CN111410493A - Linear nano hydroxyapatite/high-alumina cement composite material and preparation method and application thereof - Google Patents
Linear nano hydroxyapatite/high-alumina cement composite material and preparation method and application thereof Download PDFInfo
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
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- C01B25/325—Preparation by double decomposition
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Abstract
The invention discloses a linear nano hydroxyapatite/high alumina cement composite material and a preparation method and application thereof, wherein the composite material comprises the following components in parts by mass: 1-15 parts of linear nano hydroxyapatite and 1000 parts of high-alumina cement. The linear nano-hydroxyapatite and the high-alumina cement are creatively combined to prepare the composite material, the linear nano-hydroxyapatite and the high-alumina cement are combined by utilizing the characteristics of high flexibility, good mechanical property, high thermal stability and fire resistance of the linear nano-hydroxyapatite, and the compressive strength of the high-alumina cement is improved by the obtained composite material through the linear nano-hydroxyapatite, so that the linear nano-hydroxyapatite/high-alumina cement composite material prepared by the invention has high compressive strength, low cost and good practical value.
Description
Technical Field
The invention relates to the technical field of inorganic nonmetallic materials, in particular to a linear nano hydroxyapatite/high alumina cement composite material and a preparation method and application thereof.
Background
High alumina cement, also known as aluminate cement (CAC), is a fast-hardening, high-strength, heat-resistant and corrosion-resistant cementitious material with the main characteristics of high early strength, high temperature resistance and corrosion resistance. Due to the rapid development of the metallurgical industry, the performance requirements on refractory cement are higher and higher. CAC hydration produces CA2、CAH10、C2AH8And various hydration products, which are mutually staggered to form a crystal-gel network structure, and obtain excellent mechanical strength in the cement hardening process. When CAC is used as refractory castable, the mechanical strength of CAC is obviously reduced along with the continuous increase of external temperature. The occurrence of this situation has greatly limited the use of CAC as a refractory castable. Since the mechanical strength of cement is closely related to the hydration products produced during its hydration and its microstructure, it is important to study the hydration behavior of CAC to improve its mechanical strength.
Hydroxyapatite (HAP), also known as hydroxyapatite, basic calcium phosphate, is calcium apatite (Ca)5(PO4)3(OH)) in natural mineralization. OH group-The radicals can be replaced by fluoride, chloride and carbonate ions to produce fluorapatite or chloroapatite, wherein calcium ions can be replaced by various metal ions by ion exchange reaction to form M apatite corresponding to the metal ions (M represents metal ions substituting for calcium ions). HAP is the major inorganic component of human and animal bones. Most of the HAP reports in the literature at present are the application of the HAP as medical materials, and the application of the HAP in the field of refractory materials is never reported.
Disclosure of Invention
Aiming at the defects or shortcomings in the prior art, the invention provides a linear nano hydroxyapatite/high alumina cement composite material and a preparation method and application thereof.
The invention provides a linear nano hydroxyapatite/high alumina cement composite material, which comprises the following components in parts by mass: 1-15 parts of linear nano hydroxyapatite and 1000 parts of high-alumina cement.
In some embodiments of the present invention, the composite material comprises the following components in parts by mass: 5-10 parts of linear nano hydroxyapatite and 1000 parts of high-alumina cement.
In some embodiments of the present invention, the linear nano-hydroxyapatite has a diameter of 50 to 80nm and a length of 6 to 10 μm.
According to the invention, the linear nano-hydroxyapatite/high-alumina cement composite material comprises linear nano-hydroxyapatite and high-alumina cement, and the characteristics of high flexibility, good mechanical property, high thermal stability and fire resistance of the linear nano-hydroxyapatite are utilized, so that the composite material has higher compressive strength compared with single-phase high-alumina cement after being calcined at 1100 ℃, and thus, the compressive capacity of the composite material provided by the invention is remarkably improved. Through detection, the compressive strength of the composite material provided by the invention is above 48 KN. Because the linear nano hydroxyapatite/high-alumina cement composite material provided by the invention has high compressive strength and low cost, the linear nano hydroxyapatite/high-alumina cement composite material has good practical value.
