CN115028150B - Preparation method and application of synthetic hydroxyapatite - Google Patents
Preparation method and application of synthetic hydroxyapatite Download PDFInfo
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- C01B25/16—Oxyacids of phosphorus; Salts thereof
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/048—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
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Abstract
The invention provides a preparation method and application of synthetic hydroxyapatite, belongs to the technical field of heavy metal wastewater treatment, and solves the problem that the hydroxyapatite prepared by waste in the prior art has weak capability of removing heavy metal ions in wastewater. The preparation method comprises the following steps: calcining fowl and livestock bones and eggshells at high temperature respectively, and grinding to obtain fowl and livestock bones powder and eggshell powder; adding animal bone powder into a beaker, and dripping dilute hydrochloric acid for dissolution; adding eggshell powder into the dissolved livestock bone-dilute hydrochloric acid solution, and uniformly stirring to obtain a transition material for synthesizing hydroxyapatite; repeatedly washing the transition material with ethanol solution and deionized water, and drying to obtain the synthetic hydroxyapatite. The prepared synthetic hydroxyapatite can be used as an adsorbent to effectively remove heavy metal ions in wastewater, a new utilization way is developed for food processing wastes, and the preparation method is simple and convenient, low in cost and wide in application prospect.
Description
Technical Field
The invention relates to the technical field of heavy metal wastewater treatment, in particular to a preparation method and application of synthetic hydroxyapatite.
Background
The heavy metals in the wastewater of different industries are different in types, contents and existence forms, so that the heavy metals are extremely difficult to degrade, and after entering a water body, most of the heavy metals are absorbed by aquatic organisms and fishes, and most of the heavy metals are adsorbed by colloid and particulate matters in the water and deposited at the bottom of the water body, so that the pollution has the characteristics of long-term property, accumulation property and the like.
Hydroxyapatite is widely used in the adsorption field because of being nontoxic and harmless, and having strong surface adsorptivity and ion exchange property, and the existing preparation method of hydroxyapatite is mostly synthesized by using chemical raw materials, for example, patent nos. 2021106499371.1 and 2021110712252.2. However, the preparation cost of the method is high, the method is complex and tedious, and part of reagents can cause secondary environmental pollution.
In order to reduce the preparation cost, researchers have developed studies on the preparation of hydroxyapatite using waste. For example, patent 202111392393.1, 202110662547.8, JP 2012-148903 are prepared by hydrothermal synthesis, but such methods are not easy to mass produce and still require a large amount of chemical reagents as main raw materials. Sunil et al and patent JP 2015-182901 are used for preparing the fishbone by heat treatment, so that the problem of secondary pollution caused by chemical reagents is avoided, the operation is simple and convenient, but experiments show that the element proportion and the structure of the bone material after high-temperature treatment are changed, especially the calcium content is low, the ion exchange site of the hydroxyapatite is insufficient, and the removal effect of heavy metal ions is limited.
Disclosure of Invention
In view of the above analysis, the present invention aims to provide a preparation method and application of synthetic hydroxyapatite, which are used for solving the problem that the removal capability of the hydroxyapatite prepared by waste in the prior art on heavy metal ions in wastewater is weak.
In one aspect, the embodiment of the invention provides a preparation method for synthesizing hydroxyapatite, which comprises the following steps:
s1, respectively calcining livestock bones and eggshells at high temperature, and grinding to obtain livestock bone powder and eggshell powder;
s2, adding animal bone powder into a beaker, and dropwise adding dilute hydrochloric acid for dissolution;
s3, adding eggshell powder into the dissolved livestock bone-dilute hydrochloric acid solution, and uniformly stirring to obtain a transition material for synthesizing hydroxyapatite;
s4, repeatedly washing the transition material for synthesizing the hydroxyapatite with ethanol solution and deionized water, and drying the washed material to obtain the synthesized hydroxyapatite.
