CN106115760A - A kind of preparation method of nano strontium carbonate - Google Patents

A kind of preparation method of nano strontium carbonate Download PDF

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CN106115760A
CN106115760A CN201610477176.5A CN201610477176A CN106115760A CN 106115760 A CN106115760 A CN 106115760A CN 201610477176 A CN201610477176 A CN 201610477176A CN 106115760 A CN106115760 A CN 106115760A
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celestite
strontium
strontium carbonate
filtering residue
powder
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CN106115760B (en
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梅庆波
盛海丰
许博伟
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Chongqing Qinglong new Mstar Technology Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/18—Carbonates
    • C01F11/186—Strontium or barium carbonate
    • C01F11/187—Strontium carbonate
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/60—Compounds characterised by their crystallite size
    • 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
    • C01P2006/10—Solid density
    • 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
    • C01P2006/12—Surface area
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Fertilizers (AREA)
  • Cosmetics (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention discloses the preparation method of a kind of nano strontium carbonate, belong to strontium carbonate preparing technical field.After the present invention uses celestite to be raw material pulverizing, dissolve with the dilute sulfuric acid of excess to remove ingredients calcium carbonate therein, strontium sulfate therein is made to dissolve with dilute hydrochloric acid again, filter to remove the insoluble matters such as barium sulfate therein, again the strontium chloride solution obtained is mixed with the celestite surface microorganism bacterium colony cultivated voluntarily, utilize microbial cell surface with the organic substance of negative charge and strontium ion chelating in solution, microorganism is with carbamide as carbon source simultaneously, constantly decomposing urea makes the carbon acid ion concentration in microorganism surrounding medium be continuously increased, thus cause local carbanion and strontium ion concentration in solution to increase, both are combined into strontium carbonate crystal settling, nano strontium carbonate is obtained again through filtration drying.The invention has the beneficial effects as follows: preparation process of the present invention is simple, and products obtained therefrom impurity content reduces 70～80%, and activity improves 25～30%.

