CN104667874A - Preparation method of hydroxyapatite modified compound heavy metal adsorbent with eucalyptus structure - Google Patents

Preparation method of hydroxyapatite modified compound heavy metal adsorbent with eucalyptus structure Download PDF

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CN104667874A
CN104667874A CN201510086083.5A CN201510086083A CN104667874A CN 104667874 A CN104667874 A CN 104667874A CN 201510086083 A CN201510086083 A CN 201510086083A CN 104667874 A CN104667874 A CN 104667874A
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朱义年
朱宗强
曹爽
邓欢
魏彩春
赵芯
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Guilin University of Technology
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Abstract

The invention discloses a preparation method of a hydroxyapatite modified compound heavy metal adsorbent with a eucalyptus structure. By fully utilizing the advantage of a multistage porous structure of eucalyptus, the compound heavy metal adsorbent is obtained by fully changing the structural components of hydroxyapatite by an in-situ synthesis method and is applied to highly efficient adsorption purification treatment of cadmium and lead in a water environment. The method can be used for controlling micropollution caused by heavy metals in the water environment and reducing heavy metals in smelting wastewater. The method is characterized by mainly utilizing low-concentration (NH4)2HPO4 and a saturated Ca(OH)2 solution as basic liquids and adopting the in-situ synthesis technology to generate a modifier to prepare the compound heavy metal adsorbent with the eucalyptus structure. The hydroxyapatite modified compound heavy metal adsorbent with the eucalyptus structure and natural plant structure morphology is synthesized by manually controlling the preparation process. The preparation method has the beneficial effects that a cheap and environment-friendly material is provided for heavy metal pollution control; a new method and approach is provided for utilization of eucalyptus wood; and the compound heavy metal adsorbent has the advantages of good adsorption effects, wide range of application, simplicity and stability in material preparation, easier process, and the like.

