CN103861567B - The preparation method of hydroxyapatite/bagasse active carbon - Google Patents
The preparation method of hydroxyapatite/bagasse active carbon Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of hydroxyapatite/bagasse active carbon.In the calcium acetate solution of the 0.05mol/L ~ 0.5mol/L of 250ml, add <b> enter </b>4.4mol/L ammonium acetate buffer solution 250ml, mix, add 10 ~ 60 grams of bagasse again, after electric stirring, by supersonic oscillations 30 ~ 60 minutes, leave standstill 24 ~ 48 hours; When rapid stirring, in calcium acetate, ammonium acetate and bagasse mixture, add 0.015mol/L ~ 0.15mol/L ammonium dihydrogen phosphate of 500ml, adjust ph to 7.5 ~ 8.0, stirred at ambient temperature 10 minutes; Heating water bath, to 100 DEG C, reacts 48 ~ 60 hours, obtains hydroxyapatite/bagasse mix suspending thing solution; Naturally cool, filter, after washing, drying 16 hours at 70 DEG C, hydroxyapatite/bagasse mixture; Carbonize at 450 DEG C ~ 650 DEG C, then grind, cross 100 mesh sieves.Present invention process is simple, cost is low; Obtained product can be widely used in industrial and mining enterprises' advanced treating containing cadmium and plumbous waste water operation.
Description
Technical field
The present invention relates to a kind of preparation method of hydroxyapatite/bagasse active carbon.
Background technology
Along with the fast development of modern industry, containing cadmium and plumbous heavy metal wastewater thereby discharge capacity increasing, the pollution of heavy metal has become one of the most serious environmental problem, therefore, very urgent to the process of the heavy metal wastewater thereby containing cadmium and lead.In numerous heavy metal, cadmium ion is that toxicity is maximum, be detrimental to health one of the most serious heavy metal ion, when cadmium ion runs up to doses in human body, just easily causes the pathology of human body kidney, intestines, bone.And the harm of lead ion to human body is quite widely, if the lead of human body excess intake can cause the grievous injury of lead anaemia and nervous system, bone hemopoietic system, digestive system, kidney and reproductive system.The method containing cadmium and plumbous heavy metal wastewater thereby when pre-treatment mainly contains coprecipitation, flocculence, oxidation-reduction method, photocatalytic degradation method, ion-exchange, solvent extraction, absorption method, membrane separation process etc.Chemical precipitation method can produce a large amount of excess sludge containing heavy metal, improves processing cost, and cadmium and plumbous recovery also have certain difficulty, and the processing cost of ion-exchange is also higher.In recent years, absorption method is removed cadmium with plumbous as a research direction by Many researchers.Conventional adsorbent has: active carbon, FeOOH, goethite, titanium dioxide and activated alumina etc., and this type of adsorbent mostly is Powdered, although specific area is large, but adsorbance is still lower.
Apatite is the synthos mineral that nature extensively exists, and according to the kind of the anion that its inside exists, can be divided into the different subspecies mineral such as fluorine, chlorine, hydroxyapatite.Wherein, the investigation and application of hydroxyapatite is the most extensive.The molecular formula of hydroxyapatite is Ca
10(PO
4)
6(OH)
2for hexagonal crystal system, this crystal chemistry feature, make dissimilar heavy metal can the position of calcium in substituted hydroxy apatite, there is good ionic adsorption and commutativity, can adsorb and reclaim the fluorine ion in underground water, the heavy metal in industrial wastewater and organic polymer, and hydroxyapatite and environment have good harmony, not easily cause secondary pollution, thus become a kind of novel environmental sorbing material received much concern.Have amount of literature data to show, the removal effect of hydroxyapatite to cadmium and lead is remarkable.Active carbon is a kind of adsorbent of function admirable, but it is limited to the adsorption effect of cadmium and lead.Therefore, how the adsorbent that two kinds have good adsorbent performance being organically combined, make its absorption property reach the effect of learning from other's strong points to offset one's weaknesses, is a hot issue of research at present.Therefore, be primary raw material with bagasse, prepare hydroxyapatite/bagasse active carbon compound adsorbent and there is development prospect advantageously and Practical significance.