Description

A kind of preparation method of nano strontium carbonate
Technical field
The present invention relates to the preparation method of a kind of nano strontium carbonate, belong to strontium carbonate preparing technical field.
Background technology
Strontium carbonate, white powder or granule, odorless, tasteless.It is mainly used in glass bulb, magnetic material, metal smelt, strontium Prepared by salt, electronic component, fireworks.For manufacturing color television cathode ray tube, electric magnet, strontium ferrite, pyrotechnics, fluorescent glass, letter Number bullets etc., are also the raw materials producing other strontium salt, as special PTC thermistor element (switch activated, demagnetization, current-limiting protection, Constant temp. warming etc.) the basic powder that produces is the base stock producing strontium salt.As the carrier of palladium, can be used as hydrogenation.In addition It is additionally operable to refined, the metallic zinc electrolyte of the production of pyrotechnics, fluorescent glass, signal flare, papermaking, medicine, analytical reagent, and sugar Refined, strontium salt pigment manufacture etc..The production technology of strontium carbonate at present: 1. be to carry out double decomposition with ammonium carbonate after celestite pulverizing Reaction, obtains thick strontium carbonate, thick strontium carbonate and ammonium salt and carries out conversion reaction, after filter cleaner, adds ammonium carbonate and carries out precipitation instead Should, after filtration, filter cake drying, to pulverize, obtain strontium carbonate, the production method of above-mentioned strontium carbonate is complex, and production cost is high, Obtaining strontium carbonate impurity content high, activity is poor, it is impossible to for the production of fine Electronic pottery strontium titanates.2. replace salt with nitric acid Acid, mainly solves chloride control problem in said method, but synthesis particle diameter is bigger than normal, and production cost is high, and product is applicable to produce Luminescent materials etc., are difficult to use as electronic grade product.Work out a kind of impurity content the most on this basis low, active good Strontium carbonate, has important economic benefit and social value.
Summary of the invention
The technical problem to be solved: the strontium carbonate impurity content prepared for current method is high, and activity is poor, The drawback that particle diameter is big and production cost is high, it is provided that a kind of employing celestite is raw material, after pulverizing, dissolves with the dilute sulfuric acid of excess To remove ingredients calcium carbonate therein, then make strontium sulfate therein dissolve with dilute hydrochloric acid, filter to remove barium sulfate therein etc. Insoluble matter, then the strontium chloride solution obtained is mixed with the celestite surface microorganism bacterium colony cultivated voluntarily, utilize microorganism thin Cellular surface is with the organic substance of negative charge and the Sr in solution2+Chelating, microorganism is with carbamide as carbon source simultaneously, constantly decomposes urine Element, makes the carbon acid ion concentration in microorganism surrounding medium be continuously increased, thus cause in solution local carbanion and Sr2+Concentration increases, and both are combined into strontium carbonate crystal settling and separate out, then the method obtaining nano strontium carbonate through filtration drying.This Invention preparation process is simple, and products obtained therefrom impurity content is low, and activity is good, and particle diameter is little.
For solving above-mentioned technical problem, the present invention uses the technical scheme as described below to be:
(1) weigh 80～150kg celestite, pulverize 15～20min with Universalpulverizer, cross 150～200 mesh sieves, obtain the most reddish black Stone powder, then to be proceeded to fill 160～200mL mass concentrations be 2～5% in sulphuric acid, with magnetic stirring apparatus with 200～400r/ Min stirring 20～30min, filters to obtain filtering residue, is washed with deionized filtering residue 3～5 times, is dried 2～3h, obtains pretreatment celestite Powder；
(2) above-mentioned gained pretreatment celestite powder is added that to fill 120～150mL mass concentrations be 2～4% in hydrochloric acid, use magnetic Power agitator, with 300～500r/min stirrings 30～40min, filters to get filtrate, standby；
(3) 8～10g Carnis Bovis seu Bubali creams, 3～5g peptones, 3～5g potassium chloride, 0.5～0.8g calcium chloride, 1～2g sulphuric acid are weighed successively Magnesium and 15～20g agar, be dissolved in 1～2L deionized water, with mass concentration be 12～15% ammonia regulation pH to 8.0～8.6, Proceeding in pressure steam sterilizer by mixture again, under the conditions of 0.06～0.08MPa, sterilizing 30～40min, obtain cultivation Base；
(4) 50～60g celestite surface soils are weighed, it is evenly laid out in above-mentioned culture medium, then culture medium is moved to perseverance In temperature shaking table, after cultivating 3～5 days under the conditions of 100～120r/min, 26～28 DEG C, with 120～180mL deionized water drip washing Media surface, collect leacheate, obtain hyphal suspension, then proceeded in centrifuge, with 2500～2800r/min rotating speeds from The heart separates 20～30min, collects to obtain supernatant；