Description

The preparation method of hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent
Technical field
The invention belongs to changing waste into resources to utilize and water-treatment technology field, particularly a kind of preparation method of hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent.The method utilizes hydroxyapatite for modifier, through the technology controlling and process of situ synthesis techniques, and the heavy metal composite adsorbent that to prepare with hydroxyapatite and carbon be main component.
Background technology
The toxic element that a class can be accumulated in vivo with the heavy metal that plumbous, cadmium are representative, meeting Cumulate Sum enrichment in biological chain after its entered environment, and can not be biodegradable, can hide in the environment for a long time, and enter human body serious harm life and health with food chain.Along with socioeconomic development, heavy metal pollution is in widespread attention, in current water, the minimizing technology of heavy metal mainly contains chemical precipitation method, electroflotation, ion-exchange, membrane separation process and absorption method, and wherein absorption method has the advantages such as instant effect, renewable recovery, secondary pollution probability be low and attention due to it.
The intrinsic structure of multi-level, multidimensional, many structures of wood structure to be nature through 1 years develop self-assembling formation, its structural constituent is changed by in-situ synthetic method, can prepare and both keep nature biotechnology fine structure, pass through selectively environment functional material again.
At present, the most frequently used adsorbent has activated carbon and modified cellulose etc., but mostly adsorbent is because cost is high, complex manufacturing or heavy metal are adsorbed length consuming time and limited its application.Researchers both domestic and external possess different tendency function sorbing material with different fibrous materials (as cotton, rice husk, jute, paper products etc.) for Template preparation obtains in trial.Scholar is had to utilize aminobenzenesulfonic acid, citric acid and molysite etc. to be modifier; modification is carried out to before and after wood materials charing; prepare the Carbon Materials with loose structure; material can have very strong adsorption activity through special surface process; can be applicable to water body purification; improve living environment, the fields such as environmental protection such as electromagnetic wave shielding.
Hydroxyapatite hydroxyapatite metal surface active material, it has similar chemical composition and structure to organism sclerous tissues, there is good biocompatibility and biologically active, it is good bioceramic material, but its mechanical property still has some deficits, for the manufacture of the sorbing material of the special gap structure of tool, be difficult to meet the destruction tolerances of liquid by washing away.
Eucalyptus is one of large quick growing species of trees in the world three.The cultivated area of China eucalyptus in 2010 has reached 2,670,000 hectares, and growing stock amount surpasses 6,000 ten thousand square metres, occupies third place in the world.At present paper pulp processed mainly concentrated on to the utilization of eucalyptus, make on fiber and glued board; and mainly utilize eucalyptus bodywood; eucalyptus root and branch to be abandoned or as firewood usually using upper part; these parts are as recyclability waste material; if dealt with improperly, not only can cause the wasting of resources, more can form pollution; bring pressure to environmental protection, be unfavorable for the sustainable development of ecological environment.In addition, Eucalyptus Wood has the ordered porous special anatomical structure of different scale scope, the existence of pit membrane and torus, pit is made not to be a kind of natural perforate, easily the Jin Tian soma of guide hole in timber can be removed by the pretreatment of suitable digestion agent, increase considerably the three-dimensional network waiting to try Eucalyptus Wood internal structure connective, improve later stage saturating machine, improve the network connectivty of product simultaneously, be beneficial to preparation plant templated porous sorbing material.
Summary of the invention
The object of this invention is to provide a kind of preparation method of hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent.To obtained adsorbent carry out thing phase with structure, become to be grouped into and shape characteristic Experimental Characterization, and be applied to the adsorption treatment of water environment common heavy metal element, for Heavy Metal Pollution Control provides a kind of cheapness and eco-friendly material, provide a kind of new method, new way for Eucalyptus Wood utilizes.
The thinking of the inventive method: with low concentration (NH 4) 2hP0 4with saturated Ca (OH) 2liquid based on solution, situ synthesis techniques is adopted to generate modifier, preparation obtains Eucalyptus structure composite heavy metal absorbent, and by Artificial Control preparation technology, synthesis has the hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent of natural plants structural form.
Concrete steps are:
(1) by eucalyptus root or the peeling of limb timber, dry.
(2) dose volume concentration is that the weak aqua ammonia of 5 ~ 8% is as digestion agent.
(3) (the NH of 0.02 ~ 0.05mo1/L is prepared respectively 4) 2hP0 4solution and saturated Ca (OH) 2solution is as fabricated in situ basal liquid.
(4) product that step (1) obtains is placed in the digestion agent that step (2) obtains, under 100 ~ 110 DEG C of conditions, digestion 6 ~ 8 hours, completes extracting pretreatment.
(5) product ultra-pure water step (4) obtained is cleaned, and is roasting 3 ~ 4 hours in the Muffle furnace of 400 ~ 500 DEG C in temperature, and stove is chilled to room temperature.
(6) product that step (5) obtains is immersed in the saturated Ca (OH) that step (3) obtains 2in solution, and 25 ~ 35 DEG C of water-bath inside holding 24 ~ 48 hours.
