CN102534230A - Method for extracting strontium carbonate from metal strontium residues - Google Patents
Method for extracting strontium carbonate from metal strontium residues Download PDFInfo
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- CN102534230A CN102534230A CN2011104569319A CN201110456931A CN102534230A CN 102534230 A CN102534230 A CN 102534230A CN 2011104569319 A CN2011104569319 A CN 2011104569319A CN 201110456931 A CN201110456931 A CN 201110456931A CN 102534230 A CN102534230 A CN 102534230A
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- strontium
- residue
- salt
- carbonate powder
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a method for extracting strontium carbonate from metal strontium residues. The method comprises the following processes: (1) crushing the metal strontium residues into small particle materials; (2) adding the materials to water or an acidulous salt solution to hydrolyze; (3) adding alkalescent salt into hydrolysis liquid for a transformation reaction, and adjusting pH value to 7-10; (4) after transformation, clarifying for 2-3h, and separating strontium from aluminum; (5) adding ammonium bicarbonate or ammonium carbonate into a strontium salt solution for a carbonation reaction; and (6) washing, filtering and drying a precipitate to obtain a strontium carbonate product; and acidifying a mother liquor and rinsing water and then returning to a hydrolysis step for recycling. The method for extracting the strontium carbonate from the metal strontium residues has the advantages that: strontium oxide in strontium residue hydrolysis liquid is transformed into soluble strontium salt through adding an acidulous salt, and a strontium element and an aluminum element are effectively separated. As the strontium salt solution is carbonized at normal temperature, the formed strontium carbonate has small particle diameter and high economic values; the recovery rate of the strontium oxide reaches 85%; and the strontium carbonate content of a product is more than 98.0%.
Description
Technical field
The invention belongs to chemical production technical field, relate to the metal waste residue and recycle, be specifically related to extract in a kind of residue of metal strontium the method for Strontium carbonate powder.
Background technology
Preparation of Metallic Strontium is used for alloying, vacuum photocell and analytical chemistry, pyrotechnics etc., in industries such as electronic information, chemical industry, light industry, medicine, pottery, metallurgy purposes is widely arranged.The working method of Preparation of Metallic Strontium has electrolytic process and metallothermics.The general vacuum thermit reduction that adopts prepares, and promptly makes raw material with the Strontium carbonate powder powder, is decomposed into strontium oxide through high-temperature roasting, again strontium oxide and aluminium powder generation reduction reaction is made Preparation of Metallic Strontium, by-product residue in the production process.The residue staple is strontium oxide and aluminum oxide, and wherein the content of strontium oxide is greatly about 46%.The strontium residue to utilize approach to have multiple, as as the pyrotechnics chromogenic reagent, the gas absorption siccative extracts strontium salt, solid base catalysts etc. are not complex process, are exactly that product purity is not high, added value is low, and environment is polluted.
Summary of the invention
The purpose of this invention is to provide in a kind of residue of metal strontium the method for extracting Strontium carbonate powder, practice thrift and utilize the strontium resource, turn waste into wealth, improve the yield and the quality of strontium product, reduce the Preparation of Metallic Strontium production cost, reduce pollution simultaneously environment.
Extract the method for Strontium carbonate powder in the residue of metal strontium of the present invention, its process is following:
⑴ be ground into small particles material with kibbler with residue of metal strontium.
⑵ add entry with the small particles material of pulverizing or in the slightly acidic salts solution, be hydrolyzed, and processes the slip that solid content is 0.1-0.3g/mL.
⑶ add the reaction that makes the transition of weakly alkaline salt in slip, adjustment ph value 7～10, and the temperature that react to transition is 15-95
oC stirred 1-5 hour.
⑷ back transition solution clarification 2-3 hour is carried out strontium aluminium and is separated, and obtains strontium salt solution and rich residue of aluminum.
⑸ adding bicarbonate of ammonia or volatile salt carry out carburizing reagent in the strontium salt solution, generate the Strontium carbonate powder throw out.
