CN109179473A - A kind of short-cut method and device preparing coralliform carbonic acid strontium crystal - Google Patents

A kind of short-cut method and device preparing coralliform carbonic acid strontium crystal Download PDF

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CN109179473A
CN109179473A CN201811243149.7A CN201811243149A CN109179473A CN 109179473 A CN109179473 A CN 109179473A CN 201811243149 A CN201811243149 A CN 201811243149A CN 109179473 A CN109179473 A CN 109179473A
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crystal
coralliform
strontium
carbonic acid
overflow
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CN109179473B (en
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刘俊辰
钟学明
徐玉娜
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Nanchang Hangkong University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/18Carbonates
    • C01F11/186Strontium or barium carbonate
    • C01F11/187Strontium carbonate
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

A kind of short-cut method and device for preparing coralliform carbonic acid strontium crystal of the present invention, using Strontium dichloride hexahydrate and ammonium hydrogen carbonate as reactant, starch is bionical assembling agent, prepares coralliform carbonic acid strontium crystal.In designed reaction unit, Strontium dichloride hexahydrate, ammonium hydrogen carbonate and starch solution is added, is reacted at room temperature.The crystal generated in device is filtered after reaction 48 hours, is distilled water washing 3 times, obtains the coralliform carbonic acid strontium crystal being made of crystal bar after 1 hour dry in 105 DEG C, crystal bar diameter is the nm of 100 nm~200, length is 0.6 μm~2.0 μm, product purity >=99%, and yield is 95%~97%.The present invention has the characteristics that preparation efficiency is high, environmental-friendly, low energy consumption, easy to industrialized production, production cost is low.

