CN108910929A - A kind of preparation method of the micro-nano calcium carbonate for Pb In Exhausted Water removal - Google Patents
A kind of preparation method of the micro-nano calcium carbonate for Pb In Exhausted Water removal Download PDFInfo
- Publication number
- CN108910929A CN108910929A CN201810985770.4A CN201810985770A CN108910929A CN 108910929 A CN108910929 A CN 108910929A CN 201810985770 A CN201810985770 A CN 201810985770A CN 108910929 A CN108910929 A CN 108910929A
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- Prior art keywords
- micro
- calcium carbonate
- nano calcium
- preparation
- water removal
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Classifications
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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
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses a kind of preparation methods for the micro-nano calcium carbonate for Pb In Exhausted Water removal for belonging to field of inorganic nano material.Chemical additives are added in the calcium chloride solution of 0.01-0.5mol/L in the method, it is stirred at room temperature, reacts 1-2h, then the sodium carbonate liquor of comparable sodium is added in above-mentioned solution, at a temperature of 10-30 DEG C, precipitating is collected after stirring, reaction 0.5-24h, it dries after washing to get the micro-nano calcium carbonate.The micro-nano carbonic acid calcium grain diameter is evenly distributed, and possesses-NH2Active site has very high adsorption rate to the lead ion in waste water.
Description
Technical field
The invention belongs to field of inorganic nano material, in particular to a kind of micro-nano calcium carbonate for Pb In Exhausted Water removal
Preparation method.
Background technique
The heavy metal water pollution problems got worse has become the big threat for influencing human normal life, in recent years, suction
Attached isolation technics grows a lot in terms of the pollution control of heavy metal, especially lead ion, however, many adsorbents exist at
The low problem of this height, adsorption efficiency, this greatly limits the business applications of adsorbent for heavy metal.
Calcium carbonate is inorganic mineral material most cheap and harmless in nature, because it is with biggish dissolution
Degree promotes the precipitating transfer between calcium carbonate and ceruse, to improve its removal rate to heavy metal lead ion.But
That calcium carbonate haves the defects that time of equilibrium adsorption is too long, adsorption efficiency is too low again, cause its in water process application by
Resistance.
Researcher has carried out a large amount of effort and trial, has the calcium carbonate of special microstructure using chemical method design synthesis
With the calcium carbonate with hierarchical structure/organic composite hybrid material, with improve its adsorption efficiency and shorten its time of equilibrium adsorption,
Expand application prospect of the calcium carbonate in water process, but because the regulation of microstructure mainly passes through the various crystal form controls of addition
Agent, template synthesize in the solution, and experiment condition requires harsh, preparation process complexity.
Summary of the invention
It is special the purpose of the present invention is to provide a kind of preparation method of micro-nano calcium carbonate for Pb In Exhausted Water removal
Sign is that the method uses double decomposition synthetic method, is regulated and controled according to chemical additives, the concentration of reactant, reaction time micro-
The microstructure of nanometer calcium carbonate, specific preparation method include the following steps：
(1) chemical additives are added in the calcium chloride solution of 0.01-0.5mol/L, are stirred at room temperature, react after 1-2h
To solution A；
The chemical additives be a kind of macromolecular compound (being denoted as CH), be carboxymethyl chitosan, chitosan quaternary ammonium salt,
One of chitosan hydrochloride, chitosan lactate, glutamate, and quality is the 1-30% of sodium carbonate quality；
(2) sodium carbonate liquor for preparing 0.01-0.5mol/L concentration is clear solution B after being stirred at room temperature uniformly；
(3) B solution prepared by step (2) is added in the solution A of step (1) preparation, at a temperature of 10-30 DEG C, is stirred
It mixes, react collection precipitating after 0.5-24h, be dried in vacuo after washing to get micro-nano calcium carbonate is arrived.
The micro-nano calcium carbonate be rectangular layer stack structure, it is well dispersed, partial size be 0.5-5 μm, it is uniform in size can
It adjusts, possesses-NH2Active site, crystal phase are calcite crystal form.
The collection, mode of washing use centrifugal process, and drying mode is using vacuum drying.
