CN114959895B - Ultra-long calcium carbonate whisker and preparation method thereof - Google Patents
Ultra-long calcium carbonate whisker and preparation method thereof Download PDFInfo
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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- C30B29/10—Inorganic compounds or compositions
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The invention relates to the field of whisker preparation, and particularly discloses an ultralong calcium carbonate whisker and a preparation method thereof. The length of the ultralong calcium carbonate crystal whisker is more than 90 μm. The preparation method of the ultra-long calcium carbonate whisker comprises the following steps: step 1, preparing raw materials, which specifically comprises the following steps: step 1-1, preparing a calcium hydroxide suspension; step 1-2, mixing a crystal form control agent with water to form a crystal form control solution; wherein, the crystal form control agent at least comprises magnesium ions and nitrate ions; step 2, mixing the crystal form control solution and the calcium hydroxide suspension to form a mixed solution, and raising the temperature of the mixed solution to 90-110 ℃; and 3, keeping the temperature of the mixed solution constant, introducing carbon dioxide gas into the mixed solution for reaction, filtering when the pH value of the reaction system is reduced, and taking out the precipitate to obtain the calcium carbonate whisker. The prepared ultra-long calcium carbonate crystal whisker can be applied to mortar, and the effects of improving the fracture resistance and tensile strength of the mortar and reducing cracks are achieved.
Description
Technical Field
The invention relates to the field of whisker preparation, in particular to an ultralong calcium carbonate whisker and a preparation method thereof.
Background
A whisker refers to a fiber that is naturally formed or grown in the form of a single crystal under artificially controlled conditions (main form), has a very small diameter (generally in the order of micrometers), does not contain defects (grain boundaries, dislocations, cavities, etc.) that are generally present in materials, and has a highly ordered atomic arrangement, so that its strength is close to the theoretical value of a complete crystal. The strength of the whisker is far higher than that of other chopped fibers, and the whisker is mainly used as a reinforcement of a composite material.
In the field of mortar, whiskers are often used to replace fibers and added into mortar, so that the tensile strength and the breaking strength of the mortar are improved. The mortar only contains water, cement and river sand and does not contain coarse aggregate, so that tensile and anti-bending effects can be better achieved only by adding whiskers with a long length, and the whiskers commonly used in the mortar at present are calcium sulfate whiskers, and the longer calcium sulfate whiskers can be prepared relatively easily.
However, since the calcium sulfate whiskers are very easy to precipitate in an aqueous solution system and have poor dispersibility, the calcium sulfate whiskers are not easy to be uniformly dispersed in a mortar system after being added into the mortar, and thus the effects of improving the flexural strength and the tensile strength of the calcium sulfate whiskers are also easily influenced. Therefore, people always want to replace calcium sulfate whiskers with calcium carbonate whiskers so as to overcome the problems, however, the length of the existing calcium carbonate whiskers can only reach 20-30 μm generally, and the requirement of mortar on the length of the whiskers is difficult to meet.
Disclosure of Invention
In order to prepare the calcium carbonate whisker with the length of more than 90 mu m, the application provides the ultra-long calcium carbonate whisker and the preparation method thereof.
In a first aspect, the application provides an ultra-long calcium carbonate whisker, which adopts the following technical scheme:
the overlength calcium carbonate whisker has a length of 90 μm or more.
Preferably, the length of the overlength calcium carbonate whisker is 90-130 μm.
The calcium carbonate crystal whisker with the length of more than 90 mu m can be used in mortar to achieve the effects of improving the tensile strength and the breaking strength of the mortar and reducing cracks.
In a second aspect, the present application provides an ultra-long calcium carbonate whisker, which adopts the following technical scheme:
a preparation method of ultra-long calcium carbonate whiskers comprises the following steps:
step 1, preparing raw materials, which specifically comprises the following steps:
step 1-1, preparing a calcium hydroxide suspension;
step 1-2, mixing a crystal form control agent with water to form a crystal form control solution; wherein the crystal form control agent at least comprises magnesium ions and nitrate ions;
step 2, mixing the crystal form control solution and the calcium hydroxide suspension to form a mixed solution, and raising the temperature of the mixed solution to 90-110 ℃;
step 3, keeping the temperature of the mixed solution constant, introducing carbon dioxide gas into the mixed solution for reaction, filtering when the pH value of the reaction system is reduced, and taking out precipitates to obtain the ultralong calcium carbonate whiskers;
wherein, the step 1-1 and the step 1-2 can be carried out simultaneously or sequentially and step by step.