The beneficial effects of the technical scheme are as follows: provides an artificial synthesis method for preparing the hydroxylapatite by utilizing the discarded bones of livestock and eggshells with low cost based on the concept of treating wastes with wastes. Compared with the prior art, the method improves the problem that the calcium-phosphorus ratio of the original hydroxyapatite is too high or too low (namely, the calcium-phosphorus ratio of the hydroxyapatite is adjusted to a set range so as to enhance the adsorption effect of the hydroxyapatite on heavy metals), further improves the heavy metal removal capability of the artificially synthesized hydroxyapatite, and the hydroxyapatite obtained by the preparation method has the advantages of good adaptability, easiness in operation, high treatment efficiency, recycling of the adsorbent and the like, is a water treatment agent with low cost, simplicity and high efficiency, and has wide application prospect in the treatment of heavy metal polluted wastewater.
Based on a further improvement of the above method, the step S1 further includes:
s11, placing the livestock bones in a muffle furnace, calcining at a high temperature of 800-900 ℃ for 4-5 hours, cooling, and grinding into powder to obtain livestock bone powder;
s12, placing the eggshells in a muffle furnace, calcining at the same high temperature as that of the livestock bones for 4-5 hours, cooling, and grinding into powder to obtain eggshell powder.
Further, the step S2 is refined as follows:
s21, adding animal bone powder into a beaker;
s22, dropwise adding 1-1.5 mol/L of dilute hydrochloric acid into the beaker for dissolution, and obtaining a dissolved livestock bone-dilute hydrochloric acid solution.
Further, the step S3 is refined as follows:
s31, adding eggshell powder into the dissolved livestock bone-dilute hydrochloric acid solution, wherein the mass ratio of the livestock bone powder to the eggshell powder is 0.6-2;
s32, stirring the mixed solution added with the eggshell powder by a magnetic stirrer, and uniformly stirring to obtain the transition material for synthesizing the hydroxyapatite.
In the step S31, the mass ratio of the livestock bone powder to the eggshell powder is 1 (0.5-1.5); and, in addition, the processing unit,
in the step S32, the stirring time is 4-8 hours.
Further, the step S4 further includes:
s41, repeatedly washing the transition material for synthesizing the hydroxyapatite with an ethanol solution for a plurality of times by using a suction filtration device;
s42, repeatedly washing the transition material washed by the ethanol solution with deionized water for a plurality of times by using a suction filtration device;
s43, placing the transition material washed by the deionized water into a baking oven to be dried for 10-15 hours, and obtaining a synthetic hydroxyapatite product.
Further, in the step S41, the washing with the ethanol solution is repeated 3 times;
in the step S42, the washing is repeated for 3 times by deionized water;
in the step S43, the temperature in the oven is set to be 60-80 ℃.
Compared with the prior art, the invention has at least one of the following beneficial effects:
1. compared with the bone material obtained by only heat treatment, the prepared synthetic hydroxyapatite has obviously improved adsorption effect.
2. Compared with the prior art, the heat treatment modified bone material has low calcium content and insufficient ion exchange sites, so that the adsorption effect is limited.
3. The preparation method of the material synthesis is simple and easy to operate, is a water treatment agent with low cost, is simple and efficient, and has wide application prospect in the treatment of heavy metal polluted wastewater.
On the other hand, the embodiment of the invention provides the synthetic hydroxyapatite which is prepared by the preparation method, is in a powder shape and is a mesoporous material.
In addition, the embodiment of the invention also provides application of the synthetic hydroxyapatite prepared by the preparation method, and the synthetic hydroxyapatite is used for treating heavy metal polluted wastewater.
Further, the treatment of heavy metal contaminated wastewater with synthetic hydroxyapatite is accomplished by the following application method: 1-6 g/L of the synthetic hydroxyapatite is added into the wastewater with the heavy metal ion content of 50-500 mg/L, and the wastewater is oscillated for 2d at the temperature of 10-40 ℃ and the rotational speed of 0-150 r/min.
The summary is provided to introduce a selection of concepts in a simplified form that are further described below in the detailed description. This summary is not intended to identify key features or essential features of the disclosure, nor is it intended to be used to limit the scope of the disclosure.
