CN109592702A - A kind of nano-scale carbon hydrochlorate and preparation method thereof - Google Patents

A kind of nano-scale carbon hydrochlorate and preparation method thereof Download PDF

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CN109592702A
CN109592702A CN201811642399.8A CN201811642399A CN109592702A CN 109592702 A CN109592702 A CN 109592702A CN 201811642399 A CN201811642399 A CN 201811642399A CN 109592702 A CN109592702 A CN 109592702A
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gas
nano
carbonate
liquid
scale carbon
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廖爱芳
戴书云
刘杰
李甜
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Fujian Cisco Electronic Material Ltd By Share Ltd
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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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00Lithium compounds
    • C01D15/08Carbonates; Bicarbonates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The present invention provides a kind of nano-scale carbon hydrochlorate and preparation method thereof, wherein the nano-scale carbon hydrochlorate preparation method, and step includes: S1, water soluble alkali and solvent be added in dissolution vessel, high-speed stirred dissolution;S2, lysate obtained in S1 is delivered in injection gas-liquid synthetic reaction device, while is filled with carbon dioxide gas to injection gas-liquid synthetic reaction device and is synthesized, 0-80 DEG C of synthesis process temperature;S3, carbonate gas and liquid mixture made from S2 is delivered in gas-liquid separation device, gas-liquid separation, will be reacted after remaining carbon dioxide gas detaches, remaining carbonate slurry;S4, the carbonate slurry obtained in S3 is separated by solid-liquid separation, nano-scale carbon hydrochlorate is made through drying, sieving in decorating film;Wherein, water soluble alkali can generate carbonate with carbon dioxide gas precursor reactant.That it is an object of that present invention to provide techniques is relatively easy, product cut size is uniform, impurity content is low, environmentally friendly, low-cost nano-scale carbon hydrochlorate preparation method.

Description

A kind of nano-scale carbon hydrochlorate and preparation method thereof
Technical field
The present invention relates to the preparation process of carbonate, in particular to a kind of nano-scale carbon hydrochlorate and preparation method thereof.
Background technique
Carbonate powder is widely applied raw material in electronic industrial products, it can be applied to electron ceramic material, electronics In magnetic material, electronic ceramics capacitor and optical grade specific glass.With the fast development of electronics industry, market is to nano-scale carbon The demand of hydrochlorate is increasing, meanwhile, the physical and chemical index of carbonate is required also higher and higher.Do not require nothing more than chemical purity Height, impurity is few, but also requires that particle morphology is good, narrow particle size distribution.
The main method of industrial production carbonate is using soluble chloride and carbonate in conventional reaction kettle at present The middle precipitation method reacted.Such method has many advantages, such as that raw material is easy to get, simple process.But in actual production, such method Also highlight shortcoming, i.e., nano-carbonate crystal particle diameter can not be controlled effectively, unstable quality, product impurity mostly etc.. In addition, such method generates the by-products such as hydrogen sulfide and ammonium chloride during the preparation process, pollution on the environment is big, correspondingly The environmental protection for needing to put into is at high cost;And easily these by-products of remaining, these by-products are miscellaneous in nano-carbonate particle powder Matter can impact characteristic of the nano-carbonate in electronic material application.So the nano-carbonate of such method preparation is not It is suitable for the utilization of electronic product.How to improve nano-scale carbon hydrochlorate preparation method, achieves effective control carbonate crystal grain Diameter shape, reduce product impurity, without hydrogen sulfide and ammonium chloride by-product generation be this field urgent problem to be solved.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of nano-scale carbon hydrochlorate preparation method, includes the following steps:
S1, water soluble alkali and solvent are added in dissolution vessel, high-speed stirred dissolution is spare;
S2, lysate obtained in S1 is delivered in injection gas-liquid synthetic reaction device, while is synthesized to injection gas-liquid Reaction unit is filled with carbon dioxide gas and is synthesized, 0-80 DEG C of synthesis process temperature, and carbonate gas and liquid mixture is made;Its In, water soluble alkali can generate carbonate with carbon dioxide gas precursor reactant;
S3, carbonate gas and liquid mixture obtained in S2 injection gas-liquid synthetic reaction device is delivered to gas-liquid separation device In, gas-liquid separation will react after remaining carbon dioxide gas detaches, remaining carbonate slurry;
S4, the carbonate slurry obtained in S3 is separated by solid-liquid separation, nanoscale is made by dry, sieving in decorating film Carbonate.
