CN102534230B - 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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- CN102534230B CN102534230B CN201110456931.9A CN201110456931A CN102534230B CN 102534230 B CN102534230 B CN 102534230B CN 201110456931 A CN201110456931 A CN 201110456931A CN 102534230 B CN102534230 B CN 102534230B
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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 metal waste residue and recycle, be specifically related to a kind of method of extracting strontium carbonate from metal strontium residues.
Background technology
Preparation of Metallic Strontium, for the manufacture of alloy, phototube and analytical chemistry, pyrotechnics etc., has purposes widely in industries such as electronic information, chemical industry, light industry, medicine, pottery, metallurgy.The production method of Preparation of Metallic Strontium has electrolytic process and metallothermics.Prepared by the general vacuum aluminum hot reducing method that adopts, with Strontium carbonate powder powder, make raw material, is decomposed into strontium oxide, then strontium oxide and aluminium powder generation reduction reaction is made to Preparation of Metallic Strontium, by-product residue in production process through high-temperature roasting.Residue main component is strontium oxide and aluminum oxide, and wherein the content of strontium oxide is greatly about 46%.Strontium residue to utilize approach to have multiple, as pyrotechnics chromogenic reagent, 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 to environment.
Summary of the invention
A kind of method that the object of this invention is to provide extracting strontium carbonate from metal strontium residues, saves and utilizes strontium resource, turns waste into wealth, and improves yield and the quality of strontium product, reduces Preparation of Metallic Strontium production cost, reduces the pollution to environment simultaneously.
The method of extracting strontium carbonate from metal strontium residues of the present invention, its process is as follows:
(1) with pulverizer, residue of metal strontium is ground into small particles material.
(2) the small particles material of pulverizing added to water or be hydrolyzed in slightly acidic salts solution, making the slip that solid content is 0.1-0.3g/mL.
(3) in slip, add weakly alkaline salt to carry out isomerization, adjust ph value 7～10, the temperature of isomerization is 15-95
oc, stirs 1-5 hour.
(4) solution clarification 2-3 hour after transition, carries out the separation of strontium aluminium, obtains strontium salt solution and rich residue of aluminum.
(5) in strontium salt solution, add bicarbonate of ammonia or volatile salt to carry out carburizing reagent, generate Strontium carbonate powder throw out.
(6) isolate throw out and mother liquor, throw out obtains finished product Strontium carbonate powder through rinsing, filtration, baking operation.
Whole process is 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 ammonium nitrate.The consumption of slightly acidic salt is for press the 1-2 times of SrO isomerization stoichiometry (mol ratio).In carburizing reagent, the add-on of bicarbonate of ammonia is 1-1.2 times that in strontium salt solution, soluble strontium salt is converted into Strontium carbonate powder chemical reaction theoretical amount (mol ratio).The acidifying of mother liquor and rinse water is, with hydrochloric acid or nitric acid, solution is adjusted to pH value 5-6.Mother liquor and rinse water return to hydrolyzing process and recycle after acidifying.Rich residue of aluminum after strontium salt solution separation reclaims for aluminium salt.
The reaction principle of hydrolysis in the method for extracting strontium carbonate from metal strontium residues of the present invention, transition, carbonization and mother liquor acidifying is: →
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 compares and has the following advantages and effect with existing technology: cross and add strontium oxide in slightly acidic salt strontium residue hydrolyzed solution to make the transition into soluble strontium salt, effective separated strontium element and aluminium element, avoided a large amount of aluminium elements to be converted into aluminum soluble salt and entered in mother liquor.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 is high, production cost is low.Mother liquor after carbonization and rinse water can carry out cycling and reutilization after adding hydrochloric acid or nitric acid tune solution pH value, and rich residue of aluminum is preserved for the recovery of aluminium salt.In strontium residue, the strontium oxide rate of recovery can be up to 85%, and the Strontium carbonate powder content of producing, more than 98.0%, reaches industrial magnesium strontium standard.Whole production technique is simple, easy to operate, without waste water and dregs, produces, and environmental pollution is little, and comprehensive utilization of resources rate is high.