(5) step (2) standby filtrate and above-mentioned gained supernatant are simultaneously introduced in reactor, are warming up to 30～32 DEG C, then use Mass concentration be 18～20% urea liquid regulation pH to 8.2～8.4, subsequent start-up agitator, with 600～800r/min rotating speeds Stirring reaction 8～10h, filters to obtain filtering residue, is washed with deionized filtering residue 3～5 times, then gained filtering residue is put into 85～95 DEG C of bakings Case is dried 3～5h, obtains white powder, i.e. nano strontium carbonate.
The principle of the present invention: employing celestite is raw material, after pulverizing, dissolves with the dilute sulfuric acid of excess to remove carbon therein Acid calcium component, then make strontium sulfate therein dissolve with dilute hydrochloric acid, filter to remove the insoluble matters such as barium sulfate therein, then will obtain Strontium chloride solution mix with the celestite surface microorganism bacterium colony cultivated voluntarily, utilize microbial cell surface with negative charge Organic substance and solution in Sr2+Chelating, meanwhile, microorganism with carbamide as carbon source, continuous decomposing urea, make around microorganism (CO in solution3)2+Concentration is continuously increased, thus causes local (CO in solution3)2+And Sr2+Concentration increases, and both are combined into carbon Acid strontium crystal precipitation, then obtain nano strontium carbonate through filtration drying.
The nano strontium carbonate density 3.70～3.72g/cm that the present invention prepares3, lattice paprmeter is 0.612～0.842nm, than Surface area is 100～155m2/ g, at 25 DEG C, vapour pressure is 48.9～49.8mmHg, at 20 DEG C dissolubility be 658～ 660g/L。
The application process of the present invention: the present invention is compared with additive method, and Advantageous Effects is:
(1) preparation process of the present invention is simple, and production cost reduces 20～22%；
(2) products obtained therefrom impurity content reduces 70～80%, and activity improves 25～30%, and particle diameter is little.
Detailed description of the invention
First weigh 80～150kg celestite, pulverize 15～20min with Universalpulverizer, cross 150～200 mesh sieves, obtain carefully Celestite powder, then to be proceeded to fill 160～200mL mass concentrations be 2～5% in sulphuric acid, with magnetic stirring apparatus with 200～ 400r/min stirring 20～30min, filters to obtain filtering residue, is washed with deionized filtering residue 3～5 times, is dried 2～3h, obtains pretreatment Celestite powder；Then above-mentioned gained pretreatment celestite powder is added to fill 120～150mL mass concentrations be 2～4% salt In acid, with magnetic stirring apparatus with 300～500r/min stirrings 30～40min, filter to get filtrate, standby；Weigh the most successively 8～ 10g Carnis Bovis seu Bubali cream, 3～5g peptones, 3～5g potassium chloride, 0.5～0.8g calcium chloride, 1～2g magnesium sulfate and 15～20g agar, molten In 1～2L deionized water, it is 12～15% ammonia regulation pH to 8.0～8.6 by mass concentration, then mixture is proceeded to pressure In steam autoclave, under the conditions of 0.06～0.08MPa, sterilizing 30～40min, obtain culture medium；Weigh 50～60g reddish black Stone surface soil, it is evenly laid out in above-mentioned culture medium, then culture medium is moved in constant-temperature table, 100～120r/ Min, cultivate 3～5 days under the conditions of 26～28 DEG C after, by 120～180mL deionized water drip washing media surface, collection leacheate, Obtain hyphal suspension, then proceeded in centrifuge, with 2500～2800r/min rotating speed centrifugations 20～30min, collect Supernatant；Finally standby filtrate and above-mentioned gained supernatant are simultaneously introduced in reactor, are warming up to 30～32 DEG C, then use quality Concentration be 18～20% urea liquid regulation pH to 8.2～8.4, subsequent start-up agitator, with 600～800r/min rotating speeds stirring Reaction 8～10h, filters to obtain filtering residue, is washed with deionized filtering residue 3～5 times, then is put into by gained filtering residue in 85～95 DEG C of baking ovens It is dried 3～5h, obtains white powder, i.e. nano strontium carbonate.
Example 1
First weigh 80kg celestite, pulverize 15min with Universalpulverizer, cross 150 mesh sieves, obtain thin celestite powder, then by it Proceeding to fill 160mL mass concentration is in 2% sulphuric acid, stirs 20min with magnetic stirring apparatus with 200r/min, filters to obtain filtering residue, uses Deionized water wash filtering residue 3 times, is dried 2h, obtains pretreatment celestite powder；Then by above-mentioned gained pretreatment celestite powder It is in 2% hydrochloric acid that addition fills 120mL mass concentration, stirs 30min with magnetic stirring apparatus with 300r/min, filters to get filtrate, standby With；Weigh 8g Carnis Bovis seu Bubali cream, 3g peptone, 3g potassium chloride, 0.5g calcium chloride, 1g magnesium sulfate and 15g agar the most successively, be dissolved in 1L and go In ionized water, it is 12% ammonia regulation pH to 8.0 by mass concentration, then mixture is proceeded in pressure steam sterilizer, Sterilizing 30min under the conditions of 0.06MPa, obtains culture medium；Weigh 50g celestite surface soil, it is evenly laid out in above-mentioned In culture medium, then culture medium is moved in constant-temperature table, 100r/min, cultivate 3 days under the conditions of 26 DEG C after, with 120mL go from Sub-water wash media surface, collects leacheate, obtains hyphal suspension, then proceeded in centrifuge, with 2500r/min rotating speed Centrifugation 20min, collects to obtain supernatant；Finally standby filtrate and above-mentioned gained supernatant