CN115028150A - Preparation method and application of synthetic hydroxyapatite - Google Patents
Preparation method and application of synthetic hydroxyapatite Download PDFInfo
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
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- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—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
- 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 in the prior art, the removal capability of hydroxyapatite prepared by waste on heavy metal ions in wastewater is weak. The preparation method comprises the following steps: respectively calcining livestock bones and eggshells at high temperature, and grinding to obtain livestock bone powder and eggshell powder; adding the livestock bone powder into a beaker, and dropwise adding dilute hydrochloric acid for dissolving; adding eggshell powder into the dissolved livestock bone-dilute hydrochloric acid solution, and uniformly stirring to obtain a transition material for synthesizing hydroxyapatite; and repeatedly washing the transition material by using an ethanol solution and deionized water, and then 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 approach is developed for food processing wastes, and the preparation method is simple and convenient, has low cost and has wide 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
Heavy metals in wastewater in different industries are different in types, contents and existing forms, so that the heavy metals are extremely difficult to degrade, and after entering a water body, except that part of heavy metals are absorbed by aquatic organisms and fishes, most of heavy metals are adsorbed by colloids and particulate matters in water and then deposited at the bottom of the water body, and the pollution has the characteristics of long-term property, accumulation property and the like.
Hydroxyapatite is widely used in the field of adsorption because it is nontoxic and harmless and has strong surface adsorption and ion exchange properties, and many conventional methods for preparing hydroxyapatite are synthesized 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 complicated, and part of reagents can cause secondary environmental pollution.
In order to reduce the preparation cost, researchers have developed the research of preparing hydroxyapatite by using wastes. For example, patents 202111392393.1, 202110662547.8 and 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 perform heat treatment preparation on fishbones, avoid the problem of secondary pollution caused by chemical reagents, and are simple and convenient to operate, but experiments show that the element proportion and the structure of a bone material subjected to high-temperature treatment are changed, particularly the content of calcium is low, so that the ion exchange sites of hydroxyapatite are insufficient, and the removal effect of heavy metal ions is limited.
Disclosure of Invention
In view of the above analysis, the embodiment of the present invention aims to provide a preparation method and an application of synthetic hydroxyapatite, so as to solve the problem that in the prior art, the removal capability of hydroxyapatite prepared by using waste to heavy metal ions in wastewater is weak.
In one aspect, an embodiment of the present invention provides a method for preparing synthetic hydroxyapatite, including the following steps:
s1, respectively calcining the livestock bones and the eggshells at high temperature and then grinding to obtain livestock bone powder and eggshell powder;
s2, adding the livestock bone powder into a beaker, and dropwise adding dilute hydrochloric acid for dissolving;
s3, adding eggshell powder into the dissolved livestock bone-dilute hydrochloric acid solution, and uniformly stirring to obtain a transition material for synthesizing hydroxyapatite;
and S4, repeatedly washing the transition material for synthesizing the hydroxyapatite by using an ethanol solution and deionized water, and drying the washed material to obtain the synthesized hydroxyapatite.
The beneficial effects of the above technical scheme are as follows: based on the concept of 'treating waste by waste', provides an artificial synthesis method for preparing hydroxyapatite by using waste livestock bones and eggshells at low cost. Compared with the prior art, the method has the advantages that 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 that the adsorption effect of the hydroxyapatite on heavy metals is enhanced), the heavy metal removal capability of the artificially synthesized hydroxyapatite is further improved, and the hydroxyapatite obtained by the preparation method has the advantages of good adaptability, easiness in operation, high treatment efficiency, capability of recycling an adsorbent and the like, is a water treatment agent with low cost, simplicity and high efficiency, and has wide application prospect in heavy metal polluted wastewater treatment.
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 the 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 for 4-5 hours at the high temperature which is the same as the calcining temperature of the livestock bones, cooling, and grinding into powder to obtain the eggshell powder.
Further, the step S2 is refined as:
s21, adding the poultry and livestock bone powder into a beaker;
s22, dropwise adding 1-1.5 mol/L dilute hydrochloric acid into the beaker for dissolving to obtain a dissolved livestock bone-dilute hydrochloric acid solution.