Further, S1 step is that water soluble alkali, Grain growth inhibitor and solvent are added in dissolution vessel, high speed Stirring and dissolving, it is spare;
Grain growth inhibitor is one or more of carboxylic acid and carboxylate;Grain growth inhibitor content is solubility The 0-15% of alkali molar content.
Further, the control of the ratio between flow quantity and carbon dioxide gas flow is dissolved in S2 step in 1:1-1:500.
Further, decorating film is dry in electric heating constant-temperature blowing drying box in S4 step, and 80-200 DEG C of temperature, dry 2- 10h。
Further, the carbon dioxide gas detached in S3 step is pressurized, it is cold dry, it re-fills to injection gas-liquid synthesis Reaction is participated in reaction unit.
Further, the carbonate gas and liquid mixture in S3 step, which is delivered to before gas-liquid separation device, first carries out pH detection, The carbonate gas and liquid mixture that pH value is 4-12 is delivered to gas-liquid separation device again.
Further, the water soluble alkali is one or more of hydroxide and alkali salt;The solvent is solvable alkali The solvent of salt.
Further, the hydroxide is lithium hydroxide, barium hydroxide, strontium hydroxide or calcium hydroxide.
Further, the alkali salt is lithium salts, barium salt, strontium salt or calcium salt.
The present invention also provides nano-scale carbon hydrochlorates made from a kind of above-mentioned nano-scale carbon hydrochlorate preparation method.
Compared with the prior art, the present invention has the advantage that
(1) present invention firstly discovers that preparing carbonate by spraying gas-liquid synthetic reaction device, obtained carbonate can Nanoscale is reached, and can effectively control the particle size of carbonate, quality is stablized, and can be used as the dedicated material of electronic product Material.The carbonate powder that this method is prepared, distribution of particles D50:100-200nm, specific surface area (BET) can reach 10m2/ g with On.
(2) water soluble alkali of the present invention is dissolved into lysate in injection gas-liquid synthetic reaction device in atomized water spray, expands Response area, sufficiently reacts with carbon dioxide gas and generates carbonate gas and liquid mixture, and reaction product does not include hydrogen sulfide and chlorine Change the by-products such as ammonium, not can cause environmental pollution.
(3) it is able to suppress under the action of Grain growth inhibitor in the present invention by addition Grain growth inhibitor Grain growth manufactures specific surface area in 10-70m2The needle-shaped carbonate powder of/g.
(4) carbon dioxide gas can re-enter into gas-liquid reaction apparatus again by pressurization, Leng Ganhou in the present invention Synthetic reaction is participated in, realizing carbon dioxide gas extra after synthesizing in reaction system can be recycled, and reach energy saving purpose. And the yield that reaction system can be needed according to synthesis enables gas and liquid spraying by adjusting the flow and pressure of gas-liquid It is sufficiently reacted in gas-liquid synthetic reaction device, gas-liquid synthesis ratio can be kept away by constant pressure, current constant control within the unit time Exempt from material secondary response;Again by the carbonate gas and liquid mixture pH value of detection synthesis, the product needed guarantees synthesis knot Fruit real time monitoring.
In conclusion nano-scale carbon hydrochlorate preparation method provided by the invention is able to solve the deficiencies in the prior art, and its Process flow is relatively easy, product cut size is uniform, impurity content is low, environmental protection is low in cost.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention, Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
It should be noted that the examples of the embodiments are intended to be used to explain the present invention, and should not be understood as to the present invention Limitation, in the examples where no specific technique or condition is specified, according to the literature in the art described technology or conditions or Person carries out according to product description, reagents or instruments used without specified manufacturer, and being can be by the normal of commercially available acquisition Advise product.