(7) by (NH that the product that step (6) obtains obtains in step (3) 4) 2hP0 4soak 2 hours in solution, then taking-up product is immersed in the saturated Ca (OH) that step (3) obtains 2solution 2 hours, sample all uses ultrapure water 19 ~ 21 seconds after each immersion, and is placed in 50 DEG C of drying in oven 2 hours.
(8) step (7) four times are repeated.
(9) product that step (8) obtains is ground, cross 100 ~ 150 mesh sieves, be i.e. obtained hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent.
The inventive method is simple for process, preparation process low cost, and owing to utilizing Eucalyptus Wood, lime stone etc. to be main raw material(s), material is easy to get, and through technology controlling and process, substantially increases the absorption property of material heavy metal; The product of gained can be widely used in heavy metal pollution water treatment.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram (FI-IR) of the hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent that the embodiment of the present invention obtains.
Fig. 2 is the X-ray diffractogram (XRD) of the hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent that the embodiment of the present invention obtains.
Fig. 3 is the SEM microscopy figure (SEM, × 100 times) of the hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent that the embodiment of the present invention obtains.
Fig. 4 is the SEM microscopy figure (SEM, × 1000 times) of the hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent that the embodiment of the present invention obtains.
Fig. 5 is that the obtained hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent of the embodiment of the present invention is to the Adsorption Effect variation diagram of three kinds of variable concentrations cadmiums (II) in different initial pH value Water Under solution.
Fig. 6 is that the obtained hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent of the embodiment of the present invention is to the Adsorption Effect variation diagram of different dosage to three kinds of lead at different concentrations (II) in the aqueous solution.
Detailed description of the invention
embodiment:
One, the preparation of hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent
(1) removed the peel by eucalyptus root timber 1kg, after dry, cut lengths are about: the blocks of length × wide × height=30mm × 10mm × 3mm.
(2) dose volume concentration is that the weak aqua ammonia of 5% is as digestion agent.
(3) (the NH of 0.02mo1/L is prepared respectively 4) 2hP0 4solution and saturated Ca (OH) 2solution is as fabricated in situ basal liquid.
(4) product that step (1) obtains is placed in the digestion agent that step (2) obtains, under 105 DEG C of conditions, digestion 7 hours, completes extracting pretreatment.
(5) the product ultra-pure water that step (4) obtains is cleaned, and be roasting 3 hours in the Muffle furnace of 500 DEG C in temperature, and stove is chilled to room temperature.
(6) product that step (5) obtains is immersed in the saturated Ca (OH) that step (3) obtains 2in solution, and 25 DEG C of water-bath inside holding 48 hours.
(7) by (NH that the product that step (6) obtains obtains in step (3) 4) 2hP0 4soak 2 hours in solution, then taking-up product is immersed in the saturated Ca (OH) that step (3) obtains 2solution 2 hours, sample all uses ultrapure water 20 seconds after each immersion, and is placed in 50 DEG C of drying in oven 2 hours.
(8) step (7) four times are repeated.
(9) product that step (8) obtains is ground, cross 100 ~ 150 mesh sieves, be i.e. obtained hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent.
The thing phase of the hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent that the present embodiment is obtained and structure, become to be grouped into and shape characteristic adopts X-ray diffractometer (XRD, X'Pert PRO), ftir Analysis is used in conjunction system (STA-449C; 470 FT-IR) energy disperse spectroscopy and SEM (SEM, JSM-6380LV) carry out observation test, specifically sees Figure of description 1,2,3 and 4.
Two, heavy metal absorbent is to the adsorption effect of cadmium (II)
(1) CdNO is used 3(analyzing pure) compound concentration is each 8 bottles of cadmium (II) the pending liquid of 5mg/L, 10mg/L and 50mg/L, uses HNO 3respectively the pH value of pending liquid is adjusted to 1.0,2.0,3.0,4.0,5.0,6.0,7.0 and 8.0 with NaOH.
(2) the pending liquid numbering pipetting 50ml step (1) respectively obtained is bottled for subsequent use in 100ml centrifuge tube.
(3) the hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent that 0.1g the present embodiment is obtained is added in the pending liquid of step (2) centrifuge tube for subsequent use respectively, seal 25 DEG C of constant temperature oscillations that laggard line of hitch oscillator frequency is 150r/min, duration of oscillation is 6 hours.
(4) product getting step (3) crosses 0.22 μm of miillpore filter, use cadmium (II) concentration of Flame Atomic Absorption Spectrometry Determination remnants, obtaining product under pH value is 1.0,2.0,3.0,4.0,5.0,6.0,7.0 and 8.0 conditions is the pending liquid adsorption effect of cadmium (II) of 5mg/L, 10mg/L and 50mg/L to concentration, as shown in Figure 4.
Three, heavy metal absorbent is to the adsorption effect of plumbous (II)
(1) Pb (NO is used 3) 2(top grade is pure) compound concentration is each 10 bottles of lead (II) the pending liquid of 5mg/L, 10mg/L and 50mg/L, uses HNO 3with NaOH, the pH value of pending liquid is adjusted to 5.0.
(2) the pending liquid numbering pipetting 50ml step (1) respectively obtained is bottled for subsequent use in 100ml centrifuge tube.
(3) 0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9 and the obtained hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent of 1.0g the present embodiment is added in the pending liquid of step (2) centrifuge tube for subsequent use respectively, seal 25 DEG C of constant temperature oscillations that laggard line of hitch oscillator frequency is 150r/min, duration of oscillation is 6 hours.
(4) product getting step (3) crosses 0.22 μm of miillpore filter, use lead (II) concentration of Flame Atomic Absorption Spectrometry Determination remnants, obtain adsorbent dosage be 0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9 and 1.0g condition under product be the pending liquid adsorption effect of lead (II) of 5mg/L, 10mg/L and 50mg/L to concentration, as shown in Figure 5.