Further, the step S3 is refined as:
s31, adding egg shell powder into the dissolved livestock bone-dilute hydrochloric acid solution, wherein the mass ratio of the livestock bone powder to the egg shell powder is 0.6-2;
and S32, stirring the mixed solution added with the egg shell powder by using a magnetic stirrer, and uniformly stirring to obtain the transition material for synthesizing the hydroxyapatite.
Further, in the step S31, the mass ratio of the livestock bone powder to the egg shell powder is 1 (0.5-1.5); and the number of the first and second electrodes,
in the step S32, the stirring time is 4-8 h.
Further, the step S4 further includes:
s41, repeatedly washing the transition material for synthesizing the hydroxyapatite by using 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 for a plurality of times by using deionized water by using a suction filtration device;
s43, drying the transition material washed by the deionized water in a drying oven for 10-15 hours to obtain a synthetic hydroxyapatite product.
Further, in the step S41, washing with an ethanol solution is repeated 3 times;
in the step S42, washing with deionized water is repeated 3 times;
in the step S43, the temperature in the oven is set to be 60-80 ℃.
Compared with the prior art, the invention can realize 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 bone material modified by heat treatment in the prior art, the bone material modified by heat treatment has lower calcium content and insufficient ion exchange sites, so that the adsorption effect is limited.
3. The preparation method for synthesizing the material is simple and easy to operate, is a water treatment agent with low cost, simplicity and high efficiency, and has wide application prospect in heavy metal polluted wastewater treatment.
In another aspect, an embodiment of the present invention provides a synthetic hydroxyapatite, which is prepared by the above 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: adding 1-6 g/L of the synthetic hydroxyapatite into wastewater with the heavy metal ion content of 50-500 mg/L, and oscillating for 2 d at the rotating speed of 0-150 r/min at the temperature of 10-40 ℃.
This 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.
Figure 1 shows a schematic representation of the steps of the preparation process for the synthesis of hydroxyapatite of example 1;
figure 2 shows a diagram of synthetic hydroxyapatite material prepared by the method of example 1;
fig. 3 shows the comparison of the adsorption performance of the synthetic hydroxyapatite prepared by the method of example 2 and the adsorption performance of the chicken bone and eggshell materials of the prior art on lead ions in wastewater after only heat treatment.
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 shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited by 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 "including" and variations thereof as used herein is intended to be 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
One embodiment of the present invention discloses a method for preparing synthetic hydroxyapatite, as shown in fig. 1, comprising the following steps:
s1, respectively calcining the livestock bones and the eggshells at high temperature and then 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 dissolving;
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;
and 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 synthetic hydroxyapatite.
In practice, the synthesized hydroxyapatite is in powder form and is a mesoporous material, as shown in fig. 2.
Both the bones of livestock and the eggshells of chicken eggs belong to the waste of food processing. 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 hydroxyapatite at low cost by using waste livestock bones and eggshells based on the concept of 'treating waste by waste'. Compared with the prior art, the method has the advantages that the problem that the calcium-phosphorus ratio of the original hydroxyapatite is too high or too low is solved (namely the calcium-phosphorus ratio of the hydroxyapatite is adjusted to a set range, so that the adsorption effect of the hydroxyapatite on heavy metals is enhanced), the heavy metal removal capacity of the artificially synthesized hydroxyapatite is further improved, and the hydroxyapatite prepared by the preparation method has the advantages of good adaptability, easiness in operation, high treatment efficiency, recyclable adsorbent and the like, is a low-cost, simple and efficient water treatment agent, and has a wide application prospect in heavy metal polluted wastewater treatment.
Example 2
With the improvement on the embodiment 1, the step S1 further includes:
s11, placing the livestock bones in a muffle furnace, calcining for 4-5 hours at the high temperature of 800-900 ℃, cooling, and grinding into powder to obtain livestock bone powder; the livestock bone comprises at least one of chicken bone, pig bone, and cattle bone;
s12, placing the eggshells in a muffle furnace to be calcined at the high temperature which is the same as the calcining temperature of the livestock bones for 4-5 hours, then cooling, and grinding into powder to obtain the eggshell powder.
Preferably, the step S2 further includes:
s21, adding the poultry and livestock bone powder into a beaker;
s22, dropwise adding 1-1.5 mol/L dilute hydrochloric acid into the beaker for dissolving to obtain a dissolved livestock bone-dilute hydrochloric acid solution.