are simultaneously introduced in reactor, rise Temperature is to 30 DEG C, then is 18% urea liquid regulation pH to 8.2 by mass concentration, and subsequent start-up agitator stirs with 600r/min rotating speed Mix reaction 8h, filter to obtain filtering residue, be washed with deionized filtering residue 3 times, then gained filtering residue is put into dry 3h in 85 DEG C of baking ovens, White powder, i.e. nano strontium carbonate.Preparation process of the present invention is simple, and production cost reduces 20%；Products obtained therefrom impurity content drops Low by 70%, activity improves 25%, and particle diameter is little；Nano strontium carbonate density 3.70g/cm prepared3, lattice paprmeter is 0.612nm, Specific surface area is 100m2/ g, at 25 DEG C, vapour pressure is 48.9mmHg, and at 20 DEG C, dissolubility is 658g/L.
Example 2
First weigh 115kg celestite, pulverize 18min with Universalpulverizer, cross 175 mesh sieves, obtain thin celestite powder, then by it Proceeding to fill 180mL mass concentration is in 3% sulphuric acid, stirs 25min with magnetic stirring apparatus with 300r/min, filters to obtain filtering residue, uses Deionized water wash filtering residue 4 times, is dried 3h, obtains pretreatment celestite powder；Then by above-mentioned gained pretreatment celestite powder It is in 3% hydrochloric acid that addition fills 135mL mass concentration, stirs 35min with magnetic stirring apparatus with 400r/min, filters to get filtrate, standby With；Weigh 9g Carnis Bovis seu Bubali cream, 4g peptone, 4g potassium chloride, 0.7g calcium chloride, 2g magnesium sulfate and 18g agar the most successively, be dissolved in 2L and go In ionized water, it is 13% ammonia regulation pH to 8.3 by mass concentration, then mixture is proceeded in pressure steam sterilizer, Sterilizing 35min under the conditions of 0.07MPa, obtains culture medium；Weigh 55g celestite surface soil, it is evenly laid out in above-mentioned In culture medium, then culture medium is moved in constant-temperature table, 110r/min, cultivate 4 days under the conditions of 27 DEG C after, with 150mL go from Sub-water wash media surface, collects leacheate, obtains hyphal suspension, then proceeded in centrifuge, with 2650r/min rotating speed Centrifugation 25min, collects to obtain supernatant；Finally standby filtrate and above-mentioned gained supernatant are simultaneously introduced in reactor, rise Temperature is to 31 DEG C, then is 19% urea liquid regulation pH to 8.3 by mass concentration, and subsequent start-up agitator stirs with 700r/min rotating speed Mix reaction 9h, filter to obtain filtering residue, be washed with deionized filtering residue 4 times, then gained filtering residue is put into dry 4h in 90 DEG C of baking ovens, White powder, i.e. nano strontium carbonate.Preparation process of the present invention is simple, and production cost reduces 21%；Products obtained therefrom impurity content drops Low by 75%, activity improves 28%, and particle diameter is little；Nano strontium carbonate density 3.71g/cm prepared3, lattice paprmeter is 0.727nm, Specific surface area is 130m2/ g, at 25 DEG C, vapour pressure is 49.4mmHg, and at 20 DEG C, dissolubility is 659g/L.
Example 3
First weigh 150kg celestite, pulverize 20min with Universalpulverizer, cross 200 mesh sieves, obtain thin celestite powder, then by it Proceeding to fill 200mL mass concentration is in 5% sulphuric acid, stirs 30min with magnetic stirring apparatus with 400r/min, filters to obtain filtering residue, uses Deionized water wash filtering residue 5 times, is dried 3h, obtains pretreatment celestite powder；Then by above-mentioned gained pretreatment celestite powder It is in 4% hydrochloric acid that addition fills 150mL mass concentration, stirs 40min with magnetic stirring apparatus with 500r/min, filters to get filtrate, standby With；Weigh 10g Carnis Bovis seu Bubali cream, 5g peptone, 5g potassium chloride, 0.8g calcium chloride, 2g magnesium sulfate and 20g agar the most successively, be dissolved in 2L In deionized water, it is 15% ammonia regulation pH to 8.6 by mass concentration, then mixture is proceeded in pressure steam sterilizer, Sterilizing 40min under the conditions of 0.08MPa, obtains culture medium；Weigh 60g celestite surface soil, it is evenly laid out in above-mentioned In culture medium, then culture medium is moved in constant-temperature table, 120r/min, cultivate 5 days under the conditions of 28 DEG C after, with 180mL go from Sub-water wash media surface, collects leacheate, obtains hyphal suspension, then proceeded in centrifuge, with 2800r/min rotating speed Centrifugation 30min, collects to obtain supernatant；Finally standby filtrate and above-mentioned gained supernatant are simultaneously introduced in reactor, rise Temperature is to 32 DEG C, then is 20% urea liquid regulation pH to 8.4 by mass concentration, and subsequent start-up agitator stirs with 800r/min rotating speed Mix reaction 10h, filter to obtain filtering residue, be washed with deionized filtering residue 5 times, then gained filtering residue is put into dry 5h in 95 DEG C of baking ovens, Obtain white powder, i.e. nano strontium carbonate.Preparation process of the present invention is simple, and production cost reduces 22%；Products obtained therefrom impurity content Reducing 80%, activity improves 30%, and particle diameter is little；Nano strontium carbonate density 3.72g/cm prepared3, lattice paprmeter is 0.842nm, Specific surface area is 155m2/ g, at 25 DEG C, vapour pressure is 49.8mmHg, and at 20 DEG C, dissolubility is 660g/L.