The second aspect of the invention provides a preparation method of a linear nano hydroxyapatite/high alumina cement composite material, which is characterized by comprising the following steps:
linear nano hydroxyapatite and high-alumina cement are mixed according to the proportion of (1-15): 1000, and obtaining the linear nano hydroxyapatite/high alumina cement composite material.
In some embodiments of the present invention, the method for preparing linear nano-hydroxyapatite comprises:
dissolving soluble alkali in water to prepare alkali liquor with the hydroxide concentration of 1.7-1.8 mol/L, dissolving soluble calcium salt in water to prepare calcium solution with the calcium ion concentration of 0.2-0.3 mol/L, and dissolving soluble phosphate in water to prepare phosphate solution with the phosphate concentration of 0.3-0.4 mol/L;
methanol and oleic acid are mixed according to the following ratio (5-8): (10-12) mixing the components according to the volume ratio of (10-15): (10-15): (15-18) adding the alkali liquor, the calcium liquor and the phosphate radical solution in a volume ratio to obtain a mixed solution;
placing the mixed solution in a reaction kettle, sealing and heating for reaction to obtain a reactant;
and sequentially cooling, washing and drying the reactants to obtain the linear nano hydroxyapatite.
In some embodiments of the invention, when the mixed solution is placed in a reaction kettle for sealing and heating for reaction, the temperature of the mixed solution is raised from room temperature to 180-190 ℃ within 90min, and the mixed solution is kept at 180-190 ℃ for 24-25 h.
In some embodiments of the invention, the soluble base is sodium hydroxide.
In some embodiments of the invention, the soluble calcium salt is calcium chloride.
In some embodiments of the invention, the soluble phosphate salt is sodium dihydrogen phosphate.
According to the preparation method of the linear nano-hydroxyapatite/high-alumina cement composite material provided by the invention, the prepared linear nano-hydroxyapatite is combined with high-alumina cement by utilizing the characteristics of high flexibility, good mechanical property, high thermal stability and fire resistance of the linear nano-hydroxyapatite, and the compressive strength of the high-alumina cement is improved by the obtained composite material through the linear nano-hydroxyapatite, so that the linear nano-hydroxyapatite/high-alumina cement composite material prepared by the invention has high compressive strength, low cost and good practical value.
In a third aspect, the invention provides a high compression-resistant cement, which comprises the linear nano-hydroxyapatite/high-alumina cement composite material or the linear nano-hydroxyapatite/high-alumina cement composite material prepared by the preparation method.
The invention provides a high compression cement in a third aspect, which comprises a composite material prepared by taking linear nano-hydroxyapatite and high-alumina cement as raw materials, wherein the composite material utilizes the characteristics of high flexibility, good mechanical property, high thermal stability and fire resistance of the hydroxyapatite to combine the prepared linear nano-hydroxyapatite with the high-alumina cement, the linear nano-hydroxyapatite can improve the compression strength of the high-alumina cement, and further the high compression cement containing the linear nano-hydroxyapatite/high-alumina cement composite material has high compression strength, and the preparation cost of the linear nano-hydroxyapatite and high-alumina cement composite material is low, so that the high compression cement containing the linear nano-hydroxyapatite/high-alumina cement composite material has good practical value.