Description

A kind of short-cut method and device preparing coralliform carbonic acid strontium crystal
Technical field
A kind of short-cut method and device for preparing coralliform carbonic acid strontium crystal of the present invention, more particularly to one kind with six water two Strontium chloride and sodium bicarbonate are reactant, and starch is bionical assembling agent, and it is brilliant that coralliform strontium carbonate is prepared in unique reaction unit Body.Particular technique field of the present invention is the preparation method of coralliform carbonic acid strontium crystal.
Background technique
Carbonic acid strontium crystal has extensive use value in production fields such as glass, coating, electronics.Currently, preparing carbonic acid The method of strontium crystal mainly has mechanochemical method, hypergravity reaction precipitation, solvent-thermal process method and biosimulation self assembly Method.
In the existing method for preparing carbonic acid strontium crystal, mechanochemical method mostly uses two kinds of solution rapid high intensity machinery mixed The mode of conjunction prepares carbonic acid strontium crystal, then by hydrolysis, evaporates, and the series of steps such as distillation sink metal ion compound It forms sediment or crystallizes out, using carbonic acid strontium crystal is obtained after heat treatment, the equipment operation used in the method is complex, behaviour It is more to make step, and needs to be added the organic reagents such as EDTA, ethyl alcohol, acetone, generates pollution of the organic wastewater to environment, and produce Object particle diameter distribution is uneven, and granularity not enough refines, and industry amplification is difficult.Hypergravity reaction rule is to need to utilize hypergravity rotary filling Material bed formed Elevated Gravity make reactive crystallization, required experimental facilities energy consumption is larger, and price is more expensive, to operator require compared with Height, and react and need that organic additive is added, to the seriously polluted of environment.Solvent-thermal process method needs to improve reaction temperature extremely 300 DEG C or more, reaction temperature is higher, consumes energy larger, and the method needs to add surfactant, the use of surfactant Cost is increased, big to the pollution of environment, the stability of especially technique is lower, and industrialized production wants the precision of measuring equipment Ask higher.Biosimulation self-assembly method needs to act on the reaction for promoting ion by biological enzymeization using microculture, raw Object simulation self-assembly method difficulty is big, complicated for operation, to the more demanding and poor controllability of equipment.
It follows that the existing method for preparing carbonic acid strontium crystal is there are complicated for operation, to the more demanding of consersion unit, ring The deficiencies of border is seriously polluted, and controllability is low, energy consumption is larger, high production cost.
The present invention is directed to the deficiency of existing carbonic acid strontium crystal preparation method, proposes a kind of coralliform carbonic acid strontium crystal of preparing Short-cut method and device.The present invention has preparation efficiency high (purity is high of carbonic acid strontium crystal, yield are high), environmental-friendly (raw material Be nontoxic reagent), low energy consumption (reaction temperature is room temperature), easy to industrialized production (raw material is easy to get, equipment is simple, It is easy to operate, process flow is short), the features such as production cost low (cost of material is low, low energy consumption).
Summary of the invention
The disadvantages of present invention is directed to existing carbonic acid strontium crystal preparation condition harshness and complicated operation, proposes a kind of prepare The short-cut method and device of coralliform carbonic acid strontium crystal.A kind of short-cut method and dress for preparing coralliform carbonic acid strontium crystal of the present invention It sets with preparation efficiency height, the features such as environmental-friendly, low energy consumption, easy to industrialized production, and production cost is low.
A kind of short-cut method and device for preparing coralliform carbonic acid strontium crystal of the present invention, with Strontium dichloride hexahydrate and bicarbonate Ammonium is reactant, and starch is bionical assembling agent, and it is brilliant to prepare the coralliform strontium carbonate being made of crystal bar at room temperature in reaction unit Body.
The short-cut method specifically: according to quality than Strontium dichloride hexahydrate: ammonium hydrogen carbonate=1: 1.06~1.18, it will Strontium dichloride hexahydrate is placed in the No.1 material trough (4) of reaction unit, and ammonium hydrogen carbonate is placed in No. two material troughs (5). 0.020% starch solutions successively are added to being lower than No.1 overflow lip (1) and No. two excessive to No.1 material trough (4) and No. two material troughs (5) Along 1 cm under mouth (3), area then is formed to crystallization and is added on 0.020% starch solution to No.1 overflow lip (1) and No. two overflow lips (3) Edge.The crystal generated in reaction unit is filtered after reaction 48 hours, is washed with distilled water 3 times, after 105 DEG C 1 hour dry The coralliform carbonic acid strontium crystal being made of crystal bar is obtained, crystal bar diameter is the nm of 100 nm~200, and length is 0.6 μm ~2.0 μm, product purity >=99%, yield is 95%~97%.
The device are as follows: square reactive tank (6), its side length is 60 cm, volume is 216 L.It is placed among reactive tank No.1 material trough (4) and No. two material troughs (5), the inner wall and No.1 material trough (4) and No. two material troughs of square reactive tank (6) It (5) is Crystallization area between;It is separated between No.1 material trough (4) and No. two material troughs (5) by partition (2).No.1 material trough (4) a length of 40 cm, width is 20 cm, a height of 60 cm, volume are 48 L.A length of 40 cm, the width 20 of No. two material troughs (5) Cm, a height of 60 cm, volume are 48 L.In No.1 material trough (4), distance opens up No.1 overflow lip (1) along 5 cm thereon, No. two objects Hopper (5) distance opens up No. two overflow lips (3) along 5 cm thereon, a length of equal 20 cm of No.1 overflow lip (1) and No. two overflow lips (3), Wide be 5 cm, area is 100 cm2