Summary of the invention
Object of the present invention is just to provide one and adopts hydrothermal synthesis method and calcination method at ambient pressure, take bagasse as primary raw material, with calcium acetate, ammonium acetate and ammonium dihydrogen phosphate (ADP) for auxiliary material, prepares hydroxyapatite/bagasse active carbon compound adsorbent.
At present, study more absorption except in cadmium and plumbous sorbing material, single material has hydrated manganese dioxide, goethite, NACF, titanium dioxide and nano metal aluminium powder etc.; The material of compound has modified alta-mud, modified zeolite, illite, modified peanut, plant ash, weathered coal etc.The main component of the sorbing material had in these sorbing materials is iron-aluminium oxide, and they are also absorption cadmium and plumbous main matter, and the main component in partial adsorbates material is some organic substances such as active carbon.In order to overcome existing except cadmium and plumbous adsorbent capacity low, limited sorption capacity, and make full use of the abundant bagasse resource in Guangxi.The invention provides a kind of except cadmium and plumbous sorbing material---the preparation method of hydroxyapatite/bagasse active carbon.Hydroxyapatite/bagasse active carbon can not only make process afterwards containing the cadmium of cadmium and lead water sample and lead concentration all lower than 0.050mgL
-1, and adsorption capacity is large, when being respectively lower than 5.0mgL containing cadmium and lead water sample initial concentration
-1.After adsorption equilibrium in water sample cadmium and lead concentration lower than 0.01mgL
-1.
Concrete steps are:
(1) bagasse is placed in baking oven to dry at 80 DEG C, crosses 20 mesh sieves after broken for subsequent use.
(2) in 2L beaker, add the calcium acetate solution that 250ml concentration is 0.05mol/L ~ 0.5mol/L, then add
enter250ml concentration is 4.4mol/L ammonium acetate buffer solution, mixes, and adds 10 ~ 60 grams of step (1) gained bagasse, after electric stirring, by supersonic oscillations 30 ~ 60 minutes, leaves standstill 24 ~ 48 hours.
(3) in step (2) product, adding 500ml concentration is under fast stirring 0.015mol/L ~ 0.15mol/L ammonium dihydrogen phosphate, with full-automatic titrator, under agitation, slowly add mass percent concentration be 10% ammoniacal liquor carefully regulate the pH value of reaction to 7.5 ~ 8.0, stirred at ambient temperature 10 minutes.
(4) step (3) products therefrom is placed in water bath with thermostatic control upper, build glass surface ware, heating water bath, to 100 DEG C, reacts 48 ~ 60 hours.
(5) step (4) products therefrom is cooled naturally, filter, measure and record filtrate final ph.Solid phase precipitation thing after ultra-pure water cyclic washing twice, then uses absolute ethanol washing one time, and filter cake is placed in porcelain dish at 70 DEG C dry 16 hours, obtains hydroxyapatite/bagasse mixture.
(6) step (5) gained hydroxyapatite/bagasse mixture is carbonized at 450 DEG C ~ 650 DEG C, obtain hydroxyapatite/bagasse active carbon compound; Then grind, cross 100 mesh sieves, obtain hydroxyapatite/bagasse active carbon.
Present invention process is simple, owing to utilizing bagasse for main raw material(s), greatly reduces production cost, and improves product property indices; Obtained product can be widely used in industrial and mining enterprises' advanced treating containing cadmium and plumbous waste water operation.
Accompanying drawing explanation
The scanning electron microscope (SEM) photograph of Fig. 1, Fig. 2, Fig. 3 hydroxyapatite/bagasse active carbon obtained by the embodiment of the present invention.
Detailed description of the invention
Embodiment:
(1) bagasse is placed in baking oven to dry at 80 DEG C, for subsequent use with crossing 20 mesh sieves after omnipotent crusher in crushing.
(2) in 2L beaker, add the calcium acetate solution that 250ml concentration is 0.2mol/L, then add
enter250ml concentration is 4.4mol/L ammonium acetate buffer solution, mixes, and adds 50 grams of step (1) gained bagasse, after electric stirring, by supersonic oscillations 30 minutes, leaves standstill 24 hours.