Drawings
The foregoing and other objects, features and advantages of the disclosure will be apparent from the following more particular descriptions of exemplary embodiments of the disclosure as illustrated in the accompanying drawings wherein like reference numbers generally represent like parts throughout the exemplary embodiments of the disclosure.
FIG. 1 is a schematic diagram showing the steps of the method for preparing the synthetic hydroxyapatite of example 1;
FIG. 2 shows a diagram of a synthetic hydroxyapatite material prepared by the method of example 1;
fig. 3 shows the comparison of the adsorption performance of synthetic hydroxyapatite prepared by the method of example 2 on lead ions in wastewater of the prior art heat-treated chicken bone and eggshell material only.
Detailed Description
Embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While embodiments of the present disclosure are illustrated in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
The term "comprising" and variations thereof as used herein means open ended, i.e., "including but not limited to. The term "or" means "and/or" unless specifically stated otherwise. The term "based on" means "based at least in part on". The terms "one example embodiment" and "one embodiment" mean "at least one example embodiment. The term "another embodiment" means "at least one additional embodiment". The terms "first," "second," and the like, may refer to different or the same object. Other explicit and implicit definitions are also possible below.
Example 1
An embodiment of the invention discloses a preparation method for synthesizing hydroxyapatite, which is shown in figure 1 and comprises the following steps:
s1, respectively calcining livestock bones and eggshells at high temperature, and grinding to obtain livestock bone powder and eggshell powder;
s2, adding the livestock bone powder obtained in the step S1 into a beaker, and dropwise adding dilute hydrochloric acid for dissolution;
s3, adding the eggshell powder obtained in the step S1 into the dissolved livestock bone-dilute hydrochloric acid solution obtained in the step S2, and uniformly stirring to obtain a transition material for synthesizing hydroxyapatite;
s4, repeatedly washing the transition material for synthesizing the hydroxyapatite in the step S3 by using an ethanol solution and deionized water by using a suction filtration device, and drying the washed material to obtain the synthesized hydroxyapatite.
In practice, the prepared synthetic hydroxyapatite is in a powder form, and is a mesoporous material, as shown in figure 2.
The bones of livestock and eggshells belong to the waste of the food processing process. The obtained synthetic hydroxyapatite can be used as an adsorption material for carrying out adsorption treatment on heavy metal sewage.
Compared with the prior art, the preparation method provided by the embodiment provides an artificial synthesis method for preparing the hydroxyapatite by using the discarded bones of livestock and eggshells at low cost based on the concept of treating waste with waste. Compared with the prior art, the method improves the problem that the calcium-phosphorus ratio of the original hydroxyapatite is too high or too low (namely, the calcium-phosphorus ratio of the hydroxyapatite is adjusted to a set range so as to enhance the adsorption effect of the hydroxyapatite on heavy metals), further improves the heavy metal removal capability of the artificially synthesized hydroxyapatite, and the hydroxyapatite obtained by the preparation method has the advantages of good adaptability, easiness in operation, high treatment efficiency, recycling of the adsorbent and the like, is a water treatment agent with low cost, simplicity and high efficiency, and has wide application prospect in the treatment of heavy metal polluted wastewater.
Example 2
The improvement of the embodiment 1, the step S1 further includes:
s11, placing the livestock bones in a muffle furnace, calcining at a high temperature of 800-900 ℃ for 4-5 hours, cooling, and grinding into powder to obtain livestock bone powder; the livestock bone comprises at least one of chicken bone, pig bone, cattle bone, etc.;
s12, placing the eggshells in a muffle furnace, calcining at the same high temperature as that of the livestock bones for 4-5 hours, cooling, and grinding into powder to obtain eggshell powder.
Preferably, the step S2 further includes:
s21, adding animal bone powder into a beaker;
s22, dropwise adding 1-1.5 mol/L of dilute hydrochloric acid into the beaker for dissolution, and obtaining a dissolved livestock bone-dilute hydrochloric acid solution.