The technical scheme of the invention has the following advantages:
(1) the invention creatively combines the linear nano hydroxyapatite and the high alumina cement to prepare the high compression resistant cement material, so that the compression resistant performance of the high alumina cement is obviously improved. Through detection, the compressive strength of the material compounded by the two materials after calcination is above 48 KN;
(2) the preparation method provided by the invention is simple and easy to operate, and only needs to control the proportion of the linear nano hydroxyapatite and the high-alumina cement without other complex operations. The coating can be prepared on site or in advance, and has strong flexibility;
(3) the invention realizes the high-efficiency preparation of linear nano-hydroxyapatite, and can produce the linear nano-hydroxyapatite in batches;
(4) the invention provides a novel application method of hydroxyapatite, and expands the application field of hydroxyapatite.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is an XRD pattern of a prior art aluminous cement;
FIG. 2 is an XRD pattern of the high alumina cement and linear nano-hydroxyapatite/high alumina cement composite of example 1 of the present invention;
FIG. 3 is a graph showing the hydration exotherm for the aluminous cement and linear nano-hydroxyapatite/aluminous cement composite of example 1 of the present invention;
fig. 4 is SEM images (a, b) of the aluminous cement of example 1 of the present invention and SEM images (c, d) of the linear nano-hydroxyapatite/aluminous cement composite;
fig. 5 is a line graph showing the compressive strength of the calcined standard sample of high alumina cement and the standard sample of linear nano hydroxyapatite/high alumina cement composite material of example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention provides a linear nano hydroxyapatite/high alumina cement composite material, which comprises the following components in parts by mass: 1-15 parts of linear nano hydroxyapatite and 1000 parts of high-alumina cement.
In the invention, the proportion of the linear nano-hydroxyapatite and the high-alumina cement is an important factor influencing the compression resistance of the composite material. If the dosage of the linear nano-hydroxyapatite is too low, the compression resistance of the composite material cannot be improved; however, when the amount of the linear nano-hydroxyapatite is too high, the setting time of the cement may be increased, which is not favorable for practical construction. Therefore, the compressive strength of the high alumina cement can be more effectively improved in practical production only by adding a proper amount of the linear hydroxyapatite to the high alumina cement. Based on the problem, the invention controls the mass ratio of the two components to be (1-15): 1000 may be, for example, 1:1000, 2:1000, 3:1000, 4:1000, 5:1000, 6:1000, 7:1000, 8:1000, 9:1000, 10:1000, 11:1000, 12:1000, 13:1000, 14:1000, 15: 1000.
In an embodiment of the invention, the linear nano-hydroxyapatite/high alumina cement composite has a compressive strength of 48KN or more after calcination.
After the linear nano-hydroxyapatite/high-alumina cement composite material provided by the invention is calcined at 1100 ℃, compared with single-phase high-alumina cement, the composite material has higher compressive strength due to the addition of the linear nano-hydroxyapatite, and the compressive capacity is obviously improved. The detection shows that the compressive strength of the composite material is above 48 KN. Therefore, the linear nano hydroxyapatite/high alumina cement composite material provided by the invention has the advantages of high compressive strength, low cost and good practical value.
In the embodiment of the invention, the composition comprises the following components in parts by mass: 5-10 parts of linear nano hydroxyapatite and 1000 parts of high-alumina cement, wherein the mixing ratio is the optimal ratio of the linear nano hydroxyapatite to the high-alumina cement.
In the embodiment of the invention, the linear nano hydroxyapatite has a diameter of 50-80 nm and a length of 6-10 μm.
The second aspect of the invention provides a preparation method of a linear nano hydroxyapatite/high alumina cement composite material, which comprises the following steps:
linear nano hydroxyapatite and high-alumina cement are mixed according to the proportion of (1-15): 1000, and obtaining the linear nano hydroxyapatite/high alumina cement composite material.
According to the preparation method of the linear nano-hydroxyapatite/high-alumina cement composite material, the linear nano-hydroxyapatite and the high-alumina cement are combined to prepare the composite material, so that the compression resistance of the calcined composite material is remarkably improved. Through detection, the compressive strength of the composite material prepared by the invention is above 48 KN. The preparation method provided by the invention is simple and easy to operate, and only needs to control the proportion of the linear nano hydroxyapatite and the high-alumina cement without other complex operations. Can be prepared on site or in advance, and has strong flexibility.