Beneficial effects of the present invention: 1) preparation efficiency is high.The purity of carbonic acid strontium crystal is >=99%, and yield is 95%~97%. Obviously, product purity is high, and yield is high.Strontium carbonate crystal development is complete.2) environmental-friendly.The originals such as strontium chloride, sodium bicarbonate, starch Material is nontoxic reagent.3) low energy consumption.Reaction is completed under field conditions (factors), is not necessarily to the decompressions such as heating, pressurization, cooling, Reaction condition is mild.4) easy to industrialized production.Raw material is easy to get, and equipment is simple, easy to operate, and process flow is short.5) it is produced into This is low.Low in raw material price, energy consumption are extremely low.
Detailed description of the invention
Fig. 1 is the SEM figure of coralliform carbonic acid strontium crystal prepared by the present invention.
Fig. 2 is the XRD diagram of coralliform carbonic acid strontium crystal prepared by the present invention.
Fig. 3 is the reaction unit schematic diagram of present invention preparation coralliform carbonic acid strontium crystal.In Fig. 3,1, No.1 overflow lip;2, every Plate;3, No. two overflow lips;4, No.1 material trough;5, No. two material troughs;6, square reactive tank.
Specific embodiment
Combined with specific embodiments below to a kind of short-cut method for preparing coralliform carbonic acid strontium crystal of the present invention and Device is further described.
Embodiment 1
1.80 kg Strontium dichloride hexahydrates are placed in No.1 material trough (4), 1.93 kg ammonium hydrogen carbonate are placed in No. two objects In hopper (5).0.020% starch solutions successively are added to being lower than No.1 overflow lip to No.1 material trough (4) and No. two material troughs (5) (1) along 1 cm and under No. two overflow lips (3), 0.020% starch solution then is added to No.1 overflow lip (1) and two to Crystallization area Edge on number overflow lip (3);The crystal generated in reaction unit is filtered after reaction 48 hours, is washed with distilled water 3 times, in 105 DEG C The coralliform carbonic acid strontium crystal being made of crystal bar is obtained after 1 hour dry, crystal bar diameter is the nm of 100 nm~200, long Degree is 0.6 μm~2.0 μm, product purity >=99%, yield 96%.
The reaction unit are as follows: square reactive tank (6), its side length is 60 cm, volume is 216 L.Among reactive tank Place No.1 material trough (4) and No. two material troughs (5), the inner wall and No.1 material trough (4) and No. two objects of square reactive tank (6) It is Crystallization area between hopper (5);It is separated between No.1 material trough (4) and No. two material troughs (5) by partition (2).No.1 object A length of 40 cm, the width of hopper (4) are 20 cm, a height of 60 cm, volume are 48 L.A length of 40 cm, the width of No. two material troughs (5) It is 48 L for 20 cm, a height of 60 cm, volume.In No.1 material trough (4), distance opens up No.1 overflow lip (1) along 5 cm thereon, No. two material troughs (5) distance opens up No. two overflow lips (3) along 5 cm thereon, No.1 overflow lip (1) and No. two overflow lips (3) it is a length of equal 20 cm, it is wide be 5 cm, area be 100 cm2
Embodiment 2
1.80 kg Strontium dichloride hexahydrates are placed in No.1 material trough (4), 1.82 kg ammonium hydrogen carbonate are placed in No. two objects In hopper (5).0.020% starch solutions successively are added to being lower than No.1 overflow lip to No.1 material trough (4) and No. two material troughs (5) (1) along 1 cm and under No. two overflow lips (3), 0.020% starch solution then is added to No.1 overflow lip (1) and two to Crystallization area Edge on number overflow lip (3);The crystal generated in reaction unit is filtered after reaction 48 hours, is washed with distilled water 3 times, in 105 DEG C The coralliform carbonic acid strontium crystal being made of crystal bar is obtained after 1 hour dry, crystal bar diameter is the nm of 100 nm~200, long Degree is 0.6 μm~2.0 μm, product purity >=99%, yield 95%.
The reaction unit are as follows: square reactive tank (6), its side length is 60 cm, volume is 216 L.Among reactive tank Place No.1 material trough (4) and No. two material troughs (5), the inner wall and No.1 material trough (4) and No. two objects of square reactive tank (6) It is Crystallization area between hopper (5);It is separated between No.1 material trough (4) and No. two material troughs (5) by partition (2).No.1 object A length of 40 cm, the width of hopper (4) are 20 cm, a height of 60 cm, volume are 48 L.A length of 40 cm, the width of No. two material troughs (5) It is 48 L for 20 cm, a height of 60 cm, volume.In No.1 material trough (4), distance opens up No.1 overflow lip (1) along 5 cm thereon, No. two material troughs (5) distance opens up No. two overflow lips (3) along 5 cm thereon, No.1 overflow lip (1) and No. two overflow lips (3) it is a length of equal 20 cm, it is wide be 5 cm, area be 100 cm2
Embodiment 3
1.80 kg Strontium dichloride hexahydrates are placed in No.1 material trough (4), 2.04 kg ammonium hydrogen carbonate are placed in No. two objects In hopper (5).0.020% starch solutions successively are added to being lower than No.1 overflow lip to No.1 material trough (4) and No. two material troughs (5) (1) along 1 cm and under No. two overflow lips (3), 0.020% starch solution then is added to No.1 overflow lip (1) and two to Crystallization area Edge on number overflow lip (3);The crystal generated in reaction unit is filtered after reaction 48 hours, is washed with distilled water 3 times, in 105 DEG C The coralliform carbonic acid strontium crystal being made of crystal bar is obtained after 1 hour dry, crystal bar diameter is the nm of 100 nm~200, long Degree is 0.6 μm~2.0 μm, product purity >=99%, yield 97%.
The reaction unit are as follows: square reactive tank (6), its side length is 60 cm, volume is 216 L.Among reactive tank Place No.1 material trough (4) and No. two material troughs (5), the inner wall and No.1 material trough (4) and No. two objects of square reactive tank (6) It is Crystallization area between hopper (5);It is separated between No.1 material trough (4) and No. two material troughs (5) by partition (2).No.1 object A length of 40 cm, the width of hopper (4) are 20 cm, a height of 60 cm, volume are 48 L.A length of 40 cm, the width of No. two material troughs (5) It is 48 L for 20 cm, a height of 60 cm, volume.In No.1 material trough (4), distance opens up No.1 overflow lip (1) along 5 cm thereon, No. two material troughs (5) distance opens up No. two overflow lips (3) along 5 cm thereon, No.1 overflow lip (1) and No. two overflow lips (3) it is a length of equal 20 cm, it is wide be 5 cm, area be 100 cm2

