage reactor,
Then it send again into centrifuge, ensures that product design meets centrifuging process requirement in this way, quality of production stability is high, can be closed
The stable sodium pyrosulfite product of lattice.
(4) it is centrifuged, when reaction reaches terminal, reaction solution is sent into decrease temperature crystalline in crystallization kettle, is then fed into centrifuge
Middle centrifugation, the solid being centrifuged are product sodium pyrosulfite, and the mother liquor for being centrifuged abjection, which is sent back in pulping device, to be recycled.
(5) it dries, the sodium pyrosulfite that centrifugation obtains is delivered in pneumatic drier and is dried with hot dry air, dry
Product is sent into packing machine after cyclonic separation after dry is packaged.
The sodium pyrosulfite product being prepared by the above method, purity >=96.5% of product, meets after testing
National standard is paid out of one's own pocket processing without further progress, directly outer can be sold, greatly saved cost, turned waste into wealth, saved money
Source increases economic well-being of workers and staff, has a good application prospect.
Embodiment 2
A method of using each sodium pyrosulfite of coking sulphur cream system, sulfur dioxide gas and sodium carbonate liquor are using adverse current
Way of contact production, sulfur dioxide gas is again to third stage reactor from the first order to the second level, and sodium carbonate liquor is from the third level
To the second level again to the first stage reactor.As shown in Figure 1, comprising the following steps:
(1) it sizes mixing, is tuned into being added in pulping device from the mother liquor, water and sodium carbonate deviate from centrifuge with suitable ratio
The sodium carbonate liquor that mass concentration is 48%.
(2) burn, by coking sulphur cream crush after by into sulphur machine with from air compressor air according to 1: 70~1
: 100 mass ratio uniformly mixes, and is then fed into sulfur furnace and burns, and the high-temperature gas for generation of burning is successively through air cooler, water
Cooler is cooled to 60 DEG C, then washs removal sublimed sulfur and other impurity through water scrubber, then separates gas entrainment by demister
Drop, obtain to reaction gas.
(3) it reacts, reaction system is by thtee-stage shiplock reactor group at each other in step arrangement.Alkali slurry initially enters most
High-rise third stage reactor, then interval flows into second level reactor, enters back into the first stage reactor.Sulfur dioxide gas is then
It is continuously to be passed through the first stage reactor, enters back into the second stage reactor, is most discharged into tail after third level reactor fully absorbs afterwards
Standard discharge after spray washing recycling in gas wash tower.
In the prior art the first order, the second level and third stage reactor can produce product sodium pyrosulfite be then sent to it is dense
The processing of contracting drying system.Production will lead to the unstable product quality that the first order, the second level and third stage reactor obtain in this way,
It being easy so that product is unqualified, production technology of the present invention is material from the third level to the second level, then again to the first stage reactor,
Then it send again into centrifuge, ensures that product design meets centrifuging process requirement in this way, quality of production stability is high, can be closed
The stable sodium pyrosulfite product of lattice.
(4) it is centrifuged, when reaction reaches terminal, reaction solution is sent into decrease temperature crystalline in crystallization kettle, is then fed into centrifuge
Middle centrifugation, the solid being centrifuged are product sodium pyrosulfite, and the mother liquor for being centrifuged abjection, which is sent back in pulping device, to be recycled.
(5) it dries, the sodium pyrosulfite that centrifugation obtains is delivered in pneumatic drier and is dried with hot dry air, dry
Product is sent into packing machine after cyclonic separation after dry is packaged.
The sodium pyrosulfite product being prepared by the above method, purity >=96.5% of product, meets after testing
National standard is paid out of one's own pocket processing without further progress, directly outer can be sold, greatly saved cost, turned waste into wealth, saved money
Source increases economic well-being of workers and staff, has a good application prospect.
Sulfur dioxide gas is produced with sodium carbonate liquor using counter current contacting mode, and sulfur dioxide is from the first order to the second level
Third stage reactor is arrived again, and sodium carbonate liquor is from the third level to the second level again to the first stage reactor.This production model, first
Sulfur dioxide is in excessive state in stage reactor, can make sodium pyrosulfite product yield and product matter in first order reactor
Amount is improved significantly, and sodium carbonate is in excessive state in third stage reactor, so that sulfur dioxide gas is anti-in the third level
It answers in device and is all absorbed substantially, there is no sulfur dioxide ingredient substantially in the tail gas come out in third stage reactor, make titanium dioxide
Sulfur absorption rate is maximized, that is, is represented sodium pyrosulfite product yield and maximized.Calculate through us, same scale set
It can be improved 20~30% using present invention process production product yield, product qualification rate >=99.5%.