Preferably, the constant temperature of the mixed solution in the step 2 and the step 3 is 100-105 ℃.
The calcium carbonate whisker prepared by using a substance at least containing magnesium ions and nitrate ions as a crystal form control agent to react with a calcium hydroxide suspension at a specific temperature has a length of more than 90 mu m, so that the calcium carbonate whisker can be applied to mortar to achieve the effects of improving the fracture resistance and tensile strength of the mortar and reducing cracks.
Preferably, in the step 2, the molar ratio of magnesium ions to calcium ions in the mixed solution is 1.5-2.5.
By controlling the molar ratio of the magnesium ions to the calcium ions, the reaction process can be better controlled, so that the prepared calcium carbonate whisker can reach the length of more than 90 mu m more easily, and the content of the calcium carbonate whisker with the length of more than 90 mu m can be better improved.
Preferably, the crystal form control agent is magnesium nitrate or a compound of magnesium sulfate and magnesium nitrate.
By selecting magnesium nitrate or compounding magnesium sulfate and magnesium nitrate as a crystal form control agent, the length of the formed calcium carbonate whisker can more easily reach more than 90 mu m, and the length of the prepared calcium carbonate whisker is more easily longer.
Preferably, when the crystal form control agent is a complex of magnesium sulfate and magnesium nitrate, the molar ratio of nitrate ions to calcium ions in the mixed solution is 2-4.
By controlling the molar ratio of nitrate ions to calcium ions in the mixed solution, the length of the calcium carbonate whisker prepared by the reaction can more easily reach more than 90 mu m, and meanwhile, the length of the calcium carbonate whisker prepared by the reaction can more easily reach longer length.
Preferably, in the step 3, the carbon dioxide gas is introduced at a flow rate of 10 to 45mL/min.
Preferably, in the step 3, the carbon dioxide gas is introduced at a flow rate of 20 to 30mL/min.
The carbon dioxide is introduced at a low speed, so that the generation process of the whiskers is controlled better, calcium carbonate whiskers with the length of 90 mu m are formed more easily, and meanwhile, the longest length of the prepared calcium carbonate whiskers is longer more easily.
Preferably, in the step 1-1, quicklime or slaked lime is mixed with water, and a digestion reaction is performed at a constant temperature of 90-105 ℃ to obtain a calcium hydroxide suspension.
The calcium hydroxide suspension is prepared by reacting quicklime or slaked lime with water, and the quicklime is generally a waste material, so that the cost is low, the production cost is reduced, the resource is better saved, and the energy conservation and the environmental protection are better facilitated.
Preferably, the time of the digestion reaction in the step 1-1 is 50-70min.
By controlling the digestion temperature and the digestion time, the preparation process of the calcium hydroxide suspension is favorably controlled, so that calcium carbonate whiskers with the length of more than 90 mu m are more easily generated after the prepared calcium hydroxide reacts with the crystal form control solution; meanwhile, the production cost can be better controlled, the temperature is not easy to be too high, the time is not easy to be overlong, and the energy waste is reduced.
Preferably, in the step 3, when the pH value is 6.8-7.0, the reaction is stopped, and the precipitate is filtered to obtain the ultralong calcium carbonate whisker.
The pH value of the reaction stop node is controlled, so that more calcium carbonate whiskers with the length of more than 90 mu m can be generated by the reaction, and meanwhile, the proportion of the finally prepared calcium carbonate whiskers with the length of more than 90 mu m is increased.
In summary, the present application has the following beneficial effects:
1. the calcium carbonate crystal whisker with the length of more than 90 mu m can be used in mortar to achieve the effects of improving the tensile strength and the breaking strength of the mortar and reducing cracks.
2. The calcium carbonate whisker prepared by using a substance at least containing magnesium ions and nitrate ions as a crystal form control agent to react with a calcium hydroxide suspension at a specific temperature has a length of more than 90 mu m, so that the calcium carbonate whisker can be applied to mortar to achieve the effects of improving the fracture resistance and tensile strength of the mortar and reducing cracks.
