CN1301216C - Method for preparing calcium carbonate nano wire - Google Patents
Method for preparing calcium carbonate nano wire Download PDFInfo
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- CN1301216C CN1301216C CNB2005100115538A CN200510011553A CN1301216C CN 1301216 C CN1301216 C CN 1301216C CN B2005100115538 A CNB2005100115538 A CN B2005100115538A CN 200510011553 A CN200510011553 A CN 200510011553A CN 1301216 C CN1301216 C CN 1301216C
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- calcium carbonate
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Abstract
The present invention provides a method for preparing nanometer calcium carbonate wires, and belongs to the technical field of carbonate. The present invention utilizes a sol-gel pyrolyzing method to prepare nanometer calcium carbonate wires. Firstly, calcic intermediate compounds, namely nanometer wires, are prepared with a sol-gel method, and then the intermediate compounds are treated in a thermal mode to obtain nanometer calcium carbonate wires. Surface active agents, namely hexadecyl trimethyl ammonium bromide, are added in the reaction process, and are favorable for preventing the nanometer wires from aggregating, wherein added citric acid performs the critical function of a template and induces the intermediate compounds to linearly grow. The temperature is slowly raised during thermal treatment which keeps the shape of the intermediate compounds and removes redundant organic ingredients. The present invention has the advantages of simple and convenient process operation, and uniform grain size distribution and good dispersancy of the prepared nanometer wires.
Description
Technical field
The invention belongs to the carbonate technical field, a kind of method for preparing calcium carbonate nano wire particularly is provided, adopt little, the finely dispersed calcium carbonate nano wire of calcium carbonate powder material (chemical reagent or natural mineral) preparation particle diameter.
Background technology
Lime carbonate is widely used in many fields such as papermaking, plastics, paint, toothpaste, medicine as a kind of important chemical material.Calcium carbonate nano wire is compared with the calcium carbonate nano particulate has following characteristics: oil number is big and the nonferromagnetic substance of appropriateness arranged; Be used for the pollution that the thermoinduction paint can prevent hotness oil, whiteness height, good weatherability; Being used for thermoinduction paper, to have a noise little, need not the printing ink image-developing liquor; Add the induction paper of nano-calcium carbonate, can improve whiteness, opacity, smoothness; Multiple use such as slowly emit and await exploitation but also have absorption, desorption, grinding effect, fragrance protectiveness.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing calcium carbonate nano wire, solved the spherulitic nano material as physicals defectives such as compound undercapacity, lacking toughnesss.
The present invention utilizes the sol-gel thermal decomposition method to prepare calcium carbonate nano wire.At first sol-gel method prepares the calcic intermediate, and this intermediate also is a nano wire; Then this intermediate thermal treatment is promptly obtained calcium carbonate nano wire.In reaction process, add the tensio-active agent cetyl trimethylammonium bromide, help preventing the reunion of nano wire.Wherein the adding of citric acid plays critical template action, induces the linear growth of intermediate; The temperature temperature rise rate is wanted slowly during thermal treatment, and thermal treatment has kept intermediate to get pattern, has removed unnecessary organic composition.
Its preparation technology is specific as follows:
1. be among 0.2～2mol/L in the acetic acid water solution volumetric molar concentration, add lime carbonate 1～10g/100ml solution, in 30～80 ℃ magnetic stirring apparatus, refluxed 1～3 hour.
2. in the mixed solution that step 1 obtains, add citric acid 1～10g/100ml solution, continue to reflux 12～48 hours, obtain milk shape colloid.
3. add the tensio-active agent cetyl trimethylammonium bromide in the milk shape colloid that step 2 obtains, 0.1～1g/100ml solution continues to reflux 12～24 hours.Add tensio-active agent and more help preventing the intermediate that obtains in the later stage process and the reunion of nano wire.
4. the milk shape colloid that step 2 or step 3 are obtained filters, and washes with water 3～5 times, collects filter residue, and drying promptly is the calcic intermediate, and transmission electron microscope observing also is a nano wire.
5. the calcic intermediate thermal treatment that step 4 is obtained, temperature 400-600 ℃, soaking time 1-3 hour, temperature rise rate was wanted slowly to be 0.5-5 ℃/min, is obtained calcium carbonate nano wire at last.
The invention has the advantages that: process implementing is simple and convenient, the nano wire even particle size distribution of preparation, good dispersity; Possesses the not available optical property of spherulitic nano particle simultaneously.
Embodiment
Embodiment 1:
1. with 2g CaCO
3Be dissolved in the 0.5mol/L acetic acid solution of 100ml 60 ℃ of constant temperature magnetic agitation 2 hours.
2. add the 4g citric acid in above-mentioned gained settled solution, continued 60 ℃ of constant temperature magnetic agitation 12 hours, settled solution becomes oyster white milk shape colloid gradually in the whipping process.