Preferably, the step S3 further includes:
s31, adding egg shell powder into the dissolved livestock bone-dilute hydrochloric acid solution, wherein the mass ratio of the livestock bone powder to the egg shell powder is 0.6-2;
and S32, stirring the mixed solution added with the egg shell powder by using 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 poultry bone powder to the egg shell powder is 1 (0.5-1.5); in step S32, the stirring time is 4-8 hours.
Preferably, the step S4 further includes:
s41, repeatedly washing the transition material for synthesizing the hydroxyapatite by using 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 for a plurality of times by using deionized water by using a suction filtration device;
s43, drying the transition material washed by the deionized water in a drying oven for 10-15 hours to obtain a synthetic hydroxyapatite product.
Preferably, in the step S41, washing with the ethanol solution is repeated 3 times; in the step S42, washing with deionized water is repeated 3 times; in the step S43, the temperature in the oven is set to be 60-80 ℃.
To effectively illustrate the effect of the synthesized hydroxyapatite obtained by the above method, 4 kinds of synthesized hydroxyapatite materials with different ratios are listed below.
The preparation method of the material I (1: 0.5) comprises the following steps: s1, placing chicken bones and eggshells in a muffle furnace, calcining at 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 chicken bone powder to the eggshell powder is 1:0.5, and placing the mixture on a stirrer to stir for 8 hours; s4, washing the material obtained in the step S3 by using an ethanol solution and deionized water respectively for 3 times by using a suction filtration device, and drying the washed material in an oven at 80 ℃ for 12 h to obtain the material I.
The preparation method of the material II (1: 1) comprises the following steps: s1, placing chicken bones and eggshells in a muffle furnace, calcining at 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 chicken bone powder to the eggshell powder is 1:1, and placing the mixture on a stirrer to stir for 8 hours; s4, washing the material obtained in the step S3 by using an ethanol solution and deionized water respectively for 3 times by using a suction filtration device, and drying the washed material in an oven at 80 ℃ for 12 h to obtain a material II.
The preparation method of the material III (1: 1.5) comprises the following steps: s1, placing chicken bones and eggshells in a muffle furnace, calcining at 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 chicken bone powder to the eggshell powder is 1:1.5, and placing the mixture on a stirrer to stir for 8 hours; s4, washing the material obtained in the step S3 by using an ethanol solution and deionized water respectively for 3 times by using a suction filtration device, and drying the washed material in an oven at 80 ℃ for 12 h to obtain a third material.
The material IV (1: 2.5) and the preparation method comprises the following steps: s1, placing chicken bones and eggshells in a muffle furnace, calcining at 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 of 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 chicken bone powder to the eggshell powder is 1:2.5, and placing the mixture on a stirrer to stir for 8 hours; s4, washing the material obtained in the step S3 by using an ethanol solution and deionized water respectively for 3 times by using a suction filtration device, and drying the washed material in an oven at 80 ℃ for 12 h to obtain a material IV.
For effective experimental comparison, a heat-treated chicken bone material alone and a heat-treated chicken egg shell material alone were also prepared. The heat-treated chicken bone material alone and the heat-treated egg shell material alone were prepared as follows: the chicken bone and the eggshell are placed in a muffle furnace to be calcined for 4 hours at the high temperature of 800 ℃ and ground into powder, the heat treatment poultry bone material is named as the chicken bone, and the heat treatment eggshell material is named as the eggshell.
The prepared 4 kinds of synthetic hydroxyapatite have good adsorption effect on heavy metal ions, and the materials before and after the synthesis have good adsorption effect on the heavy metal ions Pb 2+ The removal effect is compared as shown in fig. 3. By adopting static isothermal adsorption experiment, the comparison is onlyHeat treated animal bone material, heat treated egg shell material and artificially synthesized hydroxyapatite in different proportions for heavy metal ion Pb 2+ The removal effect of (1).
Preparing Pb with the concentration of 500 mg/L 2+ The adding amount of the materials in the solution is 1 g/L, standing for 2 d at 20 ℃, measuring the concentration of the residual heavy metal ions in the solution after 48 h, and taking six materials 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, the six materials are paired with Pb 2+ The adsorption capacity of (b) is 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) > egg shell (27.95 mg/g).
As can be seen from the above comparative experiments, the synthetic hydroxyapatite prepared by the above method has the effect of treating heavy metal ions Pb 2+ The adsorption capacity of the adsorbent is far higher than that of the raw material only subjected to heat treatment, and the adsorption effect is remarkably 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 bone material modified by heat treatment in the prior art, the bone material modified by the heat treatment has lower calcium content and insufficient ion exchange sites, so that the adsorption effect is limited.