3. By controlling the molar ratio of calcium ions, magnesium ions and nitrate ions in the mixed solution, the generation of calcium carbonate whiskers with the length of more than 90 mu m is favorably promoted, and meanwhile, the calcium carbonate whiskers prepared by reaction can more easily reach longer length.
Drawings
Fig. 1 is an SEM scanning electron micrograph of the calcium carbonate whiskers prepared in example 1.
Fig. 2 is an SEM scanning electron micrograph of the calcium carbonate whiskers prepared in example 2.
Fig. 3 is an SEM scanning electron micrograph of the calcium carbonate whiskers prepared in example 3.
Fig. 4 is an SEM scanning electron micrograph of the calcium carbonate whiskers prepared in example 4.
Fig. 5 is an XRD pattern of calcium carbonate whiskers prepared in example 4.
Fig. 6 is an SEM scanning electron micrograph of the calcium carbonate whiskers prepared in example 5.
Figure 7 is an XRD pattern of calcium carbonate whiskers prepared in example 5.
Fig. 8 is an SEM scanning electron micrograph of the calcium carbonate whiskers prepared in example 6.
Figure 9 is an XRD pattern of calcium carbonate whiskers prepared in example 6.
Fig. 10 is an SEM scanning electron micrograph of the calcium carbonate whisker prepared in comparative example 1.
Fig. 11 and 12 are SEM scanning electron micrographs of the calcium carbonate whiskers prepared in comparative example 2, viewed from different angles.
Detailed Description
The present application will be described in further detail with reference to the following examples and accompanying drawings.
In the following examples and comparative examples, the magnesium nitrate was magnesium nitrate hexahydrate with a relative molecular weight of 256.41g/mol; the magnesium sulfate was heptahydrate magnesium sulfate and had a relative molecular weight of 246.47g/mol.
Example 1
A preparation method of ultra-long calcium carbonate whiskers comprises the following steps:
step 1, preparing raw materials, which specifically comprises the following steps:
step 1-1, preparing a calcium hydroxide suspension, specifically as follows:
adding 800mL of deionized water into a four-neck flask, then adding 5.60g of calcium oxide, heating to 90 ℃, carrying out digestion reaction at constant temperature for 70min, and obtaining calcium hydroxide suspension.
Step 1-2, weighing 25.64g of magnesium nitrate, 12.32g of magnesium sulfate and 200mL of water, and uniformly mixing to form a crystal form control solution.
And 2, adding the crystal form control solution into the calcium hydroxide suspension, continuously stirring at the rotating speed of 200r/min to form a mixed solution, and raising the temperature of the mixed solution to 90 ℃.
And 3, keeping the temperature of the mixed solution constant, introducing carbon dioxide gas into the mixed solution at the flow rate of 10mL/min for reaction, stopping the reaction until the pH value of the mixed solution is reduced to 6.8, filtering, and taking out a precipitate to obtain the calcium carbonate whisker.
Wherein step 1-1 and step 1-2 are performed simultaneously.
The electron micrograph of the calcium carbonate whisker prepared in this example is shown in FIG. 1;
example 2
A preparation method of ultra-long calcium carbonate whiskers comprises the following steps:
step 1, preparing raw materials, which specifically comprises the following steps:
step 1-1, preparing a calcium hydroxide suspension, specifically as follows:
adding 800mL of deionized water into a four-neck flask, then adding 5.60g of calcium oxide, heating to 105 ℃, carrying out digestion reaction under a constant temperature condition, and reacting for 50min to obtain a calcium hydroxide suspension.
Step 1-2, weighing 51.29g of magnesium nitrate, 12.32g of magnesium sulfate and 200mL of water, and uniformly mixing to form a crystal form control solution.
And 2, adding the crystal form control solution into the calcium hydroxide suspension, continuously stirring at the rotating speed of 200r/min to form a mixed solution, and raising the temperature of the mixed solution to 110 ℃.
And 3, keeping the temperature of the mixed solution constant, introducing carbon dioxide gas into the mixed solution at a flow rate of 45mL/min for reaction, stopping the reaction until the pH value of the mixed solution is reduced to 7.0, filtering, and taking out a precipitate to obtain the calcium carbonate whisker.