Claims (1)

1. the preparation method of a nano strontium carbonate, it is characterised in that concrete preparation process is:
(1) weigh 80～150kg celestite, pulverize 15～20min with Universalpulverizer, cross 150～200 mesh sieves, obtain the most reddish black Stone powder, then to be proceeded to fill 160～200mL mass concentrations be 2～5% in sulphuric acid, with magnetic stirring apparatus with 200～400r/ Min stirring 20～30min, filters to obtain filtering residue, is washed with deionized filtering residue 3～5 times, is dried 2～3h, obtains pretreatment celestite Powder；
(2) above-mentioned gained pretreatment celestite powder is added that to fill 120～150mL mass concentrations be 2～4% in hydrochloric acid, use magnetic Power agitator, with 300～500r/min stirrings 30～40min, filters to get filtrate, standby；
(3) 8～10g Carnis Bovis seu Bubali creams, 3～5g peptones, 3～5g potassium chloride, 0.5～0.8g calcium chloride, 1～2g sulphuric acid are weighed successively Magnesium and 15～20g agar, be dissolved in 1～2L deionized water, with mass concentration be 12～15% ammonia regulation pH to 8.0～8.6, Proceeding in pressure steam sterilizer by mixture again, under the conditions of 0.06～0.08MPa, sterilizing 30～40min, obtain cultivation Base；
(4) 50～60g celestite surface soils are weighed, it is evenly laid out in above-mentioned culture medium, then culture medium is moved to perseverance In temperature shaking table, after cultivating 3～5 days under the conditions of 100～120r/min, 26～28 DEG C, with 120～180mL deionized water drip washing Media surface, collect leacheate, obtain hyphal suspension, then proceeded in centrifuge, with 2500～2800r/min rotating speeds from The heart separates 20～30min, collects to obtain supernatant；
(5) step (2) standby filtrate and above-mentioned gained supernatant are simultaneously introduced in reactor, are warming up to 30～32 DEG C, then use Mass concentration be 18～20% urea liquid regulation pH to 8.2～8.4, subsequent start-up agitator, with 600～800r/min rotating speeds Stirring reaction 8～10h, filters to obtain filtering residue, is washed with deionized filtering residue 3～5 times, then gained filtering residue is put into 85～95 DEG C of bakings Case is dried 3～5h, obtains white powder, i.e. nano strontium carbonate.
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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN107010650A (en) * 2017-04-21 2017-08-04 孙祎 A kind of preparation method of nm-class active calcium carbonate

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CN101906440A (en) * 2010-06-30 2010-12-08 西南科技大学 Method for preparing barium carbonate and strontium carbonate through microorganism mineralization
CN104313055A (en) * 2014-09-25 2015-01-28 南京工业大学 Microbial preparation method of strontium carbonate

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CN101906440A (en) * 2010-06-30 2010-12-08 西南科技大学 Method for preparing barium carbonate and strontium carbonate through microorganism mineralization
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107010650A (en) * 2017-04-21 2017-08-04 孙祎 A kind of preparation method of nm-class active calcium carbonate

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