Accompanying drawing explanation
Fig. 1 is the flow process signal of extracting strontium carbonate from metal strontium residues of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described, and following examples are intended to illustrate the present invention rather than limitation of the invention further.
The process of extracting strontium carbonate from metal strontium residues of the present invention as shown in Figure 1, mainly comprises the following steps: pulverizing, hydrolysis, transition, the separation of strontium aluminium, carbonization, product purification and recovery.Product purification comprises that rinsing, filtration, baking operation make strontium carbonate product.Being recovered as mother liquor and rinse water reclaims.With pulverizer, strontium residue is ground into small-particle, makes it pass through 80 mesh sieves.Strontium residue small-particle is hydrolyzed in water, makes the slip that solid content is 0.1-0.3g/mL.Add slightly acidic salt to make SrO become soluble strontium salt transition, clarify 2～3 hours strontium salt solutions separated with rich residue of aluminum.Strontium salt solution adds bicarbonate of ammonia to carry out carburizing reagent, obtains Strontium carbonate powder throw out; Carry out clarified separation, isolated throw out obtains Strontium carbonate powder finished product through twice rinsing, filtration, baking operation.Hydrochloric acid or nitric acid acidifying for isolated mother liquor and rinse water, adjust pH 5-6, returns to hydrolysis operation transition and recycle.
Embodiment 1
Residue of metal strontium particle after taking 100g and pulverizing, adds in the water of 500ml70 ℃, adds 20g ammonium chloride under strong stirring, and surveying pH is 9, stirs 2 hours transition.Clarify 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.In filtrate, add bicarbonate of ammonia, add-on is for making soluble strontium salt in strontium salt solution be converted into 1.2 times of Strontium carbonate powder chemical reaction theoretical amount (mol ratio).To carrying out clarified separation after carbonization, by throw out rinsing twice, through filtering, drying, arrive to obtain Strontium carbonate powder finished product.The content of the Strontium carbonate powder of finished product is 98.10%.Mother liquor and rinse water are adjusted pH value to 6 with hydrochloric acid, as next batch strontium slag hydrolyzed solution.
Embodiment 2
Mother liquor after the acidifying that embodiment 1 obtains and rinse water, add and be crushed to 80 object strontium slag 100g, 30
oc adds 18g ammonium chloride under stirring, and surveying pH 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.In filtrate, add bicarbonate of ammonia, add-on is 1.2 times that in strontium salt solution, soluble strontium salt is converted into Strontium carbonate powder chemical reaction theoretical amount (mol ratio).Feed liquid after carbonization is carried out to clarified separation, twice of throw out rinsing, filtration, baking procedure are obtained to Strontium carbonate powder finished product.The Strontium carbonate powder content of finished product is 98.05%.Mother liquor and rinse water are adjusted pH value to 6 with hydrochloric acid, as next batch strontium slag hydrolyzed solution.
Embodiment 3
Take the residue of metal strontium after 100g pulverizes, add in 500ml90 ℃ of water, under strong stirring, add 40g ammonium nitrate, surveying pH 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.In filtrate, add bicarbonate of ammonia, add-on is to make soluble strontium salt in strontium salt solution be converted into 1.1 times of Strontium carbonate powder chemical reaction theoretical amount.Feed liquid after carbonization is carried out to clarified separation, by throw out rinsing twice, through filtering, drying, obtain Strontium carbonate powder finished product.The Strontium carbonate powder content of finished product is 98.24%.Mother liquor and rinse water are adjusted pH value to 6 with nitric acid, as next batch strontium slag hydrolyzed solution.