The dissolution vessel that embodiment uses is insulated and stirred formula dissolving tank;Injection gas-liquid synthetic reaction device is venturi gas Liquid mixer;This is not meant to that dissolution vessel and injection gas-liquid synthetic reaction device can only be using above-mentioned apparatus, all uses Other devices with above-mentioned apparatus identical functions carry out carbonate preparation and also each fall within protection scope of the present invention.
The raw material explanation that embodiment uses:
Soluble barium source: barium hydroxide (purity requirement >=95% or more, impurity Sr content≤0.1%).
Soluble lithium source: lithium hydroxide (purity requirement >=95% or more).
Soluble calcium source: calcium hydroxide (purity requirement >=95% or more).
Soluble barium source: strontium hydroxide (purity requirement >=95% or more).
Solvent: water.
Carbon dioxide gas: purity is more than 99.9%, and in steel cylinder carbon dioxide gas pressure 0.5-6.5 megapascal it Between.
Embodiment needs to pre-process dissolution vessel and gas-liquid separation device before implementing, in which:
The pretreatment of dissolution vessel: being passed through nitrogen protection gas in advance, and air in container is caught up with to the greatest extent, dioxy in air is avoided Change carbon and water soluble alkali reaction generate carbonate, and (the nitrogen protection gas being passed through is recycled after starting stirring, is transported to storage Tank recycles).
The pretreatment of gas-liquid separation device: it is carried out being evacuated to negative pressure with vacuum pump, then is filled with into gas-liquid separation device Carbon dioxide gas, it is closed.
The preparation method of 1-7 of the embodiment of the present invention includes the following steps:
(1) lysate is prepared:
By barium hydroxide or lithium hydroxide or calcium hydroxide or strontium hydroxide, Grain growth inhibitor, specific temperature Water be added in pretreated dissolution vessel, keep water temperature, high-speed stirred is made into the alkali lysate of certain concentration;
(2) gas-liquid synthetic reaction:
The alkali lysate of above-mentioned certain concentration is evacuated in injection gas-liquid synthetic reaction device with peristaltic pump, controls titanium dioxide Carbon gas and lysate flow-rate ratio are filled with carbon dioxide gas to injection gas-liquid synthetic reaction device and are synthesized, carbonic acid is made Salt gas and liquid mixture.
(3) gas-liquid separation:
It sprays and is filled on the charging line between gas-liquid synthetic reaction device and closed gas-liquid separation device equipped with pH detection Electrically-controlled valve is set and is equipped with, pH detection device is used to detect the pH value of liquid in injection gas-liquid synthetic reaction device end pipe road, works as inspection It measures carbonate gas and liquid mixture pH value obtained above and reaches 6-9, carbonate gas and liquid mixture is delivered to closed gas-liquid In separator, gas-liquid separation will react remaining carbon dioxide with air compressor and be extracted into gas storage in gas-liquid separation device In slot, gas-liquid separation device pressure is made to be maintained at micro-vacuum state, continued after to be synthesized by dioxy in gas-liquid separation device Change carbon gas to be evacuated in gas reservoir, until pressure is negative pressure (- 0.02MPa);Remaining carbonic acid salt slurry in gas-liquid separation device Liquid is from bottom row pressure discharging.
The carbon dioxide gas in gas reservoir is extracted into after cooling driers remove steam, continues cycling through utilization.
(4) prepared by nano-scale carbon silicate powder:
The carbonate slurry of above-mentioned acquisition is filtered, carbonate muffin and water are obtained;Carbonate muffin is dried with 100 DEG C It is dried in case 3 hours, then is sieved to obtain needle-shaped carbonate powder with 120 mesh screens.
The water filtered out is recycled, and can be re-used as solvent use, be reached and recycle effect.
It should be noted that in calcium carbonate preparation process, since calcium hydroxide is to be slightly soluble in water, thus spray gas-liquid synthesis Reactant and product in reaction unit can be re-delivered in injection gas-liquid synthetic reaction device and carry out multiple gas liquid reaction.