In an embodiment of the present invention, the method for preparing linear nano hydroxyapatite comprises:
(1) dissolving soluble alkali in water to prepare alkali liquor with the hydroxide concentration of 1.7-1.8 mol/L, dissolving soluble calcium salt in water to prepare calcium solution with the calcium ion concentration of 0.2-0.3 mol/L, and dissolving soluble phosphate in water to prepare phosphate solution with the phosphate concentration of 0.3-0.4 mol/L;
(2) methanol and oleic acid are mixed according to the following ratio (5-8): (10-12) mixing the components according to the volume ratio of (10-15): (10-15): (15-18) adding alkali liquor, calcium liquor and phosphate radical solution in a volume ratio to obtain a mixed solution;
(3) placing the mixed solution in a reaction kettle, sealing and heating for reaction to obtain a reactant;
(4) and cooling, washing and drying the reactants in sequence to obtain the linear nano-hydroxyapatite.
The preparation method of the linear nano-hydroxyapatite provided by the embodiment is simple and easy to operate, can realize the high-efficiency preparation of the linear nano-hydroxyapatite, and further can realize the batch production of the linear nano-hydroxyapatite.
In the embodiment of the present invention, when the mixed solution is placed in a reaction kettle for sealed heating reaction, the temperature of the mixed solution is raised from room temperature to 180-.
In an embodiment of the invention, the soluble base is sodium hydroxide.
In an embodiment of the invention, the soluble calcium salt is calcium chloride.
In an embodiment of the invention, the soluble phosphate is sodium dihydrogen phosphate.
In a third aspect, the invention provides a high compression-resistant cement, which comprises the linear nano-hydroxyapatite/high-alumina cement composite material or the linear nano-hydroxyapatite/high-alumina cement composite material prepared by the preparation method.
The following are examples of the present invention.
Example 1
A preparation method of a linear nano hydroxyapatite/high alumina cement composite material comprises the following steps:
(1) 1.0500g of sodium hydroxide (NaOH, analytically pure) is dissolved in 15m L of deionized water to prepare an alkali solution, 0.3330g of calcium chloride (CaCl2, analytically pure) is dissolved in 12m L of deionized water to prepare a calcium solution, and 0.9360g of sodium dihydrogen phosphate dihydrate (NaH) is added2PO4·2H2O, analytical pure) was dissolved in 18m L of deionized water to prepare a phosphate solution.
Mixing 6m L and methanol (CH)3OH) with 10.5m L oleic acid (C)18H34O2) Mixing to obtain mixed solution, and adding the alkali solution, the calcium solution and the phosphate solution into the mixed solution respectively under mechanical stirring.
The resulting mixture was transferred to a polytetrafluoroethylene-lined stainless steel autoclave (100m L), sealed and heated to 180 ℃, and reacted at 180 ℃ for 24 hours.
(4) Cooling the obtained mixture to room temperature, adding ethanol solution, washing the mixture with a centrifuge for 3 times, and drying the mixture in a drying oven to obtain linear nano-hydroxyapatite (Ca)10(PO4)6(OH)2)。
(5) 0.75g of linear nano-hydroxyapatite is taken and fully mixed with 150g of high-alumina cement to obtain the linear nano-hydroxyapatite/high-alumina cement composite material.
As can be seen from FIGS. 1 and 2, CaAl in the composite material prepared in this example2O4·10H2O(CAH10) And Ca2Al2O6·8H2O(C2AH8) The two chemical products are increased, so that the compressive strength of the cement can be effectively improved by adding the nano hydroxyapatite.
FIG. 3 is a hydration heat release curve diagram of high alumina cement and linear nano hydroxyapatite/high alumina cement composite material, and it can be seen from the diagram that the hydration process of the composite material can be advanced by adding the nano hydroxyapatite.
Fig. 4 is SEM images (a, b) of the high alumina cement and SEM images (c, d) of the linear nano-hydroxyapatite/high alumina cement composite material, and it can be seen from d that there is a significant linear nano-hydroxyapatite in the composite material.