Wherein step 1-1 and step 1-2 are performed simultaneously.
The electron micrograph of the calcium carbonate prepared in this example is shown in FIG. 2.
Example 3
A preparation method of ultra-long calcium carbonate whiskers comprises the following steps:
step 1, preparing raw materials, specifically as follows:
step 1-1, preparing a calcium hydroxide suspension, specifically as follows:
adding 800mL of deionized water into a four-neck flask, then adding 5.60g of calcium oxide, heating to 90 ℃, carrying out digestion reaction under the constant temperature condition, and reacting for 70min to obtain a calcium hydroxide suspension.
Step 1-2, weighing 38.46g of magnesium nitrate and 200mL of water, and uniformly mixing to form a crystal form control solution.
And 2, adding the crystal form control solution into the calcium hydroxide suspension, continuously stirring at the rotating speed of 200r/min to form a mixed solution, and raising the temperature of the mixed solution to 90 ℃.
And 3, keeping the temperature of the mixed solution constant, introducing carbon dioxide gas into the mixed solution at the flow rate of 10mL/min for reaction, stopping the reaction until the pH value of the mixed solution is reduced to 6.8, filtering, and taking out a precipitate to obtain the calcium carbonate whisker.
Wherein, the step 1-1 and the step 1-2 are carried out simultaneously.
The electron micrograph of the calcium carbonate whiskers prepared in this example is shown in detail in FIG. 3.
Example 4
A preparation method of ultra-long calcium carbonate whiskers comprises the following steps:
step 1, preparing raw materials, which specifically comprises the following steps:
step 1-1, preparing a calcium hydroxide suspension, specifically as follows:
adding 800mL of deionized water into a four-neck flask, then adding 5.60g of calcium oxide, heating to 105 ℃, carrying out digestion reaction under a constant temperature condition, and reacting for 50min to obtain a calcium hydroxide suspension.
Step 1-2, weighing 64.10g of magnesium nitrate and 200mL of water, and uniformly mixing to form a crystal form control solution.
And 2, adding the crystal form control solution into the calcium hydroxide suspension, continuously stirring at the rotating speed of 250r/min to form a mixed solution, and raising the temperature of the mixed solution to 110 ℃.
And 3, keeping the temperature of the mixed solution constant, introducing carbon dioxide gas into the mixed solution at the flow rate of 45mL/min for reaction, stopping the reaction until the pH value of the mixed solution is reduced to 7.0, filtering, and taking a precipitate to obtain the calcium carbonate whisker.
Wherein step 1-1 and step 1-2 are performed simultaneously.
The electron micrograph of the calcium carbonate whiskers prepared in this example is shown in detail in FIG. 4.
The XRD pattern of the calcium carbonate whiskers prepared in this example is shown in detail in FIG. 5.
Example 5
A preparation method of ultra-long calcium carbonate whiskers comprises the following steps:
step 1, preparing raw materials, specifically as follows:
step 1-1, preparing a calcium hydroxide suspension, specifically as follows:
adding 800mL of deionized water into a four-neck flask, then adding 5.60g of calcium oxide, heating to 100 ℃, carrying out digestion reaction under a constant temperature condition, and reacting for 60min to obtain a calcium hydroxide suspension.
Step 1-2, weighing 51.28g of magnesium nitrate and 200mL of water, and uniformly mixing to form a crystal form control solution.
And 2, adding the crystal form control solution into the calcium hydroxide suspension, continuously stirring at the rotating speed of 200r/min to form a mixed solution, and raising the temperature of the mixed solution to 100 ℃.
And 3, keeping the temperature of the mixed solution constant, introducing carbon dioxide gas into the mixed solution at the flow rate of 20mL/min for reaction, stopping the reaction until the pH value of the mixed solution is reduced to 6.9, filtering, and taking out a precipitate to obtain the calcium carbonate whisker.
Wherein, the step 1-1 and the step 1-2 are carried out simultaneously.
The electron micrograph of the calcium carbonate whisker prepared in this example is shown in detail in fig. 6;
the XRD pattern of the calcium carbonate whiskers prepared in this example is shown in FIG. 7.