Claims (9)
1. a kind of method for preparing sodium pyrosulfite using coking sulphur cream, which is characterized in that sulfur dioxide gas and sodium carbonate are molten
Liquid is produced using counter current contacting mode, and sulfur dioxide gas is successively passed through the first order, the second level and third stage reactor, sodium carbonate
Solution is successively passed through from the third level, the second level and the first stage reactor.
2. the method according to claim 1 for preparing sodium pyrosulfite using coking sulphur cream, which is characterized in that specifically include
Following steps:
(1) it sizes mixing, the mother liquor deviate from from centrifuge, water and sodium carbonate is tuned into sodium carbonate liquor；
(2) it burns, coking sulphur cream is uniformly mixed with air, is then burnt；To the high-temperature gas cooling that burning generates, then
Removal sublimed sulfur and other impurity are washed through water scrubber, the drop of gas entrainment is then separated by demister, is obtained wait react
Sulfur dioxide gas；
(3) it reacts, sodium carbonate liquor successively passes through the third level, the second level and the first stage reactor；Sulfur dioxide gas be then according to
It is secondary to be passed through the first order, the second level and third stage reactor, then sulfur dioxide gas is discharged into tail gas washing tower；Spray washing
Outlet after recycling；
(4) be centrifuged, after reaction by step (3) reaction solution be sent into crystallization kettle in decrease temperature crystalline, be then fed into centrifuge from
The heart, the solid being centrifuged are product sodium pyrosulfite, and the mother liquor for being centrifuged abjection, which is sent back in pulping device, to be recycled；
(5) it dries, the sodium pyrosulfite that centrifugation obtains is delivered in pneumatic drier and is dried with hot dry air, dry
Afterwards, product separation is packaged.
3. the method according to claim 2 for preparing sodium pyrosulfite using coking sulphur cream, which is characterized in that the step
(1), the mass concentration of sodium carbonate liquor is 45%~48%.
4. the method according to claim 2 for preparing sodium pyrosulfite using coking sulphur cream, which is characterized in that the step
(2), the mixing quality ratio of coking sulphur cream and air is 1: 70~1: 100.
5. the method according to claim 2 for preparing sodium pyrosulfite using coking sulphur cream, which is characterized in that the step
(2), high-temperature gas is cooled down by cooler, and the cooler is the air cooler and water cooler being successively arranged.
6. the method according to claim 2 for preparing sodium pyrosulfite using coking sulphur cream, which is characterized in that the step
(2), the temperature of gas is 50~60 DEG C after cooler cools down.
7. the method according to claim 2 for preparing sodium pyrosulfite using coking sulphur cream, which is characterized in that the step
(2), coking sulphur cream is first crushed before mixing with air.
8. the method according to claim 2 for preparing sodium pyrosulfite using coking sulphur cream, which is characterized in that the step
(5), drying mode is pneumatic conveying drying.
9. the method according to claim 2 for preparing sodium pyrosulfite using coking sulphur cream, which is characterized in that the step
(5), the separate mode is cyclonic separation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111153418A (en) * | 2020-01-21 | 2020-05-15 | 北京中航泰达环保科技股份有限公司 | System and method for resource preparation of multi-salt by using regenerated gas of active coke |
| CN112250089A (en) * | 2020-10-29 | 2021-01-22 | 新晃鲁湘钡业有限公司 | Method for producing sodium metabisulfite by utilizing sulfur-containing tail gas |
| CN112408433A (en) * | 2020-11-11 | 2021-02-26 | 宣城市楷昂化工有限公司 | Production method of sodium metabisulfite with low nitrogen oxide emission |
| WO2021114851A1 (en) * | 2019-12-13 | 2021-06-17 | 江苏德义通环保科技有限公司 | System for producing sodium pyrosulfite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2021114851A1 (en) * | 2019-12-13 | 2021-06-17 | 江苏德义通环保科技有限公司 | System for producing sodium pyrosulfite |
| CN111153418A (en) * | 2020-01-21 | 2020-05-15 | 北京中航泰达环保科技股份有限公司 | System and method for resource preparation of multi-salt by using regenerated gas of active coke |
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| CN112408433B (en) * | 2020-11-11 | 2022-11-18 | 宣城市楷昂化工有限公司 | Production method of sodium metabisulfite with low nitrogen oxide emission |
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