The linear nano hydroxyapatite/high alumina cement composite material is added into deionized water according to the proportion (mass ratio) of 0.4 of water ash, and after being fully mixed, 450g of standard river sand is added. Fully stirring the mixture by a stirrer, and shaping the mixture by a mould to prepare a standard sample block. And placing the standard sample block in a curing box with the humidity of 95% for curing for 1 day, then demolding, then respectively curing for 3 days and 7 days, drying the cured sample block for 24 hours at the temperature of 110 ℃, and finally calcining for 3 hours at the temperature of 1100 ℃. The compression strength of the standard sample block is tested by a cement compression strength tester for 1 day, 3 days and 7 days. The test results are shown in FIG. 5. As can be seen from fig. 5, compared with the non-composite linear nano-hydroxyapatite, the compression resistance of the high-alumina cement material compounded with the linear nano-hydroxyapatite is obviously improved.
Example 2
This example is prepared essentially identically to example 1, except that: and (3) fully mixing 1.5g of linear nano-hydroxyapatite with 150g of high-alumina cement to obtain the linear nano-hydroxyapatite/high-alumina cement composite material.
The linear nano hydroxyapatite/high alumina cement composite material prepared by the embodiment is added into deionized water according to the proportion (mass ratio) of 0.4 of water ash, and is fully mixed and added with 450g of standard river sand. Fully stirring the mixture by a stirrer, and shaping the mixture by a mould to prepare a standard sample block. And placing the standard sample block in a curing box with the humidity of 95% for curing for 1 day, then demolding, then respectively curing for 3 days and 7 days, drying the cured sample block for 24 hours at the temperature of 110 ℃, and finally calcining for 3 hours at the temperature of 1100 ℃. The compression strength of the standard sample block is tested by a cement compression strength tester for 1 day, 3 days and 7 days.
Example 3
This example is prepared essentially identically to example 1, except that: 2.25g of linear nano-hydroxyapatite is taken and fully mixed with 150g of high-alumina cement to obtain the linear nano-hydroxyapatite/high-alumina cement composite material.
The linear nano hydroxyapatite/high alumina cement composite material prepared by the embodiment is added into deionized water according to the proportion (mass ratio) of 0.4 of water ash, and is fully mixed and added with 450g of standard river sand. Fully stirring the mixture by a stirrer, and shaping the mixture by a mould to prepare a standard sample block. And placing the standard sample block in a curing box with the humidity of 95% for curing for 1 day, then demolding, then respectively curing for 3 days and 7 days, drying the cured sample block for 24 hours at the temperature of 110 ℃, and finally calcining for 3 hours at the temperature of 1100 ℃. The compression strength of the standard sample block is tested by a cement compression strength tester for 1 day, 3 days and 7 days.
Example 4
This example is prepared essentially identically to example 1, except that: 0.15g of linear nano-hydroxyapatite is taken and fully mixed with 150g of high-alumina cement to obtain the linear nano-hydroxyapatite/high-alumina cement composite material.
The linear nano hydroxyapatite/high alumina cement composite material prepared by the embodiment is added into deionized water according to the proportion (mass ratio) of 0.4 of water ash, and is fully mixed and added with 450g of standard river sand. Fully stirring the mixture by a stirrer, and shaping the mixture by a mould to prepare a standard sample block. And placing the standard sample block in a curing box with the humidity of 95% for curing for 1 day, then demolding, then respectively curing for 3 days and 7 days, drying the cured sample block for 24 hours at the temperature of 110 ℃, and finally calcining for 3 hours at the temperature of 1100 ℃. The compression strength of the standard sample block is tested by a cement compression strength tester for 1 day, 3 days and 7 days.
Example 5
This example is prepared essentially identically to example 1, except that: 3.0g of linear nano-hydroxyapatite is taken and fully mixed with 150g of high-alumina cement to obtain the linear nano-hydroxyapatite/high-alumina cement composite material.
The linear nano hydroxyapatite/high alumina cement composite material prepared by the embodiment is added into deionized water according to the proportion (mass ratio) of 0.4 of water ash, and is fully mixed and added with 450g of standard river sand. Fully stirring the mixture by a stirrer, and shaping the mixture by a mould to prepare a standard sample block. And placing the standard sample block in a curing box with the humidity of 95% for curing for 1 day, then demolding, then respectively curing for 3 days and 7 days, drying the cured sample block for 24 hours at the temperature of 110 ℃, and finally calcining for 3 hours at the temperature of 1100 ℃. The compression strength of the standard sample block is tested by a cement compression strength tester for 1 day, 3 days and 7 days.