(3) in step (2) products therefrom, adding 500ml concentration is under fast stirring 0.06mol/L ammonium dihydrogen phosphate, with full-automatic titrator, under agitation, slowly add mass percent concentration be 10% ammoniacal liquor carefully regulate the pH value of reaction to 7.5, stirred at ambient temperature 10 minutes.
(4) step (3) products therefrom is placed in water bath with thermostatic control upper, build glass surface ware, heating water bath, to 100 DEG C, reacts 48 hours.
(5) step (4) products therefrom is cooled naturally, filter, measure and record filtrate final ph.Solid phase precipitation thing after ultra-pure water cyclic washing twice, then uses absolute ethanol washing one time, and filter cake is placed in porcelain dish at 70 DEG C dry 16 hours, obtains hydroxyapatite/bagasse mixture.
(6) step (5) gained hydroxyapatite/bagasse mixture is carbonized at 600 DEG C, obtain hydroxyapatite/bagasse active carbon compound; Then grind, cross 100 mesh sieves, hydroxyapatite/bagasse active carbon.
The thing phase of obtained hydroxyapatite/bagasse active carbon with structure, become to be grouped into, adopt German Bruker-axsD8ADVANCE type X-ray diffractometer to test, angle of diffraction scope 2 θ=10-90 °, diffraction speed 4 °/minute.The pattern of sample and particle diameter adopt ESEM to observe.Electronic Speculum test adopts the JSM-5610LV type ESEM of NEC, amplifies 5000-20000 and doubly carries out morphology observation.
Claims (1)
1. a preparation method for hydroxyapatite/bagasse active carbon, is characterized in that concrete steps are:
(1) bagasse is placed in baking oven to dry at 80 DEG C, for subsequent use with crossing 20 mesh sieves after omnipotent crusher in crushing;
(2) in 2L beaker, add the calcium acetate solution that 250ml concentration is 0.2mol/L, then add
enter250ml concentration is 4.4mol/L ammonium acetate buffer solution, mixes, and adds 50 grams of step (1) gained bagasse, after electric stirring, by supersonic oscillations 30 minutes, leaves standstill 24 hours;
(3) in step (2) products therefrom, adding 500ml concentration is under fast stirring 0.06mol/L ammonium dihydrogen phosphate, with full-automatic titrator, under agitation, slowly add mass percent concentration be 10% ammoniacal liquor regulate reaction pH value to 7.5, stirred at ambient temperature 10 minutes;
(4) step (3) products therefrom is placed in water bath with thermostatic control upper, build glass surface ware, heating water bath, to 100 DEG C, reacts 48 hours;
(5) step (4) products therefrom is cooled naturally, filter, measure and record filtrate final ph; Solid phase precipitation thing after ultra-pure water cyclic washing twice, then uses absolute ethanol washing one time, and filter cake is placed in porcelain dish at 70 DEG C dry 16 hours, obtains hydroxyapatite/bagasse mixture;
(6) step (5) gained hydroxyapatite/bagasse mixture is carbonized at 600 DEG C, obtain hydroxyapatite/bagasse active carbon compound; Then grind, cross 100 mesh sieves, hydroxyapatite/bagasse active carbon.
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| CN110038514A (en) * | 2019-03-29 | 2019-07-23 | 山东师范大学 | A kind of nanometer hydroxyapatite dry method modification nano black carbon heavy metal absorbent and the preparation method and application thereof |
| CN110551504A (en) * | 2019-05-13 | 2019-12-10 | 北京化工大学 | Hydroxyapatite-modified biochar material and application thereof |
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| CN111495315B (en) * | 2020-04-23 | 2021-05-25 | 齐鲁工业大学 | Pb in water body2+Application and preparation method of adsorbing material |
| CN112547021A (en) * | 2020-10-27 | 2021-03-26 | 南京长三角绿色发展研究院有限公司 | Biomass-based hydroxyapatite composite material and preparation method and application thereof |
| CN114259987A (en) * | 2021-12-28 | 2022-04-01 | 辽宁大学 | Peanut shell/hydroxyapatite composite material, preparation method thereof and application thereof in Pb (II) adsorption separation |
| CN114956635B (en) * | 2022-06-15 | 2023-02-28 | 清华珠三角研究院 | Sludge pretreatment method and production system and method for manufacturing recycled aggregate |
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