CN105883720A - Method for preparing chlorides by using sulfuric acid cinder - Google Patents
Method for preparing chlorides by using sulfuric acid cinder Download PDFInfo
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- CN105883720A CN105883720A CN201410538191.7A CN201410538191A CN105883720A CN 105883720 A CN105883720 A CN 105883720A CN 201410538191 A CN201410538191 A CN 201410538191A CN 105883720 A CN105883720 A CN 105883720A
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- chloride
- cinder
- sulfuric acid
- chlorides
- magnesium
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Abstract
The invention relates to a method for preparing chlorides by using sulfuric acid cinder, belonging to the treatment and comprehensive utilization of waste cinder in the sulfuric acid industry of the inorganic chemical industry. Chlorides are prepared from sulfuric acid cinder through an acid treatment and recovery process and an extraction and purification process. The acid treatment and recovery process comprises the following steps of: making aluminum chloride in sulfuric acid cinder and hydrochloric acid to react to produce chlorides such as aluminum chloride, ferric chloride, calcium chloride, magnesium chloride and the like in a first corrosion-resisting reactor; and filtering the chlorides to obtain black filter cake silicides and elementary sulfur, and further processing the black filter cake silicides and the elementary sulfur. The extraction and purification process comprises the following steps of: introducing the clarified chlorides obtained in the acid treatment recovery process into a corrosion-resisting reduced-pressure distiller for reduced-pressure distillation, discharging the distillation liquid when the distillation liquid reaches a saturated solution, and introducing the distillation liquid into a cooler for stage cooling. Ferric chloride, aluminum chloride, magnesium chloride and calcium chloride crystals are cooled in sequence according to different freezing points. Four chloride crystal products are obtained through washing, drying, packaging and weight checking. The economic benefit of sulfuric acid cinder treatment is increased.
Description
Technical field
The present invention relates to inorganic chemical industry sulfuric acid industry and discard the technical field that slag is administered and utilized, particularly relate to one and utilize sulphur
Acid slag produces muriatic method.
Background technology
Sulfuric acid industry is the sulfuric acid produced for raw material contact method with troilite, mainly by raw material roasting, purify, convert and absorption etc.
Several operations form.To purify technological process in general custom, gas washing in SA production is divided into the big class of dry and wet two.Wet cleaning
Have again that pickling, hot concentrated acid wash and wash point.Pyrite-based sulfuric acid production minority factory of China is pickling process at present, and majority is still for washing
Flow process.
Troilite is mainly made up of sulphur and iron, with a small amount of non-ferrous metal and rare metal.Pyrite cinder is pyrite burning
The residue discharged after extracting sulphur.In troilite in addition to sulphur is utilized, iron and other elements remain in slag.Slag is used to
Ironmaking, extracts non-ferrous metal and manufactures the raw material of construction material.
The slag discharge capacity of unit sulfuric acid product is relevant with the grade of troilite and process conditions.Sulphur iron under identical process conditions
The highest then bed drain purge of grade in ore deposit is the fewest, otherwise the highest.When troilite sulfur content is 25~35%, general production is per ton about
Produce the clinker of 0.7~1 ton.Wherein various compositions and the percentage composition of pyrite cinder is: ferroso-ferric oxide content is 43.31
%, alundum (Al2O3) content is 8.13%, and calcium oxide content is 1.63%, and content of magnesia is 0.46%, silica content
Being 35.73%, the content of sulphur is 0.16%.
At present, the comprehensive utilization of pyrite cinder is unsatisfactory, and in addition to small part is used as ironmaking and construction material, major part uses
Landfill processes, and causes the waste of resource and the pollution of environment.
Utilization to pyrite cinder should improve constantly the value of output object, product that some markets of output are in short supply, that added value is big,
To improve the economic benefit that pyrite cinder utilizes.
Summary of the invention
It is contemplated that for the utilization of pyrite cinder and the market demand, it is provided that one utilizes pyrite cinder to produce muriatic method.