The present invention provide embodiment 1-7 as shown in table 1 technological parameter (include: the temperature of water in lysate preparation steps, The concentration of alkali in the additive amount of Grain growth inhibitor, alkali lysate;Alkali lysate and dioxy in gas-liquid synthetic reaction step Change carbon flow ratio;The pH value detected in gas-liquid separation step):
Table 1
Comparative example 1
Barium hydroxide and 45 DEG C of water are added in the reaction kettle of included stirring, start agitating device, carries out high speed Stirring obtains barium hydroxide lysate to being completely dissolved, and wherein the molar concentration of barium hydroxide is 0.25;Two are passed through toward reaction kettle Carbon oxide gas, carbon dioxide flow and solution ratio are 50:1, and duration of ventilation 30min detects the pH of product in reaction kettle Value reaches 6.4, exhaust pressure relief (CO2It is discharged with exhausting system), obtain barium carbonate slurries;Barium carbonate slurries are arranged from reactor bottom Out, it is filtered, obtains barium carbonate muffin and water;Barium carbonate muffin is placed on drying 3 hours in 100 DEG C of baking ovens, uses after dry The sieving of 120 mesh screens, obtains barium carbonate powder.
Comparative example 2
Purification barium chloride is dissolved in deionized water, is stirred evenly, obtained solution A, barium chloride concentration is 0.5M, spare; Prepared calcium carbonate hydrogen ammonium is dissolved in deionized water, is stirred evenly, obtained solution B, ammonium bicarbonate concentration 0.5M, spare;By solution B It is added in reaction kettle, adds solution A, be stirred to react, reaction temperature room temperature, reaction time 1h;From reaction kettle bottom Barium carbonate slurries are discharged in portion, and barium carbonate slurries are filtered, barium carbonate muffin and water are obtained;Barium carbonate muffin deionized water It is cleaned, removes removing chloride, barium carbonate muffin is placed 100 DEG C of dryings 3 in an oven by chloride ion content requirement≤200ppm Hour, it is sieved after dry with 120 mesh screens.Obtain barium carbonate powder.
Comparative example 3
Commercially available carbonic acid powder for lithium
Comparative example 4
Commercially available calcium carbonate powder
Comparative example 5
Commercially available strontium carbonate powder
Carbonate powder progressive made from embodiment 1-7 and comparative example 1-5 can be detected, detection method is as follows:
Barium carbonate assay: GB/T 654-2011;
Lithium carbonate assay: GB/T 11075-2003;
Calcium carbonate content measurement: GB/T 19281-2003
Strontium carbonate contents measurement: HG/T 4508-2013
Determination of Specific Surface Area: it is measured by Bi Aode Kubo 1108;
Size distribution measurement: it is measured by American-European gram of laser particle analyzer TopSize;
Grain shape measurement: it is measured by Hitachi's S-3 400N scanning electron microscope (SEM);
Its testing result is as shown in table 2:
Table 2
As seen in Table 2, compared with comparative example 1-2, its surface area (BET) of the barium carbonate of embodiment can reach embodiment 1-4 To 10m2/ g or more, highest can be 61.93, especially compared with comparative example 2 (traditional precipitation method prepare barium carbonate), pass through this Barium carbonate specific surface area obtained by the preparation method of invention nanoscale barium carbonate has promotion outstanding;In addition, embodiment 1-4 Barium carbonate size distribution D50 obtained is much smaller than comparative example 1-2, it was demonstrated that preparation method through the invention at 0.1-0.2 μm Nanoscale barium carbonate can be made.In addition, as known from Table 2, lithium carbonate, calcium carbonate, the strontium carbonate of embodiment 5-7 preparation pass through this The nanoscale product that the preparation method of invention obtains is above existing commercial product.Nanoscale can be prepared through the invention by demonstrating Carbonate.