3. The preparation method for synthesizing the material is simple and easy to operate, is a water treatment agent with low cost, simplicity and high efficiency, and has wide application prospect in heavy metal polluted wastewater treatment.
Example 3
The invention also discloses a synthetic hydroxyapatite which is prepared by the preparation method of the embodiment 1 or 2, is powdery 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: adding 1-6 g/L of the synthetic hydroxyapatite into wastewater with the heavy metal ion content of 50-500 mg/L, and oscillating for 2 d at the rotating speed of 0-150 r/min at the temperature of 10-40 ℃.
The foregoing description of the embodiments of the present disclosure has been presented for purposes of illustration and description, but 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 described embodiments. The terminology used herein is chosen to best explain the principles of the embodiments, the practical application, or improvements made to the prior art, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (10)
1. A preparation method of synthetic hydroxyapatite is characterized by comprising the following steps:
s1, respectively calcining the livestock bones and the eggshells at high temperature and then grinding to obtain livestock bone powder and eggshell powder;
s2, adding the livestock bone powder into a beaker, and dropwise adding dilute hydrochloric acid to dissolve;
s3, adding eggshell powder into the dissolved livestock bone-dilute hydrochloric acid solution, and uniformly stirring to obtain a transition material for synthesizing hydroxyapatite;
and S4, repeatedly washing the transition material for synthesizing the hydroxyapatite by using an 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 the step S1 further comprises:
s11, placing the livestock bones in a muffle furnace, calcining at the 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 to be calcined at the high temperature which is the same as the calcining temperature of the livestock bones for 4-5 hours, then cooling, and grinding into powder to obtain the eggshell powder.
3. The method for preparing synthetic hydroxyapatite according to claim 1 or 2, wherein the step S2 further comprises:
s21, adding the poultry and livestock bone powder into a beaker;
s22, dropwise adding 1-1.5 mol/L dilute hydrochloric acid into the beaker for dissolving to obtain a dissolved livestock bone-dilute hydrochloric acid solution.
4. The method for preparing synthetic hydroxyapatite according to claim 3, wherein the step S3 further includes:
s31, adding egg shell powder into the dissolved livestock bone-dilute hydrochloric acid solution, wherein the mass ratio of the livestock bone powder to the egg shell powder is 0.6-2;
and S32, stirring the mixed solution added with the egg shell powder by using a magnetic stirrer, and uniformly stirring to obtain the transition material for synthesizing the hydroxyapatite.
5. The method for preparing synthetic hydroxyapatite according to claim 4, wherein in the step S31, the mass ratio of the livestock bone powder to the eggshell powder is 1 (0.5-1.5); and the number of the first and second electrodes,
in the step S32, the stirring time is 4-8 h.
6. The method for preparing synthetic hydroxyapatite according to any one of claims 1, 2, 4 and 5, wherein the step S4 further comprises:
s41, repeatedly washing the transition material for synthesizing the hydroxyapatite by using 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 for a plurality of times by using deionized water by using a suction filtration device;
s43, drying the transition material washed by the deionized water in a drying oven for 10-15 hours to obtain a synthetic hydroxyapatite product.
7. The method for preparing synthetic hydroxyapatite according to claim 6, wherein in the step S41, the washing with the ethanol solution is repeated 3 times;
in the step S42, washing with deionized water is repeated 3 times;
in the step S43, the temperature in the oven is set to be 60-80 ℃.
8. A synthetic hydroxyapatite prepared by the method according to any one of claims 1 to 7, which is in the form of a powder and is a mesoporous material.
9. Use of a synthetic hydroxyapatite prepared by the method according to any one of claims 1 to 7, characterized in that the synthetic hydroxyapatite is used for treating wastewater contaminated by heavy metals.
10. Use of the synthetic hydroxyapatite according to claim 9, characterized in that the treatment of heavy metal contaminated wastewater with the synthetic hydroxyapatite is accomplished by the following application method: adding 1-6 g/L of the synthetic hydroxyapatite into wastewater with the heavy metal ion content of 50-500 mg/L, and oscillating for 2 d at the rotating speed of 0-150 r/min at the temperature of 10-40 ℃.
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