To achieve these goals, a kind of technical scheme utilizing pyrite cinder to produce muriatic method of the present invention is as follows:
One utilizes pyrite cinder to produce muriatic method, and pyrite cinder reclaims by acid treatment and deduct a percentage purifying process, prepared
Chloride;
Described acid treatment recovery process is: pyrite cinder (in terms of aluminium chloride) and hydrochloric acid are thrown with pure mass ratio 1: 1.83~2.48
Enter in corrosion-resistant reactor, open agitator simultaneously and slowly stir and make material carry out chemical reaction;After 24 minutes, reaction generates chlorination
The chlorides such as aluminium, iron chloride, calcium chloride, magnesium chloride.It is filtrated to get black filter cake silicide and elemental sulfur sends to other deep processing,
The chloride liquid simultaneously obtaining clarification carries out next step extraction;
Described purifying technique is: the clarification chloride that described acid treatment recovery process obtains is sent into and carried out in corrosion-resistant decompression distiller
Decompression distillation, ejects entrance cooler and carries out classification cooling when distillating liquid has reached saturated solution.Solidification according to them
Point difference will cool down out iron chloride, aluminium chloride, magnesium chloride, calcium chloride crystals successively.The most scrubbed drying, packaging are checked the weight and are obtained
Iron chloride, aluminium chloride, magnesium chloride and four kinds of chloride crystals products of calcium chloride;
Clarification chloride is sent into and in corrosion-resistant decompression distiller, carries out decompression distillation, arrange when distillating liquid has reached saturated solution
Out enter cooler and carry out classification cooling.Freezing point difference according to them will cool down out iron chloride, aluminium chloride, chlorination successively
Magnesium, calcium chloride crystals.The most scrubbed drying, packaging are checked the weight and are obtained iron chloride, aluminium chloride, magnesium chloride and four kinds of chlorinations of calcium chloride
Thing crystal product;Finally distilling remaining liquid is that hydrochloric acid solution returns the utilization of upper track process cycles.
Pyrite cinder used by the present invention is to produce the pyrite cinder that troilite is the production of raw material contact method, described pyrite cinder, its
Containing iron chloride, aluminium chloride, magnesium chloride and calcium chloride in component.
The main chemical reactions equation of the present invention is:
Al2O3+ 6HCl=2AlCl3+3H2O
The beneficial effects of the present invention is: one, it is provided that one utilizes pyrite cinder to produce muriatic method, for effectively place
Reason pyrite cinder opens up an approach.Its two, preparation includes that iron chloride, aluminium chloride, magnesium chloride, calcium chloride are all economic valencys
It is worth bigger best-selling product, improves the economic benefit processing pyrite cinder.Its three, small investment, to process for producing troilite be
Pyrite cinder and the pyrite cinder of similar components that raw material contact method produces are especially suitable, it may be said that open a Tiao Xin road.Its four,
The purity of preparation is high, and quality is guaranteed.
Detailed description of the invention
Embodiment one
A kind of chemical method prepares the method that pyrite cinder is nitrate, and pyrite cinder is reclaimed by acid treatment and deduct a percentage purifying process,
Prepare chloride;
Described acid treatment recovery process is: take pyrite cinder 500 kilograms (wherein containing alundum (Al2O3) content is 8.13%) by sulfuric acid
Aluminium chloride in slag puts in the first corrosion-resistant reactor with pure mass ratio 1: 2.15 with hydrochloric acid, opens agitator slowly simultaneously
Stirring makes material carry out chemical reaction;After 24 minutes, reaction generates 106.8 kilograms of aluminium chloride and iron chloride, calcium chloride, magnesium chloride
Deng chloride;It is filtrated to get black filter cake silicide and elemental sulfur sends to other deep processing, obtain the chloride liquid of clarification simultaneously
Carry out next step to extract;
Described deduction purifying process is: the clarification chloride that described acid treatment recovery process obtains is sent in corrosion-resistant decompression distiller
Carry out decompression distillation, eject entrance cooler when distillating liquid has reached saturated solution and carry out classification cooling.According to theirs
Freezing point difference will cool down out iron chloride, aluminium chloride, magnesium chloride, calcium chloride crystals successively.The most scrubbed drying, packaging are checked the weight
Obtain iron chloride, aluminium chloride, magnesium chloride and four kinds of chloride crystals products of calcium chloride;
Clarification chloride is sent into and in corrosion-resistant decompression distiller, carries out decompression distillation, the row when distillating liquid has reached saturated molten rolling
Out enter cooler and carry out classification cooling.Freezing point difference according to them will cool down out iron chloride, aluminium chloride, chlorination successively
Magnesium, calcium chloride crystals.The most scrubbed drying, packaging are checked the weight and are obtained iron chloride, aluminium chloride, magnesium chloride and four kinds of chlorinations of calcium chloride
Thing crystal product;Finally distilling remaining liquid is that hydrochloric acid solution returns the utilization of upper track process cycles.