Example 6
A preparation method of ultra-long calcium carbonate whiskers comprises the following steps:
step 1, preparing raw materials, which specifically comprises the following steps:
step 1-1, preparing a calcium hydroxide suspension, specifically as follows:
800mL of deionized water is added into a four-neck flask, then 5.60g of calcium oxide is added, the mixture is heated to 95 ℃, digestion reaction is carried out under the constant temperature condition, and reaction time is 65min, so as to obtain calcium hydroxide suspension.
Step 1-2, weighing 51.28g of magnesium nitrate and 200mL of water, and uniformly mixing to form a crystal form control solution.
And 2, adding the crystal form control solution into the calcium hydroxide suspension, continuously stirring at the rotating speed of 200r/min to form a mixed solution, and raising the temperature of the mixed solution to 105 ℃.
And 3, keeping the temperature of the mixed solution constant, introducing carbon dioxide gas into the mixed solution at the flow rate of 30mL/min for reaction, stopping the reaction until the pH value of the mixed solution is reduced to 7.0, filtering, and taking a precipitate to obtain the calcium carbonate whisker.
Wherein step 1-1 and step 1-2 are performed simultaneously.
The electron micrograph of the calcium carbonate whisker prepared in this example is shown in FIG. 8;
the XRD pattern of the calcium carbonate whiskers prepared in this example is shown in detail in FIG. 9.
Comparative example 1
The difference from example 3 is that: in step 1-2, magnesium nitrate is replaced by equal amount of magnesium chloride.
An electron micrograph of the calcium carbonate whiskers prepared in this comparative example is shown in detail in FIG. 10.
Comparative example 2
The difference from example 3 is that: in step 1-2, magnesium nitrate was replaced with an equal amount of magnesium sulfate.
The electron micrographs of the calcium carbonate whiskers prepared in this comparative example are shown in fig. 11 and 12.
Experiment 1
The calcium carbonate whiskers prepared in the above examples and comparative examples were scanned by a scanning electron microscope, the lengths of the calcium carbonate whiskers were observed, and the longest lengths (μm) of the calcium carbonate whiskers and the proportion (%) of the calcium carbonate whiskers having a length of more than 90 μm were recorded.
The scanning electron micrographs of the calcium carbonate whiskers prepared in the above examples and comparative examples are shown in FIGS. 1 to 12 in detail.
The longest length (. Mu.m) of the calcium carbonate whiskers obtained in the above examples and comparative examples and the proportion (%) of calcium carbonate whiskers having a length of more than 90 μm are shown in Table 1.
TABLE 1
| Longest length (mum) of whisker | Whisker percentage (%), with length greater than 90 μm | |
| Example 1 | 90 | 5％ |
| Example 2 | 95 | 10％ |
| Example 3 | 100 | 20％ |
| Example 4 | 105 | 30％ |
| Example 5 | 120 | 45％ |
| Example 6 | 130 | 50％ |
| Comparative example 1 | 40 | 0％ |
| Comparative example 2 | 20 | 0％ |
As can be seen from the comparison of the data of examples 1 to 6 in table 1, by controlling the reaction conditions during the preparation of calcium carbonate whiskers, it is advantageous to increase the length of the prepared calcium carbonate whiskers better, to make the longest length of the prepared calcium carbonate whiskers longer, and to increase the proportion of the calcium carbonate whiskers having a length greater than 90 μm better.
According to the comparison of the data of examples 1-6 and comparative examples 1-2 in Table 1, calcium carbonate whiskers larger than 90 μm can be generated only when the crystal form control agent contains magnesium ions and nitrate ions, and calcium carbonate whiskers larger than 90 μm cannot be generated when the crystal form control agent is replaced by other magnesium salts for reaction.
Application example 1
The wet-mixed M10 mortar is prepared from the following components in parts by mass:
180kg of water; 200kg of Portland cement; 80 kilograms of fly ash; 1380kg of sand; 5kg of calcium carbonate whiskers.
In this application example, the calcium carbonate whiskers were the calcium carbonate whiskers obtained in example 1.