3. filter above-mentioned oyster white milk shape colloid, use deionized water, absolute ethanol washing 3 times, 50 ℃ of oven dry, obtaining white powder is that wire contains the Ca intermediate.
4. intermediate slowly is warming up to 450 ℃, 5 ℃/min of temperature rise rate is incubated 2 hours, naturally cooling, and obtaining white powder is calcium carbonate nano wire.
Embodiment 2:
1. in the 0.45mol/L acetic acid solution, add 4g lime carbonate, 60 ℃ were refluxed 2 hours.
2. in above-mentioned mixing solutions, add citric acid 4g, continue to reflux 24 hours, become cotton-shaped liquid.
3. add cetyl trimethylammonium bromide 3g again, continue to reflux 24 hours, become milk sap, use deionized water, absolute ethanol washing 4 times, 50 ℃ of oven dry.
4.450 ℃ thermal treatment 2 hours is incubated 2 hours, obtains calcium carbonate nano wire.
Claims (1)
1, a kind of method for preparing calcium carbonate nano wire is characterized in that: concrete technology is:
A, be in the acetic acid water solution of 0.2～2mol/L, add lime carbonate 1～10g/100ml solution, in 30～80 ℃ magnetic stirring apparatus, refluxed 1～3 hour in volumetric molar concentration;
B, in the mixed solution that step a obtains, add citric acid 1～10g/100ml solution, continue backflow 12-48 hour, obtain milk shape colloid;
C, in the milk shape colloid that step b obtains, add the cetyl trimethylammonium bromide solution of tensio-active agent 0.1～1g/100ml, continue to reflux 12～24 hours;
D, the milk shape colloid that step b or step c are obtained filter, and wash with water 3～5 times, collect filter residue, and drying promptly is the calcic intermediate, and transmission electron microscope observing also is a nano wire;
E, the calcic intermediate thermal treatment that steps d is obtained, 400～600 ℃ of temperature, soaking time 1～3 hour, temperature rise rate is 0.5～5 ℃/minute, obtains calcium carbonate nano wire at last.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100115538A CN1301216C (en) | 2005-04-11 | 2005-04-11 | Method for preparing calcium carbonate nano wire |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100115538A CN1301216C (en) | 2005-04-11 | 2005-04-11 | Method for preparing calcium carbonate nano wire |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1699177A CN1699177A (en) | 2005-11-23 |
| CN1301216C true CN1301216C (en) | 2007-02-21 |
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ID=35475462
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100115538A Expired - Fee Related CN1301216C (en) | 2005-04-11 | 2005-04-11 | Method for preparing calcium carbonate nano wire |
Country Status (1)
| Country | Link |
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| CN (1) | CN1301216C (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05308956A (en) * | 1991-03-19 | 1993-11-22 | Mitsubishi Heavy Ind Ltd | Preservation of nitric acid bacteria and method for restoration |
| JPH11349321A (en) * | 1998-06-05 | 1999-12-21 | Osaka Gas Co Ltd | Production of functional silicon material |
| US6376449B2 (en) * | 1993-03-27 | 2002-04-23 | Novozymes A/S | Acidic cleaning composition comprising an acidic protease I |
| WO2003004414A1 (en) * | 2001-07-04 | 2003-01-16 | Solvay (Société Anonyme) | Method for obtaining precipitated calcium carbonate particles of nanometric scale structure |
| CN1559983A (en) * | 2004-02-20 | 2005-01-05 | 浙江大学 | Process of preparing magnesium boron oxygen nano thread |
| CN1559899A (en) * | 2004-02-20 | 2005-01-05 | 浙江大学 | Process for preparing aluminium boroxide nano thread |
-
2005
- 2005-04-11 CN CNB2005100115538A patent/CN1301216C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05308956A (en) * | 1991-03-19 | 1993-11-22 | Mitsubishi Heavy Ind Ltd | Preservation of nitric acid bacteria and method for restoration |
| US6376449B2 (en) * | 1993-03-27 | 2002-04-23 | Novozymes A/S | Acidic cleaning composition comprising an acidic protease I |
| JPH11349321A (en) * | 1998-06-05 | 1999-12-21 | Osaka Gas Co Ltd | Production of functional silicon material |
| WO2003004414A1 (en) * | 2001-07-04 | 2003-01-16 | Solvay (Société Anonyme) | Method for obtaining precipitated calcium carbonate particles of nanometric scale structure |
| CN1559983A (en) * | 2004-02-20 | 2005-01-05 | 浙江大学 | Process of preparing magnesium boron oxygen nano thread |
| CN1559899A (en) * | 2004-02-20 | 2005-01-05 | 浙江大学 | Process for preparing aluminium boroxide nano thread |
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| Publication number | Publication date |
|---|---|
| CN1699177A (en) | 2005-11-23 |
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Granted publication date: 20070221 Termination date: 20100411 |