Preferably, the step S3 further includes:
s31, adding eggshell powder into the dissolved livestock bone-dilute hydrochloric acid solution, wherein the mass ratio of the livestock bone powder to the eggshell powder is 0.6-2;
s32, stirring the mixed solution added with the eggshell powder by a magnetic stirrer, and uniformly stirring to obtain the transition material for synthesizing the hydroxyapatite.
Preferably, in the step S31, the mass ratio of the livestock bone powder to the eggshell powder is 1 (0.5-1.5); in the step S32, the stirring time is 4 to 8 hours.
Preferably, the step S4 further includes:
s41, repeatedly washing the transition material for synthesizing the hydroxyapatite with an ethanol solution for a plurality of times by using a suction filtration device;
s42, repeatedly washing the transition material washed by the ethanol solution with deionized water for a plurality of times by using a suction filtration device;
s43, placing the transition material washed by the deionized water into a baking oven to be dried for 10-15 hours, and obtaining a synthetic hydroxyapatite product.
Preferably, in the step S41, the washing with the ethanol solution is repeated 3 times; in the step S42, the washing is repeated for 3 times by deionized water; in the step S43, the temperature in the oven is set to be 60-80 ℃.
In order to effectively explain the effect of the synthetic hydroxyapatite obtained by the above method, 4 kinds of hydroxyapatite materials synthesized in different proportions are listed below.
Material one (1:0.5), the preparation method is as follows: s1, placing chicken bones and eggshells in a muffle furnace, calcining at a high temperature of 800 ℃ for 4 h, and grinding into powder; s2, adding the chicken bone powder obtained in the step S1 into a beaker, and dropwise adding 1 mol/L dilute hydrochloric acid into the beaker to dissolve the chicken bone powder; s3, adding the eggshell powder obtained in the step S1 into the beaker in the step S2, wherein the mass ratio of the eggshell powder to the eggshell powder is 1:0.5, and placing the mixture on a stirrer to stir 8 h; s4, washing the material obtained in the step S3 with ethanol solution and deionized water for 3 times by using a suction filtration device, and putting the washed material into an oven to dry at 80 ℃ for 12 h to obtain the material I.
Material II (1:1), the preparation method is as follows: s1, placing chicken bones and eggshells in a muffle furnace, calcining at a high temperature of 800 ℃ for 4 h, and grinding into powder; s2, adding the chicken bone powder obtained in the step S1 into a beaker, and dropwise adding 1 mol/L dilute hydrochloric acid into the beaker to dissolve the chicken bone powder; s3, adding the eggshell powder obtained in the step S1 into the beaker in the step S2, wherein the mass ratio of the eggshell powder to the eggshell powder is 1:1, and placing the mixture on a stirrer to stir 8 h; s4, washing the material obtained in the step S3 with ethanol solution and deionized water for 3 times by using a suction filtration device, and putting the washed material into an oven to dry at 80 ℃ for 12 h to obtain the material II.
Material III (1:1.5), the preparation method is as follows: s1, placing chicken bones and eggshells in a muffle furnace, calcining at a high temperature of 800 ℃ for 4 h, and grinding into powder; s2, adding the chicken bone powder obtained in the step S1 into a beaker, and dropwise adding 1 mol/L dilute hydrochloric acid into the beaker to dissolve the chicken bone powder; s3, adding the eggshell powder obtained in the step S1 into the beaker in the step S2, wherein the mass ratio of the eggshell powder to the eggshell powder is 1:1.5, and placing the mixture on a stirrer to stir 8 h; s4, washing the material obtained in the step S3 with ethanol solution and deionized water for 3 times by using a suction filtration device, and putting the washed material into an oven to dry at 80 ℃ for 12 h to obtain the material III.