Pyrite cinder used by the present invention is to produce the pyrite cinder that troilite is the production of raw material contact method, and its component is such that
Ferroso-ferric oxide content is 43.31%, and alundum (Al2O3) content is 8.13%, and calcium oxide content is 1.63%, content of magnesia
Being 0.46%, silica content is 35.73%, and the content of sulphur is 0.16%.
Embodiment two
One utilizes pyrite cinder to produce muriatic method, and pyrite cinder reclaims by acid treatment and deduct a percentage purifying process, prepared
Chloride;
Described acid treatment recovery process is: take pyrite cinder 500 kilograms (wherein containing alundum (Al2O3) content is 8.13%) by sulfuric acid
Aluminium chloride in slag puts in the first corrosion-resistant reactor with pure mass ratio 1: 2.35 with hydrochloric acid, opens agitator slowly simultaneously
Stirring makes material carry out chemical reaction;After 24 minutes, reaction generates 116.7 kilograms of aluminium chloride and iron chloride, calcium chloride, magnesium chloride
Deng chloride;It is filtrated to get black filter cake silicide and elemental sulfur sends to other deep processing, obtain the chloride liquid of clarification simultaneously
Carry out next step to extract;
Described deduction purifying process is: the clarification chloride that described acid treatment recovery process obtains is sent in corrosion-resistant decompression distiller
Carry out decompression distillation, eject entrance cooler when distillating liquid has reached saturated solution and carry out classification cooling.According to theirs
Freezing point difference will cool down out iron chloride, aluminium chloride, magnesium chloride, calcium chloride crystals successively.The most scrubbed drying, packaging are checked the weight
Obtain iron chloride, aluminium chloride, magnesium chloride and four kinds of chloride crystals products of calcium chloride;
Clarification chloride is sent into and in corrosion-resistant decompression distiller, carries out decompression distillation, arrange when distillating liquid has reached saturated solution
Out enter cooler and carry out classification cooling.Freezing point difference according to them will cool down out iron chloride, aluminium chloride, chlorination successively
Magnesium, calcium chloride crystals.The most scrubbed drying, packaging are checked the weight and are obtained iron chloride, aluminium chloride, magnesium chloride and four kinds of chlorinations of calcium chloride
Thing crystal product;Finally distilling remaining liquid is that hydrochloric acid solution returns the utilization of upper track process cycles.
Pyrite cinder used by the present invention is to produce the pyrite cinder that troilite is the production of raw material contact method, and its component is such that
Ferroso-ferric oxide content is 43.31%, and alundum (Al2O3) content is 8.13%, and calcium oxide content is 1.63%, content of magnesia
Being 0.46%, silica content is 35.73%, and the content of sulphur is 0.16%.