Claims (10)

1. a kind of nano-scale carbon hydrochlorate preparation method, which comprises the steps of:
S1, water soluble alkali and solvent are added in dissolution vessel, high-speed stirred dissolution is spare;
S2, by lysate obtained in S1 be delivered to injection gas-liquid synthetic reaction device in, while to injection gas-liquid synthetic reaction Device is filled with carbon dioxide gas and is synthesized, 0-80 DEG C of synthesis process temperature, and carbonate gas and liquid mixture is made;Wherein, may be used Dissolubility alkali can generate carbonate with carbon dioxide gas precursor reactant;
S3, carbonate gas and liquid mixture obtained in S2 injection gas-liquid synthetic reaction device is delivered in gas-liquid separation device, Gas-liquid separation will react after remaining carbon dioxide gas detaches, remaining carbonate slurry;
S4, the carbonate slurry obtained in S3 is separated by solid-liquid separation, nanoscale carbonic acid is made by dry, sieving in decorating film Salt.
2. nano-scale carbon hydrochlorate preparation method according to claim 1, which is characterized in that S1 step be by water soluble alkali, Grain growth inhibitor and solvent are added in dissolution vessel, high-speed stirred dissolution, spare;
Grain growth inhibitor is one or more of carboxylic acid and carboxylate;Grain growth inhibitor content rubs for water soluble alkali The 0-15% of your content.
3. nano-scale carbon hydrochlorate preparation method according to claim 1 or 2, which is characterized in that dissolve liquid stream in S2 step The control of the ratio between amount and carbon dioxide gas flow is in 1:1-1:500.
4. nano-scale carbon hydrochlorate preparation method according to claim 1 or 2, which is characterized in that decorating film exists in S4 step It is dry in electric heating constant-temperature blowing drying box, 80-200 DEG C of temperature, dry 2-10h.
5. nano-scale carbon hydrochlorate preparation method according to claim 1 or 2, which is characterized in that by what is detached in S3 step Carbon dioxide gas pressurization, it is cold dry, it re-fills and participates in reaction into injection gas-liquid synthetic reaction device.
6. nano-scale carbon hydrochlorate preparation method according to claim 1 or 2, which is characterized in that the carbonate in S3 step Gas and liquid mixture, which is delivered to before gas-liquid separation device, first carries out pH detection, then the carbonate gas and liquid mixture that pH value is 4-12 is defeated It send to gas-liquid separation device.
7. nano-scale carbon hydrochlorate preparation method according to claim 1 or 2, which is characterized in that the water soluble alkali is hydrogen One or more of oxide and alkali salt;The solvent is the solvent of solvable alkali salt.
8. nano-scale carbon hydrochlorate preparation method according to claim 7, which is characterized in that the hydroxide is hydroxide Lithium, barium hydroxide, strontium hydroxide or calcium hydroxide.
9. nano-scale carbon hydrochlorate preparation method according to claim 7, which is characterized in that the alkali salt be lithium salts, barium salt, Strontium salt or calcium salt.
10. a kind of using nano-scale carbon hydrochlorate made from the described in any item nano-scale carbon hydrochlorate preparation methods of claim 1-9.