The preparation method of the mortar comprises the following steps:
and weighing the water, the portland cement, the fly ash, the sand and the calcium carbonate whiskers according to the mass, putting the weighed materials into a mortar stirrer for mixing, stirring at the rotating speed of 100r/min, and uniformly stirring to obtain the mortar.
Application example 2
The difference from application example 1 is that: the calcium carbonate whiskers were the calcium carbonate whiskers obtained in example 6.
Comparative application example 1
The difference from application example 1 is that: calcium sulfate whiskers with the same amount and the length of 100 mu m are adopted to replace calcium carbonate whiskers.
Comparative application example 2
The difference from application example 1 is that: the calcium carbonate whiskers were the calcium carbonate whiskers prepared in comparative example 1.
Comparative application example 3
The difference from application example 1 is that: the calcium carbonate whiskers were the calcium carbonate whiskers prepared in comparative example 2.
Experiment 2
According to 9. Cube compressive strength tests in JGJ/T70-2009 Standard for testing high basic Performance of building mortar, 28d compressive strength (MPa) of the mortar prepared by the application example and the comparative application example is detected.
The data from the above experiments are detailed in table 2.
TABLE 2
| 28d compressive strength (MPa) | |
| Application example 1 | 12.5 |
| Application example 2 | 15.8 |
| Comparative application example 1 | 10.5 |
| Comparative application example 2 | 10.2 |
| Comparative application example 3 | 9.5 |
According to the comparison of the data of the application examples 1-2 and the comparative application example 1 in the table 2, the addition of the calcium carbonate whiskers to the mortar is beneficial to better improving the compressive strength of the mortar and reducing the influence on the strength of the mortar caused by the difficulty in uniform dispersion of the whiskers in the mortar after the whiskers are added to the mortar.
According to the comparison of the data of application examples 1-2 and comparative application examples 2-3 in table 2, the longer the calcium carbonate whisker is, the better the calcium carbonate whisker is added into the mortar to reinforce the mortar.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: equivalent changes in structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (5)
1. A preparation method of an ultralong calcium carbonate whisker, wherein the length of the ultralong calcium carbonate whisker is more than 90 μm, is characterized by comprising the following steps:
step 1, preparing raw materials, specifically as follows:
step 1-1, preparing a calcium hydroxide suspension;
step 1-2, mixing a crystal form control agent with water to form a crystal form control solution; wherein the crystal form control agent is magnesium nitrate or a compound of magnesium sulfate and magnesium nitrate;
the molar ratio of magnesium ions to calcium ions in the mixed solution is 1.5-2.5;
when the crystal form control agent is a compound of magnesium sulfate and magnesium nitrate, the molar ratio of nitrate ions to calcium ions in the mixed solution is 2-4;
step 2, mixing the crystal form control solution and the calcium hydroxide suspension to form a mixed solution, and raising the temperature of the mixed solution to 90-110 ℃;
step 3, keeping the temperature of the mixed solution constant, introducing carbon dioxide gas into the mixed solution for reaction, filtering when the pH value of a reaction system is reduced, and taking out precipitates to obtain the ultralong calcium carbonate whiskers;
wherein, the step 1-1 and the step 1-2 can be carried out simultaneously or sequentially and step by step.
2. The method for preparing the ultralong calcium carbonate whiskers, according to claim 1, is characterized in that: in the step 3, the flow rate of the carbon dioxide gas is 10-45mL/min.
3. The method for preparing the ultralong calcium carbonate whiskers according to any one of claims 1 to 2, characterized in that: in the step 1-1, quicklime or slaked lime is mixed with water, and a digestion reaction is carried out at a constant temperature of 90-105 ℃ to prepare a calcium hydroxide suspension.
4. The method for preparing the ultra-long calcium carbonate whiskers as claimed in claim 3, characterized in that: the time of the digestion reaction in the step 1-1 is 50-70min.
5. The method for preparing the ultra-long calcium carbonate whiskers as claimed in any one of claims 1 to 2, characterized in that: and in the step 3, when the pH value is 6.8-7.0, stopping the reaction, filtering, and taking out the precipitate to obtain the ultralong calcium carbonate crystal whisker.
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| AU2002359958A1 (en) * | 2001-12-31 | 2003-07-15 | Beijing University Of Chemical Technology | Calcium carbonate of different shapes and the preparing process thereof |
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