Beneficial effects of the present invention are：Provide a kind of preparation side of micro-nano calcium carbonate for Pb In Exhausted Water removal
Method, the micro-nano calcium carbonate of this method preparation are stable calcite crystal form, and partial size is 0.5-5 μm, uniform in size adjustable, and are gathered around
There is-NH2Active site has high adsorption rate to heavy metal lead ion；Meanwhile the rectangular calcium carbonate of micro-nano stratiform of the invention
Preparation process is simple, and reaction condition is mild, low in cost.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure of micro-nano calcium carbonate prepared by embodiment 1；
Fig. 2 is scanning electron microscope (SEM) figure of micro-nano calcium carbonate prepared by embodiment 2；
Fig. 3 is scanning electron microscope (SEM) figure of micro-nano calcium carbonate prepared by embodiment 3；
Fig. 4 is scanning electron microscope (SEM) figure of micro-nano calcium carbonate prepared by embodiment 4；
Fig. 5 be the micro-nano calcium carbonate dosage of embodiment 1-4 preparation be 500mg/L, suction-operated 2h except lead effect picture.
Specific embodiment
The present invention provides a kind of preparation methods of micro-nano calcium carbonate for Pb In Exhausted Water removal, with reference to the accompanying drawing
The present invention is described further with embodiment.
Embodiment 1：
Accurately weigh 0.5550g CaCl2And be dissolved in the beaker equipped with 100mL distilled water, magnetic agitation is uniform
It is configured to the CaCl of 0.05mol/L2Solution；Accurately weigh 0.5300g Na2CO3And it is dissolved in equipped with 100mL distilled water
In beaker, magnetic agitation is uniformly configured to the Na of 0.05mol/L2CO3Solution；0.3g chitosan hydrochloride is accurately weighed in 10mL
The CaCl of 0.05mol/L2In solution, room temperature magnetic agitation 2h adds the Na of 10mL 0.05mol/L2CO3Solution, room temperature magnetic
Power is stirred to react 1h, and precipitating is collected in centrifuge separation, and precipitating distilled water and dehydrated alcohol centrifuge washing is true in 80 DEG C after for several times
Sky is dry to obtain the rectangular calcium carbonate powder of micro-nano stratiform for 24 hours, and the partial size of rectangular calcium carbonate is 1-2 μm, is accumulated by nano particle
It forms, possesses-NH2Active site, crystal phase are calcite crystal form.
Embodiment 2：
Accurately weigh 0.1110g CaCl2And be dissolved in the beaker equipped with 100mL distilled water, magnetic agitation is uniform
It is configured to the CaCl of 0.01mol/L2Solution；Accurately weigh 0.1060g Na2CO3And it is dissolved in equipped with 100mL distilled water
In beaker, magnetic agitation is uniformly configured to the Na of 0.01mol/L2CO3Solution；0.3g chitosan hydrochloride is accurately weighed in 10mL
The CaCl of 0.01mol/L2In solution, room temperature magnetic agitation 2h adds the Na of 10mL 0.01mol/L2CO3Solution, room temperature magnetic
Power is stirred to react 1h, and precipitating is collected in centrifuge separation, and precipitating distilled water and dehydrated alcohol centrifuge washing is true in 80 DEG C after for several times
Sky drying obtains micro-nano calcium carbonate powder for 24 hours, and grain shape is irregular, and for partial size less than 1 μm, crystal phase is calcite crystal form.
Embodiment 3：
Accurately weigh 0.5550g CaCl2And be dissolved in the beaker equipped with 100mL distilled water, magnetic agitation is uniform
It is configured to the CaCl of 0.05mol/L2Solution；Accurately weigh 0.5300g Na2CO3And it is dissolved in equipped with 100mL distilled water
In beaker, magnetic agitation is uniformly configured to the Na of 0.05mol/L2CO3Solution；0.1g chitosan hydrochloride is accurately weighed in 10mL
The CaCl of 0.05mol/L2In solution, room temperature magnetic agitation 2h adds the Na of 10mL 0.05mol/L2CO3Solution, room temperature magnetic
Power is stirred to react 1h, and precipitating is collected in centrifuge separation, and precipitating distilled water and dehydrated alcohol centrifuge washing is true in 80 DEG C after for several times
Sky is dry to obtain ym square calcium carbonate powder for 24 hours, and partial size is 2-5 μm, and crystal phase is calcite crystal form.