⑹ isolate throw out and mother liquor, and throw out obtains the finished product Strontium carbonate powder through rinsing, filtration, baking operation.
Whole process is an atmospheric operation, and hydrolysis and carbonation process are normal temperature.
Small particles material is 80 order screen underflows.Slightly acidic salt is ammonium chloride or an ammonium nitrate.The consumption of slightly acidic salt is 1-2 times of press reactive chemistry metering SrO transition (mol ratio).The add-on of bicarbonate of ammonia is 1-1.2 times that soluble strontium salt is converted into Strontium carbonate powder chemical reaction theoretical amount (mol ratio) in the strontium salt solution in the carburizing reagent.The acidifying of mother liquor and rinse water is with hydrochloric acid or nitric acid solution to be adjusted to pH value 5-6.Mother liquor and rinse water return hydrolyzing process and recycle after acidifying.Rich residue of aluminum after strontium salt solution separates is used for aluminium salt and reclaims.
Hydrolysis in the method for extraction Strontium carbonate powder, transition, carbonization and mother liquor acidifying reaction principle are in the residue of metal strontium of the present invention: →
Hydrolysis: SrO+H
2O → Sr (OH)
2
Transition: Sr (OH)
2+ 2NH
4Cl → SrCl
2+ 2NH
3↑+2H
2O
Sr(OH)
2+?2NH
4NO
3 → Sr(?NO
3)
2+2NH
3↑+2H
2O
Carbonization: SrCl
2+ 2 NH
4HCO
3→ SrCO
3↓+2 NH
4Cl+H
2O+ CO
2↑
Sr(?NO
3)
2+?NH
4HCO
3 → SrCO
3↓?+2?NH
4?NO
3+?H
2O?+?CO
2↑
Acidifying: NH
4HCO
3+ HCl → NH
4Cl+H
2O+CO
2↑
NH
4HCO
3?+?HNO
3 → NH
4?NO
3+?H
2O?+?CO
2↑
The present invention has the following advantages and effect with existing compared with techniques: strontium oxide makes the transition into soluble strontium salt in the adding slightly acidic salt strontium residue hydrolyzed solution excessively; Effectively separate strontium element and aluminium element, avoided a large amount of aluminium elements to be converted into aluminum soluble salt and got in the mother liquor.The mother liquor carbonization is carried out under normal temperature condition, and the Strontium carbonate powder particle diameter of formation is little, good physical and chemical properties, economic worth high, production cost is low.Mother liquor after the carbonization and rinse water can carry out cycling and reutilization after adding hydrochloric acid or nitric acid accent solution pH value, and rich residue of aluminum is preserved for the recovery of aluminium salt.The strontium oxide recovery can be up to 85% in the strontium residue, and the Strontium carbonate powder content of producing reaches the industrial magnesium strontium standard more than 98.0%.Whole production technology is simple, and is easy to operate, and no waste water and dregs produces, and environmental pollution is little, and the comprehensive utilization of resources rate is high.
Description of drawings
Fig. 1 is for extracting the flow process signal of Strontium carbonate powder in the residue of metal strontium of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further described, following examples are intended to illustrate the present invention rather than to further qualification of the present invention.
The process of extracting Strontium carbonate powder in the residue of metal strontium of the present invention is as shown in Figure 1, mainly may further comprise the steps: pulverizing, hydrolysis, transition, the separation of strontium aluminium, carbonization, product purification and recovery.Product purification comprises that rinsing, filtration, baking operation process strontium carbonate product.Being recovered as mother liquor and rinse water reclaims.With kibbler the strontium residue is ground into small-particle, makes it pass through 80 mesh sieves.The slip that solid content is 0.1-0.3g/mL is processed in the hydrolysis in water of strontium residue small-particle.Add slightly acidic salt and make SrO become soluble strontium salt transition, clarify 2～3 hours strontium salt solutions and separate with rich residue of aluminum.Strontium salt solution adds bicarbonate of ammonia and carries out carburizing reagent, gets the Strontium carbonate powder throw out; Clarify separation, isolated throw out gets the Strontium carbonate powder finished product through twice rinsing, filtration, baking operation.Isolated mother liquor and rinse water are with hydrochloric acid or nitric acid acidifying, and adjustment pH value of solution value 5-6 returns hydrolysis operation transition and recycles.