Claims (1)

1. a kind of short-cut method and device for preparing coralliform carbonic acid strontium crystal, it is characterised in that: the short-cut method is with six Chloride hydrate strontium and ammonium hydrogen carbonate are reactant, and starch is bionical assembling agent, prepare coralliform carbon at room temperature in reaction unit Sour strontium crystal;
The short-cut method specifically: according to quality than Strontium dichloride hexahydrate: ammonium hydrogen carbonate=1: 1.06~1.18, by six water It closes strontium chloride to be placed in the No.1 material trough (4) of reaction unit, ammonium hydrogen carbonate is placed in No. two material troughs (5);Successively 0.020% starch solutions are added to being lower than No.1 overflow lip (1) and No. two overflow lips to No.1 material trough (4) and No. two material troughs (5) (3) along 1 cm under, edge on 0.020% starch solution to No.1 overflow lip (1) and No. two overflow lips (3) then is added to Crystallization area; The crystal generated in reaction unit is filtered after reaction 48 hours, is washed with distilled water 3 times, is obtained after 1 hour dry in 105 DEG C The coralliform carbonic acid strontium crystal being made of crystal bar, crystal bar diameter are the nm of 100 nm~200, and length is 0.6 μm~2.0 μm, product purity >=99%, yield is 95%~97%;
The device are as follows: square reactive tank (6), its side length is 60 cm, volume is 216 L;No.1 is placed among reactive tank Material trough (4) and No. two material troughs (5), the inner wall of square reactive tank (6) and No.1 material trough (4) and No. two material troughs (5) Between be Crystallization area;It is separated between No.1 material trough (4) and No. two material troughs (5) by partition (2);No.1 material trough (4) A length of 40 cm, width be 20 cm, a height of 60 cm, volume are 48 L;A length of 40 cm, the width 20 of No. two material troughs (5) Cm, a height of 60 cm, volume are 48 L;In No.1 material trough (4), distance opens up No.1 overflow lip (1) along 5 cm thereon, No. two objects Hopper (5) distance opens up No. two overflow lips (3) along 5 cm thereon, a length of equal 20 cm of No.1 overflow lip (1) and No. two overflow lips (3), Wide be 5 cm, area is 100 cm2
CN201811243149.7A 2018-10-24 2018-10-24 Simple method for preparing coralline strontium carbonate crystal Expired - Fee Related CN109179473B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113104879A (en) * 2021-05-07 2021-07-13 南昌航空大学 Method for preparing strontium fluoride crystal

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CN1699178A (en) * 2005-05-11 2005-11-23 重庆大学 Process for preparing high purity strontium carbonate
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CN104313055A (en) * 2014-09-25 2015-01-28 南京工业大学 Method for preparing strontium carbonate by microorganisms
CN105836779A (en) * 2016-03-28 2016-08-10 余国礼 Apparatus of converting celestite into strontium carbonate under cavitation effect
CN106927492A (en) * 2015-12-30 2017-07-07 吴礼秀 A kind of high-purity strontium salt preparation method
CN107381612A (en) * 2017-09-11 2017-11-24 西南科技大学 For the preparation method for the strontium carbonate for producing glass substrate
CN108203113A (en) * 2016-12-20 2018-06-26 青岛祥智电子技术有限公司 The production method of agricultural ammonium chloride and industrial sodium bicarbonate
CN108675335A (en) * 2018-09-03 2018-10-19 南昌航空大学 A kind of bionical method for preparing carbonic acid strontium crystal

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1699178A (en) * 2005-05-11 2005-11-23 重庆大学 Process for preparing high purity strontium carbonate
CN104016395A (en) * 2014-06-26 2014-09-03 中国科学院青海盐湖研究所 Strontium carbonate powder and preparation method thereof
CN104313055A (en) * 2014-09-25 2015-01-28 南京工业大学 Method for preparing strontium carbonate by microorganisms
CN106927492A (en) * 2015-12-30 2017-07-07 吴礼秀 A kind of high-purity strontium salt preparation method
CN105836779A (en) * 2016-03-28 2016-08-10 余国礼 Apparatus of converting celestite into strontium carbonate under cavitation effect
CN108203113A (en) * 2016-12-20 2018-06-26 青岛祥智电子技术有限公司 The production method of agricultural ammonium chloride and industrial sodium bicarbonate
CN107381612A (en) * 2017-09-11 2017-11-24 西南科技大学 For the preparation method for the strontium carbonate for producing glass substrate
CN108675335A (en) * 2018-09-03 2018-10-19 南昌航空大学 A kind of bionical method for preparing carbonic acid strontium crystal

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113104879A (en) * 2021-05-07 2021-07-13 南昌航空大学 Method for preparing strontium fluoride crystal

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