Embodiment 4
Carbonization mother liquor after the acidifying that embodiment 3 obtains and wash water, add and be crushed to negative 80 object strontium slag 120g, 30
oc adds 30g ammonium nitrate under stirring, and surveying pH 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.In filtrate, add bicarbonate of ammonia, add-on is to make soluble strontium salt in strontium salt solution be converted into 1.2 times of Strontium carbonate powder chemical reaction theoretical amount.Feed liquid after carbonization is carried out to clarified separation, by throw out rinsing twice, filter, dry, obtain Strontium carbonate powder finished product.The Strontium carbonate powder content of finished product is 98.17%.Mother liquor and rinse water are adjusted pH value to 6 with nitric acid, as next batch strontium slag hydrolyzed solution.
Claims (5)
1. a method for extracting strontium carbonate from metal strontium residues, its process is as follows:
(1) with pulverizer, residue of metal strontium is ground into small particles material;
(2) the small particles material of pulverizing added to water or be hydrolyzed in slightly acidic salts solution, making the slip that solid content is 0.1-0.3g/mL; Described slightly acidic salt is ammonium chloride or ammonium nitrate;
(3) isomerization: add weakly alkaline salt to carry out isomerization in slip, adjust pH value 7～10, the temperature of isomerization is 15-95
oc, stirs 1-5 hour;
(4) solution clarification 2-3 hour after transition, carries out the separation of strontium aluminium, obtains strontium salt solution and rich residue of aluminum;
(5) in strontium salt solution, add bicarbonate of ammonia or volatile salt to carry out carburizing reagent, generate Strontium carbonate powder throw out;
(6) isolate throw out and mother liquor, throw out obtains finished product Strontium carbonate powder through rinsing, filtration, baking operation;
Mother liquor and rinse water return to hydrolyzing process and recycle after acidifying; Described acidifying is, with hydrochloric acid or nitric acid, mother liquor and rinse water solution are adjusted to pH value 5-6; Whole process is atmospheric operation, and hydrolysis and carbonation process are normal temperature.
2. the method for extracting strontium carbonate from metal strontium residues according to claim 1, is characterized in that: described small particles material is 80 order screen underflows.
3. the method for extracting strontium carbonate from metal strontium residues according to claim 1, is characterized in that: the consumption of described slightly acidic salt is for press the stoichiometric 1-2 of SrO isomerization times.
4. the method for extracting strontium carbonate from metal strontium residues according to claim 1, is characterized in that: in described carburizing reagent the add-on of bicarbonate of ammonia be 1-1.2 that in strontium salt solution, soluble strontium salt is converted into Strontium carbonate powder chemical reaction theoretical amount doubly.
5. the method for extracting strontium carbonate from metal strontium residues according to claim 1, is characterized in that: the rich residue of aluminum after strontium salt solution separation reclaims for aluminium salt.
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| 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 |
| CN104016396B (en) * | 2014-06-27 | 2015-07-22 | 重庆邮电大学 | Preparation method of controllable-particle-size high-purity strontium carbonate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1609242A (en) * | 2004-02-03 | 2005-04-27 | 祁顺东 | Process for recovering strontium and aluminium from metal strontium residue |
| 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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| WO2011001282A2 (en) * | 2009-06-29 | 2011-01-06 | Bairong Li | Metal reduction processes, metallurgical processes and products and apparatus |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1609242A (en) * | 2004-02-03 | 2005-04-27 | 祁顺东 | Process for recovering strontium and aluminium from metal strontium residue |
| 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 |
Non-Patent Citations (4)
| Title |
|---|
| "碳酸锶渣中锶的氯化铵浸出回收工艺";徐龙君等;《重庆大学学报》;20081031;第31卷(第10期);第1174-1177,1184页 * |
| "锶尾矿和废渣的污染现状及资源化利用进展";徐龙君等;《资源环境与工程》;20080430;第22卷(第2期);第222-224,242页 * |
| 徐龙君等."碳酸锶渣中锶的氯化铵浸出回收工艺".《重庆大学学报》.2008,第31卷(第10期),第1174-1177,1184页. |
| 徐龙君等."锶尾矿和废渣的污染现状及资源化利用进展".《资源环境与工程》.2008,第22卷(第2期),第222-224,242页. |
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