Embodiment 1
Take by weighing the residue of metal strontium particle after 100g pulverizes, adds in 500ml70 ℃ the water, the powerful stirring adds 20g ammonium chloride down, and surveying the pH value of solution value is 9, stirs to make the transition 2 hours.Clarified 2 hours, and filtered to isolate strontium salt solution and rich residue of aluminum, rich residue of aluminum is preserved for the recovery of aluminium salt.Add bicarbonate of ammonia in the filtrating, add-on is converted into 1.2 times of Strontium carbonate powder chemical reaction theoretical amount (mol ratio) for making soluble strontium salt in the strontium salt solution.To clarifying separation after the carbonization, with throw out rinsing twice, through filtration, dry the Strontium carbonate powder finished product.The content of the Strontium carbonate powder of finished product is 98.10%.Mother liquor and rinse water are with hydrochloric acid adjustment pH value to 6, as next batch strontium slag hydrolyzed solution.
Embodiment 2
Mother liquor after the acidifying that embodiment 1 obtains and rinse water, adding is crushed to 80 purpose strontium slag 100g, 30
oC stirs down and adds 18g ammonium chloride, and surveying the pH value of solution value is 9, stirs 4 hours transition, clarifies 2 hours, filters to isolate strontium salt solution and rich residue of aluminum, and rich residue of aluminum is preserved for the recovery of aluminium salt.Add bicarbonate of ammonia in the filtrating, add-on is soluble strontium salt is converted into Strontium carbonate powder chemical reaction theoretical amount (mol ratio) in the strontium salt solution 1.2 times.Feed liquid after the carbonization is clarified separation, twice of throw out rinsing, filtration, baking procedure are got the Strontium carbonate powder finished product.The Strontium carbonate powder content of finished product is 98.05%.Mother liquor and rinse water are with hydrochloric acid adjustment pH value to 6, as next batch strontium slag hydrolyzed solution.
Embodiment 3
Take by weighing the residue of metal strontium after 100g pulverizes, add in the 500ml90 ℃ of water, the powerful stirring adds 40g an ammonium nitrate down; Surveying the pH value of solution value is 9, stirs 2 hours transition, clarifies 2 hours; Filter to isolate strontium salt solution and rich residue of aluminum, rich residue of aluminum is preserved for the recovery of aluminium salt.Add bicarbonate of ammonia in the filtrating, add-on is to make soluble strontium salt in the strontium salt solution be converted into 1.1 times of Strontium carbonate powder chemical reaction theoretical amount.Feed liquid after the carbonization is clarified separation,, obtain the Strontium carbonate powder finished product through filtering, drying with throw out rinsing twice.The Strontium carbonate powder content of finished product is 98.24%.Mother liquor and rinse water are with nitric acid adjustment pH value to 6, as next batch strontium slag hydrolyzed solution.
Embodiment 4
Carbonization mother liquor after the acidifying that embodiment 3 obtains and wash water add to be crushed to and bear 80 purpose strontium slag 120g, 30
oC stirs down and adds 30g an ammonium nitrate, and surveying the pH value of solution value is 8, stirs 5 hours transition, clarifies 2 hours, filters to isolate strontium salt solution and rich residue of aluminum, and rich residue of aluminum is preserved for the recovery of aluminium salt.Add bicarbonate of ammonia in the filtrating, add-on is to make soluble strontium salt in the strontium salt solution be converted into 1.2 times of Strontium carbonate powder chemical reaction theoretical amount.Feed liquid after the carbonization is clarified separation, with throw out rinsing twice, filter, oven dry gets the Strontium carbonate powder finished product.The Strontium carbonate powder content of finished product is 98.17%.Mother liquor and rinse water are with nitric acid adjustment pH value to 6, as next batch strontium slag hydrolyzed solution.