Material IV (1:2.5), the preparation method is as follows: s1, placing chicken bones and eggshells in a muffle furnace, calcining at a high temperature of 800 ℃ for 4 h, and grinding into powder; s2, adding the chicken bone powder obtained in the step S1 into a beaker, and dropwise adding 1 mol/L dilute hydrochloric acid into the beaker to dissolve the chicken bone powder; s3, adding the eggshell powder obtained in the step S1 into the beaker in the step S2, wherein the mass ratio of the eggshell powder to the eggshell powder is 1:2.5, and placing the mixture on a stirrer to stir 8 h; s4, washing the material obtained in the step S3 with ethanol solution and deionized water for 3 times by using a suction filtration device, and putting the washed material into an oven to dry at 80 ℃ for 12 h to obtain the material IV.
For effective experimental comparison, only heat treated chicken bone material and only heat treated eggshell material were also prepared. The preparation of the heat-treated chicken bone material and the heat-treated eggshell material were as follows: the chicken bones and eggshells are placed in a muffle furnace to be calcined at a high temperature of 800 ℃ for 4 h, and are ground into powder, the heat-treated livestock bone material is named as chicken bones, and the heat-treated eggshell material is named as eggshells.
The prepared 4 kinds of synthetic hydroxyapatite have good adsorption effect on heavy metal ions, and the material before and after synthesis has good adsorption effect on heavy metal ions Pb 2+ The removal effect is compared as shown in fig. 3. By adopting a static isothermal adsorption experiment, comparing the poultry and livestock bone material after only heat treatment with the egg shell material after only heat treatment and the artificially synthesized hydroxyapatite under different proportions to heavy metal ions Pb 2+ Is not limited, and the removal effect of the catalyst is not limited.
Pb with a concentration of 500mg/L 2+ Solution, material adding amount is 1 g/L, standing for 2d at 20 ℃ for 48 h, measuring concentration of residual heavy metal ions in the solution, and six materials are used for Pb 2+ The removal effect of (2) is shown in FIG. 3, the abscissa represents the materials before and after synthesis and at different ratios, and the ordinate represents the adsorption capacity of the materials to heavy metal ions.
As can be seen from FIG. 3, pb is a target for six materials 2+ The adsorption capacity of (C) was 1:1 (401.66 mg/g) > 1:0.5 (393.72 mg/g) > 1:1.5 (352.48 mg/g) > 1:2.5 (253.62 mg/g) > chicken bone (52.80 mg/g) > eggshell (27.95 mg/g).
As can be seen from the comparative experiments, the synthetic hydroxyl groups prepared by the above methodApatite heavy metal ion Pb 2+ The adsorption capacity of the catalyst is far higher than that of the raw material subjected to heat treatment only, and the adsorption effect is obviously improved.
Compared with the prior art, the preparation method provided by the embodiment has the following beneficial effects:
1. compared with the bone material obtained by only heat treatment, the prepared synthetic hydroxyapatite has obviously improved adsorption effect.
2. Compared with the prior art, the heat treatment modified bone material has low calcium content and insufficient ion exchange sites, so that the adsorption effect is limited.
3. The preparation method of the material synthesis is simple and easy to operate, is a water treatment agent with low cost, is simple and efficient, and has wide application prospect in the treatment of heavy metal polluted wastewater.
Example 3
The invention also discloses a synthetic hydroxyapatite which is prepared by the preparation method described in the embodiment 1 or 2, is in a powder shape and is a mesoporous material.
Example 4
The invention also discloses application of the synthetic hydroxyapatite prepared by the method in the embodiment 1 or 2, and the synthetic hydroxyapatite is used for treating heavy metal polluted wastewater.
Preferably, the treatment of heavy metal contaminated wastewater with synthetic hydroxyapatite is accomplished by the following application method: 1-6 g/L of the synthetic hydroxyapatite is added into the wastewater with the heavy metal ion content of 50-500 mg/L, and the wastewater is oscillated for 2d at the temperature of 10-40 ℃ and the rotational speed of 0-150 r/min.