Embodiment 4：
Accurately weigh 0.5550g CaCl2And be dissolved in the beaker equipped with 100mL distilled water, magnetic agitation is uniform
It is configured to the CaCl of 0.05mol/L2Solution；Accurately weigh 0.5300g Na2CO3And it is dissolved in equipped with 100mL distilled water
In beaker, magnetic agitation is uniformly configured to the Na of 0.05mol/L2CO3Solution；CH is not added, measures 10mL 0.05mol/L's
CaCl2Under room temperature magnetic agitation, the Na of 10mL 0.05mol/L is added in solution2CO3Solution, room temperature magnetic agitation react 1h, from
The heart separates and collects precipitating, and precipitating distilled water and dehydrated alcohol centrifuge washing are obtained not after for several times in 80 DEG C of vacuum drying for 24 hours
Regular diamond shape calcium carbonate, partial size are 5 μm, and crystal phase is calcite crystal form.
Claims (4)
1. a kind of preparation method of the micro-nano calcium carbonate for Pb In Exhausted Water removal, which is characterized in that include the following steps：
(1) chemical additives are added in the calcium chloride solution of 0.01-0.5mol/L, be stirred at room temperature, react obtain after 1-2h it is molten
Liquid A；
(2) sodium carbonate liquor for preparing 0.01-0.5mol/L, obtains clear solution B after being stirred at room temperature uniformly；
(3) B solution prepared by step (2) is added in the solution A of step (1) preparation, at a temperature of 10-30 DEG C, stirs, is anti-
Precipitating is collected after answering 0.5-24h, vacuum drying obtains micro-nano calcium carbonate after washing.
2. a kind of preparation method of micro-nano calcium carbonate for Pb In Exhausted Water removal according to claim 1, feature
It is, the micro-nano calcium carbonate is rectangular stacked in layers structure, and uniform in size, partial size is adjustable, and particle size range is 0.5-5 μm,
Possess-NH2 active site, crystal phase is calcite crystal form.
3. a kind of preparation method of micro-nano calcium carbonate for Pb In Exhausted Water removal according to claim 1, feature
It is, the chemical additives are carboxymethyl chitosan, chitosan quaternary ammonium salt, chitosan hydrochloride, chitosan lactate, shell are poly-
One of sugared glutamate, and quality is the 1-30% of sodium carbonate quality.
4. a kind of preparation method of micro-nano calcium carbonate for Pb In Exhausted Water removal according to claim 1, feature
It is, the collection precipitating is collected by the way of centrifugation.
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| CN201810985770.4A CN108910929A (en) | 2018-08-28 | 2018-08-28 | A kind of preparation method of the micro-nano calcium carbonate for Pb In Exhausted Water removal |
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| CN201810985770.4A CN108910929A (en) | 2018-08-28 | 2018-08-28 | A kind of preparation method of the micro-nano calcium carbonate for Pb In Exhausted Water removal |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111921486A (en) * | 2020-07-09 | 2020-11-13 | 内江师范学院 | Nano calcium carbonate and preparation method and application thereof |
| CN112408450A (en) * | 2020-11-27 | 2021-02-26 | 广西华纳新材料科技有限公司 | Preparation method of cubic-like nano calcium carbonate |
| CN113976084A (en) * | 2021-11-03 | 2022-01-28 | 玉林师范学院 | Used for adsorbing Pb in water2+Composite adsorbent and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101249977A (en) * | 2008-03-07 | 2008-08-27 | 中国科学院上海硅酸盐研究所 | Method for preparing different crystal system calcium carbonate by using chitosan |
-
2018
- 2018-08-28 CN CN201810985770.4A patent/CN108910929A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101249977A (en) * | 2008-03-07 | 2008-08-27 | 中国科学院上海硅酸盐研究所 | Method for preparing different crystal system calcium carbonate by using chitosan |
Non-Patent Citations (2)
| Title |
|---|
| 赵东辉: "基于生物矿化的不同晶型与形貌碳酸钙的研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
| 郭厚勇: "Pb~(2+)/有机基质协同调控碳酸钙结晶行为研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111921486A (en) * | 2020-07-09 | 2020-11-13 | 内江师范学院 | Nano calcium carbonate and preparation method and application thereof |
| CN112408450A (en) * | 2020-11-27 | 2021-02-26 | 广西华纳新材料科技有限公司 | Preparation method of cubic-like nano calcium carbonate |
| WO2022110127A1 (en) * | 2020-11-27 | 2022-06-02 | 广西华纳新材料科技有限公司 | Method for preparing cube-like nano calcium carbonate |
| CN113976084A (en) * | 2021-11-03 | 2022-01-28 | 玉林师范学院 | Used for adsorbing Pb in water2+Composite adsorbent and preparation method thereof |
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