Claims (8)
1. extract the method for Strontium carbonate powder in the residue of metal strontium, its process is following:
⑴ be ground into small particles material with kibbler with residue of metal strontium;
⑵ add entry with the small particles material of pulverizing or in the slightly acidic salts solution, be hydrolyzed, and processes the slip that solid content is 0.1-0.3g/mL;
⑶ the reaction that makes the transition: in slip, add the reaction that makes the transition of weakly alkaline salt, adjustment ph value 7～10, the temperature of reacting that makes the transition is 15-95
oC stirred 1-5 hour;
⑷ back transition solution clarification 2-3 hour is carried out strontium aluminium and is separated, and obtains strontium salt solution and rich residue of aluminum;
⑸ adding bicarbonate of ammonia or volatile salt carry out carburizing reagent in the strontium salt solution, generate the Strontium carbonate powder throw out;
⑹ isolate throw out and mother liquor, and throw out obtains the finished product Strontium carbonate powder through rinsing, filtration, baking operation;
Whole process is an atmospheric operation, and hydrolysis and carbonation process are normal temperature.
2. according to the method for extracting Strontium carbonate powder in the said residue of metal strontium of claim 1, it is characterized in that: said small particles material is 80 order screen underflows.
3. according to the method for extracting Strontium carbonate powder in the said residue of metal strontium of claim 1, it is characterized in that: said slightly acidic salt is ammonium chloride or an ammonium nitrate.
4. according to the method for extracting Strontium carbonate powder in the said residue of metal strontium of claim 3, it is characterized in that: the consumption of said slightly acidic salt is for press 1-2 times of SrO reactive chemistry transition metering.
5. according to the method for extracting Strontium carbonate powder in the said residue of metal strontium of claim 1, it is characterized in that: the add-on of bicarbonate of ammonia is 1-1.2 times that soluble strontium salt is converted into Strontium carbonate powder chemical reaction theoretical amount in the strontium salt solution in the said carburizing reagent.
6. according to the method for extracting Strontium carbonate powder in the said residue of metal strontium of claim 1, it is characterized in that: mother liquor and rinse water return hydrolyzing process and recycle after acidifying.
7. according to the method for extracting Strontium carbonate powder in the said residue of metal strontium of claim 6, it is characterized in that: said acidifying is with hydrochloric acid or nitric acid mother liquor and rinse water solution to be adjusted to pH value 5-6.
8. according to the method for extracting Strontium carbonate powder in the said residue of metal strontium of claim 1, it is characterized in that: the rich residue of aluminum after strontium salt solution separates is used for aluminium salt and reclaims.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103910372A (en) * | 2014-04-23 | 2014-07-09 | 河北辛集化工集团有限责任公司 | Novel method for preparing strontium carbonate for industrial use by using strontium salt residues |
| CN104016396A (en) * | 2014-06-27 | 2014-09-03 | 重庆邮电大学 | Preparation method of controllable-particle-size high-purity strontium carbonate |
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| CN101100308A (en) * | 2007-07-17 | 2008-01-09 | 南京云海特种金属股份有限公司 | Method for preparing strontium carbonate salt from metal strontium slag |
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2011
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103910372A (en) * | 2014-04-23 | 2014-07-09 | 河北辛集化工集团有限责任公司 | Novel method for preparing strontium carbonate for industrial use by using strontium salt residues |
| CN103910372B (en) * | 2014-04-23 | 2016-01-13 | 河北辛集化工集团有限责任公司 | A kind of novel method adopting strontium salt residue to prepare industrial magnesium strontium |
| CN104016396A (en) * | 2014-06-27 | 2014-09-03 | 重庆邮电大学 | Preparation method of controllable-particle-size high-purity strontium carbonate |
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