CN201811642399.8A 2018-12-29 2018-12-29 A kind of nano-scale carbon hydrochlorate and preparation method thereof Pending CN109592702A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115180639A (en) * 2022-08-08 2022-10-14 湖南五创循环科技有限公司 Method for purifying lithium sulfate solution to remove impurities and producing lithium carbonate

Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW200702303A (en) * 2005-07-01 2007-01-16 Hon Hai Prec Ind Co Ltd Method to prepare nanoparticles
CN101428838A (en) * 2007-11-05 2009-05-13 日本化学工业株式会社 Barium carbonate particle powder, production method thereof, and production method of perovskite barium titanate
CN202164134U (en) * 2011-03-15 2012-03-14 池州凯尔特纳米科技有限公司 Energy-saving carbonization reactor for producing nanometer calcium carbonate
CN102674425A (en) * 2012-05-19 2012-09-19 祁阳建明化工有限责任公司 Production technique of nano calcium carbonate by normal temperature method
CN103011225A (en) * 2012-12-07 2013-04-03 池州凯尔特纳米科技有限公司 Carbonization kettle and method for preparing spherical calcium carbonate by using carbonization kettle
CN202953833U (en) * 2012-11-08 2013-05-29 广西华纳新材料科技有限公司 Continuous preparation device of nano calcium carbonate
EP2796412A1 (en) * 2013-04-24 2014-10-29 Università Del Salento - Dipartimento Di Ingegneria Dell'Innovazione Synthesis of nano-sized CaCO3 particles by spray dryer
CN105502462A (en) * 2015-12-22 2016-04-20 东莞理工学院 Device and method for preparing nanometer calcium carbonate through micropore pipe
CN105800659A (en) * 2016-05-24 2016-07-27 广西平南县恒祥钙业有限公司 Spraying reactor and carbonization reaction system of nano calcium carbonate
CN205676168U (en) * 2016-05-24 2016-11-09 广西平南县恒祥钙业有限公司 A kind of carburizing reagent system of injection reactor and nano-calcium carbonate
CN206886698U (en) * 2017-06-07 2018-01-16 江西九峰纳米钙有限公司 One kind production nano-calcium carbonate rotating-spray carbonizing plant
CN107601542A (en) * 2017-09-30 2018-01-19 广西华洋矿源材料有限公司 A kind of preparation method of nano-calcium carbonate
CN207330389U (en) * 2017-09-14 2018-05-08 常山县祥鑫纳米科技有限公司 One kind production nano-calcium carbonate rotating-spray carbonizing plant

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW200702303A (en) * 2005-07-01 2007-01-16 Hon Hai Prec Ind Co Ltd Method to prepare nanoparticles
CN101428838A (en) * 2007-11-05 2009-05-13 日本化学工业株式会社 Barium carbonate particle powder, production method thereof, and production method of perovskite barium titanate
CN202164134U (en) * 2011-03-15 2012-03-14 池州凯尔特纳米科技有限公司 Energy-saving carbonization reactor for producing nanometer calcium carbonate
CN102674425A (en) * 2012-05-19 2012-09-19 祁阳建明化工有限责任公司 Production technique of nano calcium carbonate by normal temperature method
CN202953833U (en) * 2012-11-08 2013-05-29 广西华纳新材料科技有限公司 Continuous preparation device of nano calcium carbonate
CN103011225A (en) * 2012-12-07 2013-04-03 池州凯尔特纳米科技有限公司 Carbonization kettle and method for preparing spherical calcium carbonate by using carbonization kettle
EP2796412A1 (en) * 2013-04-24 2014-10-29 Università Del Salento - Dipartimento Di Ingegneria Dell'Innovazione Synthesis of nano-sized CaCO3 particles by spray dryer
CN105502462A (en) * 2015-12-22 2016-04-20 东莞理工学院 Device and method for preparing nanometer calcium carbonate through micropore pipe
CN105800659A (en) * 2016-05-24 2016-07-27 广西平南县恒祥钙业有限公司 Spraying reactor and carbonization reaction system of nano calcium carbonate
CN205676168U (en) * 2016-05-24 2016-11-09 广西平南县恒祥钙业有限公司 A kind of carburizing reagent system of injection reactor and nano-calcium carbonate
CN206886698U (en) * 2017-06-07 2018-01-16 江西九峰纳米钙有限公司 One kind production nano-calcium carbonate rotating-spray carbonizing plant
CN207330389U (en) * 2017-09-14 2018-05-08 常山县祥鑫纳米科技有限公司 One kind production nano-calcium carbonate rotating-spray carbonizing plant
CN107601542A (en) * 2017-09-30 2018-01-19 广西华洋矿源材料有限公司 A kind of preparation method of nano-calcium carbonate

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115180639A (en) * 2022-08-08 2022-10-14 湖南五创循环科技有限公司 Method for purifying lithium sulfate solution to remove impurities and producing lithium carbonate
CN115180639B (en) * 2022-08-08 2023-12-15 湖南五创循环科技有限公司 Method for purifying and removing impurities from lithium sulfate solution and producing lithium carbonate

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Application publication date: 20190409