The results of the compression resistance test of examples 2 to 5 are shown in Table 1.
TABLE 1
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The linear nano hydroxyapatite/high alumina cement composite material is characterized by comprising the following components in parts by mass: 1-15 parts of linear nano hydroxyapatite and 1000 parts of high-alumina cement.
2. The composite material as claimed in claim 1, which is characterized by comprising the following components in parts by mass: 5-10 parts of linear nano hydroxyapatite and 1000 parts of high-alumina cement.
3. The composite material according to claim 1, wherein the linear nano-hydroxyapatite has a diameter of 50 to 80nm and a length of 6 to 10 μm.
4. A preparation method of a linear nano hydroxyapatite/high alumina cement composite material is characterized by comprising the following steps:
linear nano hydroxyapatite and high-alumina cement are mixed according to the proportion of (1-15): 1000, and obtaining the linear nano hydroxyapatite/high alumina cement composite material.
5. The preparation method according to claim 4, wherein the preparation method of the linear nano-hydroxyapatite comprises the following steps:
dissolving soluble alkali in water to prepare alkali liquor with the hydroxide concentration of 1.7-1.8 mol/L, dissolving soluble calcium salt in water to prepare calcium solution with the calcium ion concentration of 0.2-0.3 mol/L, and dissolving soluble phosphate in water to prepare phosphate solution with the phosphate concentration of 0.3-0.4 mol/L;
methanol and oleic acid are mixed according to the following ratio (5-8): (10-12) mixing the components according to the volume ratio of (10-15): (10-15): (15-18) adding the alkali liquor, the calcium liquor and the phosphate radical solution in a volume ratio to obtain a mixed solution;
placing the mixed solution in a reaction kettle, sealing and heating for reaction to obtain a reactant;
and sequentially cooling, washing and drying the reactants to obtain the linear nano hydroxyapatite.
6. The preparation method of claim 5, wherein the temperature of the mixed solution is raised from room temperature to 180-190 ℃ within 90min, and the mixed solution is kept at 180-190 ℃ for 24-25 h when the mixed solution is placed in a reaction kettle for sealing and heating for reaction.
7. The method of claim 5, wherein the soluble base is sodium hydroxide.
8. The method of claim 5, wherein the soluble calcium salt is calcium chloride.
9. The method according to claim 5, wherein the soluble phosphate is sodium dihydrogen phosphate.
10. A cement with high compression resistance, which comprises the linear nano-hydroxyapatite/high alumina cement composite material according to claims 1 to 4 or the linear nano-hydroxyapatite/high alumina cement composite material prepared by the preparation method according to claims 5 to 9.
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| KR20180051087A (en) * | 2016-11-08 | 2018-05-16 | 경상대학교산학협력단 | Hydroxyapatite-transition metal composite, preparation method thereof and meterial for blocking ultraviolet rays and visible rays comprising the same |
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| CN103626144A (en) * | 2013-12-13 | 2014-03-12 | 中国科学院上海硅酸盐研究所 | High temperature resistant non-combustible hydroxyapatite paper with high flexibility and preparation method thereof |
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| CN107721221A (en) * | 2016-08-12 | 2018-02-23 | 中国石油天然气集团公司 | A kind of high temperature resistant phosphate cement and its application |
| KR20180051087A (en) * | 2016-11-08 | 2018-05-16 | 경상대학교산학협력단 | Hydroxyapatite-transition metal composite, preparation method thereof and meterial for blocking ultraviolet rays and visible rays comprising the same |
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| CN112939565A (en) * | 2021-04-01 | 2021-06-11 | 武汉帅麟科技有限公司 | Geopolymer light mortar and preparation method and application thereof |
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