Claims (1)

1. a preparation method for hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent, is characterized in that concrete steps are:
(1) by eucalyptus root or the peeling of limb timber, dry;
(2) dose volume concentration is that the weak aqua ammonia of 5 ~ 8% is as digestion agent;
(3) (the NH of 0.02 ~ 0.05mo1/L is prepared respectively 4) 2hP0 4solution and saturated Ca (OH) 2solution is as fabricated in situ basal liquid;
(4) product that step (1) obtains is placed in the digestion agent that step (2) obtains, under 100 ~ 110 DEG C of conditions, digestion 6 ~ 8 hours, completes extracting pretreatment;
(5) product ultra-pure water step (4) obtained is cleaned, and is roasting 3 ~ 4 hours in the Muffle furnace of 400 ~ 500 DEG C in temperature, and stove is chilled to room temperature;
(6) product that step (5) obtains is immersed in the saturated Ca (OH) that step (3) obtains 2in solution, and 25 ~ 35 DEG C of water-bath inside holding 24 ~ 48 hours;
(7) by (NH that the product that step (6) obtains obtains in step (3) 4) 2hP0 4soak 2 hours in solution, then taking-up product is immersed in the saturated Ca (OH) that step (3) obtains 2solution 2 hours, sample all uses ultrapure water 19 ~ 21 seconds after each immersion, and is placed in 50 DEG C of drying in oven 2 hours;
(8) step (7) four times are repeated;
(9) product that step (8) obtains is ground, cross 100 ~ 150 mesh sieves, be i.e. obtained hydroxyapatite modified Eucalyptus structure composite heavy metal absorbent.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106111067A (en) * 2016-07-27 2016-11-16 中国科学院新疆理化技术研究所 A kind of preparation method and application of silane coupler modified magnetic halloysite material
CN106268634A (en) * 2016-08-09 2017-01-04 江苏陆博环保科技有限公司 Preparation method for the inorganic compound particles of effluent containing heavy metal ions advanced treating
CN108636339A (en) * 2018-04-26 2018-10-12 桂林理工大学 The preparation method of hydroxyapatite modified moso bamboo structure composite heavy metal absorbent
CN111229156A (en) * 2020-01-20 2020-06-05 齐鲁工业大学 Preparation and application of hydroxyapatite modified mesoporous silica adsorption material
CN111495315A (en) * 2020-04-23 2020-08-07 齐鲁工业大学 Pb in water body2+Application and preparation method of adsorbing material
WO2021007986A1 (en) * 2019-07-12 2021-01-21 华南理工大学 Carboxylated banyan aerial root fiber adsorbent and preparation method therefor and application thereof

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CN102258976A (en) * 2011-05-20 2011-11-30 桂林理工大学 Preparation method of eucalyptus biomorphic Fe2O3/Fe3O4 composite heavy metal adsorbent
CN102380350A (en) * 2011-10-24 2012-03-21 上海海洋大学 Method for removing hydroxyapatite modified eggshell adsorbent material and recycling phosphate from wastewater
CN102895957A (en) * 2012-11-11 2013-01-30 桂林理工大学 Preparation method of moso bamboo biomorphic Fe2O3/Fe3O4 compound heavy metal absorbent
CN103861567A (en) * 2014-03-21 2014-06-18 桂林理工大学 Preparation method of hydroxyapatite/bagasse active carbon

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EP0342932A1 (en) * 1988-05-16 1989-11-23 MITSUI TOATSU CHEMICALS, Inc. Solid support and column for liquid chromatography
CN102258976A (en) * 2011-05-20 2011-11-30 桂林理工大学 Preparation method of eucalyptus biomorphic Fe2O3/Fe3O4 composite heavy metal adsorbent
CN102380350A (en) * 2011-10-24 2012-03-21 上海海洋大学 Method for removing hydroxyapatite modified eggshell adsorbent material and recycling phosphate from wastewater
CN102895957A (en) * 2012-11-11 2013-01-30 桂林理工大学 Preparation method of moso bamboo biomorphic Fe2O3/Fe3O4 compound heavy metal absorbent
CN103861567A (en) * 2014-03-21 2014-06-18 桂林理工大学 Preparation method of hydroxyapatite/bagasse active carbon

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106111067A (en) * 2016-07-27 2016-11-16 中国科学院新疆理化技术研究所 A kind of preparation method and application of silane coupler modified magnetic halloysite material
CN106111067B (en) * 2016-07-27 2018-10-26 中国科学院新疆理化技术研究所 A kind of preparation method and application of silane coupler modified magnetic halloysite material
CN106268634A (en) * 2016-08-09 2017-01-04 江苏陆博环保科技有限公司 Preparation method for the inorganic compound particles of effluent containing heavy metal ions advanced treating
CN108636339A (en) * 2018-04-26 2018-10-12 桂林理工大学 The preparation method of hydroxyapatite modified moso bamboo structure composite heavy metal absorbent
CN108636339B (en) * 2018-04-26 2021-05-25 桂林理工大学 Preparation method of hydroxyapatite modified moso bamboo structure composite heavy metal adsorbent
WO2021007986A1 (en) * 2019-07-12 2021-01-21 华南理工大学 Carboxylated banyan aerial root fiber adsorbent and preparation method therefor and application thereof
CN111229156A (en) * 2020-01-20 2020-06-05 齐鲁工业大学 Preparation and application of hydroxyapatite modified mesoporous silica adsorption material
CN111229156B (en) * 2020-01-20 2021-07-13 齐鲁工业大学 Preparation and application of hydroxyapatite modified mesoporous silica adsorption material
CN111495315A (en) * 2020-04-23 2020-08-07 齐鲁工业大学 Pb in water body2+Application and preparation method of adsorbing material
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

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