The foregoing description of the embodiments of the present disclosure has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described. The terminology used herein is chosen in order to best explain the principles of the embodiments, the practical application, or the improvement of the prior art, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (10)
1. The preparation method of the synthetic hydroxyapatite is characterized by comprising the following steps:
s1, respectively calcining livestock bones and eggshells at high temperature, and grinding to obtain livestock bone powder and eggshell powder; wherein the high-temperature calcination temperature is 800-900 ℃;
s2, adding animal bone powder into a beaker, and dropwise adding dilute hydrochloric acid for dissolution;
s3, adding eggshell powder into the dissolved livestock bone-dilute hydrochloric acid solution, and uniformly stirring to obtain a transition material for synthesizing hydroxyapatite; the mass ratio of the livestock bone powder to the eggshell powder is 0.6-2;
s4, repeatedly washing the transition material for synthesizing the hydroxyapatite with ethanol solution and deionized water, and drying the washed material to obtain the synthesized hydroxyapatite.
2. The method for preparing synthetic hydroxyapatite according to claim 1, wherein said step S1 further comprises:
s11, placing the livestock bones in a muffle furnace, calcining at a high temperature of 800-900 ℃ for 4-5 hours, cooling, and grinding into powder to obtain livestock bone powder;
s12, placing the eggshells in a muffle furnace, calcining at the same high temperature as that of the livestock bones for 4-5 hours, cooling, and grinding into powder to obtain eggshell powder.
3. The method for preparing synthetic hydroxyapatite according to claim 1 or 2, wherein said step S2 further comprises:
s21, adding animal bone powder into a beaker;
s22, dropwise adding 1-1.5 mol/L of dilute hydrochloric acid into the beaker for dissolution to obtain a dissolved livestock bone-dilute hydrochloric acid solution.
4. A method of preparing synthetic hydroxyapatite according to claim 3, wherein said step S3 further comprises:
s31, adding eggshell powder into the dissolved livestock bone-dilute hydrochloric acid solution;
s32, stirring the mixed solution added with the eggshell powder by a magnetic stirrer, and uniformly stirring to obtain the transition material for synthesizing the hydroxyapatite.
5. The method according to claim 4, wherein in the step S31, the mass ratio of the powder of the livestock bones to the powder of the eggshells is 1 (0.5-1.5); and, in addition, the processing unit,
in the step S32, the stirring time is 4-8 hours.
6. The method of any one of claims 1, 2, 4, and 5, wherein step S4 further comprises:
s41, repeatedly washing the transition material for synthesizing the hydroxyapatite with an ethanol solution for a plurality of times by using a suction filtration device;
s42, repeatedly washing the transition material washed by the ethanol solution with deionized water for a plurality of times by using a suction filtration device;
s43, putting the transition material washed by the deionized water into a baking oven to be dried for 10-15 h, and obtaining a synthetic hydroxyapatite product.
7. The method for preparing synthetic hydroxyapatite according to claim 6, wherein in said step S41, washing with ethanol solution is repeated 3 times;
in the step S42, the washing is repeated for 3 times by deionized water;
in the step S43, the temperature in the oven is set to be 60-80 ℃.
8. A synthetic hydroxyapatite prepared by the method of any one of claims 1 to 7, in powder form, and being a mesoporous material.
9. Use of a synthetic hydroxyapatite prepared by the method according to any one of claims 1 to 7, characterised in that said synthetic hydroxyapatite is used for the treatment of heavy metal contaminated wastewater.
10. The use of synthetic hydroxyapatite according to claim 9, wherein the treatment of heavy metal contaminated wastewater with synthetic hydroxyapatite is accomplished by the following application method: adding 1-6 g/L of the synthetic hydroxyapatite into the wastewater with the heavy metal ion content of 50-500 mg/L, and oscillating for 2d at the temperature of 10-40 ℃ and the rotating speed of 0-150 r/min.
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CN108992707A (en) * | 2018-09-27 | 2018-12-14 | 广东海洋大学 | The preparation method of injectable chitosan oyster shell hydroxyapatite temperature-sensitive hydrogel |
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