Embodiment three
A kind of chemical method prepares the method that pyrite cinder is nitrate, and pyrite cinder is reclaimed by acid treatment and synthesizing and purifying technique,
Prepare nitrate;
Described acid treatment recovery process is: take pyrite cinder 500 kilograms (wherein containing alundum (Al2O3) content is 8.13%) by sulfuric acid
Aluminium chloride in slag puts in the first corrosion-resistant reactor with pure mass ratio 1: 1.95 with hydrochloric acid, opens agitator slowly simultaneously
Stirring makes material carry out chemical reaction;After 24 minutes, reaction generates 96.9 kilograms of aluminium chloride and iron chloride, calcium chloride, magnesium chloride
Deng chloride;It is filtrated to get black filter cake silicide and elemental sulfur sends to other deep processing, obtain the chloride liquid of clarification simultaneously
Carry out next step to extract;
Described deduction purifying process is: the clarification chloride that described acid treatment recovery process obtains is sent in corrosion-resistant decompression distiller
Carry out decompression distillation, eject entrance cooler when distillating liquid has reached saturated solution and carry out classification cooling.According to theirs
Freezing point difference will cool down out iron chloride, aluminium chloride, magnesium chloride, calcium chloride crystals successively.The most scrubbed drying, packaging are checked the weight
Obtain iron chloride, aluminium chloride, magnesium chloride and four kinds of chloride crystals products of calcium chloride;
Clarification chloride is sent into and in corrosion-resistant decompression distiller, carries out decompression distillation, arrange when distillating liquid has reached saturated solution
Out enter cooler and carry out classification cooling.Freezing point difference according to them will cool down out iron chloride, aluminium chloride, chlorination successively
Magnesium, calcium chloride crystals.The most scrubbed drying, packaging are checked the weight and are obtained iron chloride, aluminium chloride, magnesium chloride and four kinds of chlorinations of calcium chloride
Thing crystal product;Finally distilling remaining liquid is that hydrochloric acid solution returns the utilization of upper track process cycles.
Pyrite cinder used by the present invention is to produce the pyrite cinder that troilite is the production of raw material contact method, and its component is such that
Ferroso-ferric oxide content is 43.31%, and alundum (Al2O3) content is 8.13%, and calcium oxide content is 1.63%, content of magnesia
Being 0.46%, silica content is 35.73%, and the content of sulphur is 0.16%.
Claims (2)
1. one kind utilizes pyrite cinder to produce muriatic method, it is characterised in that: pyrite cinder is reclaimed by acid treatment and deducts a percentage
Purifying process, prepares chloride;Described acid treatment recovery process is: by pyrite cinder and hydrochloric acid with pure mass ratio 1: 1.83~
2.48 put in corrosion-resistant reactors, open agitator simultaneously and slowly stir and make material carry out chemical reaction;After 24 minutes, reaction is raw
Become the chlorides such as aluminium chloride, iron chloride, calcium chloride, magnesium chloride;It is filtrated to get black filter cake silicide and elemental sulfur is sent to additionally
Deep processing, the chloride liquid simultaneously obtaining clarification carries out next step extraction;Described purifying technique is: work is reclaimed in described acid treatment
The clarification chloride that skill obtains is sent into and is carried out decompression distillation in corrosion-resistant decompression distiller, when distillating liquid has reached saturated solution
Eject entrance cooler and carry out classification cooling;Freezing point difference according to them will cool down out iron chloride, aluminium chloride, chlorine successively
Change magnesium, calcium chloride crystals;The most scrubbed drying, packaging are checked the weight and are obtained iron chloride, aluminium chloride, magnesium chloride and four kinds of chlorine of calcium chloride
Compound crystal product;Clarification chloride is sent into and in corrosion-resistant decompression distiller, carries out decompression distillation, when distillating liquid has reached full
Eject entrance cooler during with solution and carry out classification cooling;Freezing point difference according to them will cool down out iron chloride, chlorine successively
Change aluminium, magnesium chloride, calcium chloride crystals;The most scrubbed drying, packaging are checked the weight and are obtained iron chloride, aluminium chloride, magnesium chloride and chlorination
Four kinds of chloride crystals products of calcium;Finally distilling remaining liquid is that hydrochloric acid solution returns the utilization of upper track process cycles.
One the most according to claim 1 utilizes pyrite cinder to produce muriatic method, it is characterised in that: described sulfuric acid
Slag, containing iron chloride, aluminium chloride, magnesium chloride and calcium chloride in its component.
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CN201410538191.7A CN105883720A (en) | 2014-09-24 | 2014-09-24 | Method for preparing chlorides by using sulfuric acid cinder |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110127772A (en) * | 2019-06-06 | 2019-08-16 | 河南省岩石矿物测试中心 | Method for preparing high-purity ammonium ferric chloride from sulfuric acid cinder |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110127772A (en) * | 2019-06-06 | 2019-08-16 | 河南省岩石矿物测试中心 | Method for preparing high-purity ammonium ferric chloride from sulfuric acid cinder |
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Application publication date: 20160824 |