CN103055803A - Preparation method of aluminum modified hydrotalcite fluoride-removal adsorbent - Google Patents

Preparation method of aluminum modified hydrotalcite fluoride-removal adsorbent Download PDF

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Publication number
CN103055803A
CN103055803A CN2012105605567A CN201210560556A CN103055803A CN 103055803 A CN103055803 A CN 103055803A CN 2012105605567 A CN2012105605567 A CN 2012105605567A CN 201210560556 A CN201210560556 A CN 201210560556A CN 103055803 A CN103055803 A CN 103055803A
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aluminate
hydrotalcite
preparation
modified hydrotalcite
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彭先佳
栾兆坤
王军
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Research Center for Eco Environmental Sciences of CAS
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Research Center for Eco Environmental Sciences of CAS
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Abstract

The invention relates to a preparation method of aluminum modified hydrotalcite fluoride-removal adsorbent. The preparation method includes the following steps: preparing hydrotalcite powder and aluminate or meta-aluminate with weight ratio of 1000: 0.27-54 into a reaction system, heating and reacting under the reaction temperature of 60-95 celsius degrees, reacting under the condition of stirring, wherein the aluminate and the meta-aluminate are calculated based on the mass of aluminum element, separating to obtain solid products after reaction is finished, watering and drying, and calcining, and preparing the modified hydrotalcite fluoride-removal adsorbent. The adsorbent which is prepared from the preparation method has a good adsorption function, can achieve that fluoride-contained water source can achieve standards of drinking water after being processed, and separation performance is good.

Description

A kind of aluminium modified hydrotalcite de-fluoridation adsorbent preparation method
Technical field
The present invention relates to a kind of aluminium modified hydrotalcite de-fluoridation adsorbent preparation method, belong to the material for water treatment field.
Background technology
In recent years, a lot of techniques have appearred in the removal for fluorine ion in the water both at home and abroad, and study hotspot focuses mostly at coagulant sedimentation, ion-exchange-resin process, electrochemical process, membrane process and absorbing process etc.
Absorbing process is that more a kind of method is used in research in the Drinking Water in China defluorination, mainly be by the equipment of fluorine adsorbent is housed with fluorinated water, because fluorine ion has different distribution coefficients in the adsorbent surface solid, liquid two-phase, thereby utilize solid matter to reach the effect of defluorination for the absorption compatibility of fluorine in the water, adsorbent then can recover adsorption capacity by regeneration.Absorption method is mainly used in processes the low concentration fluorinated water, also can be used as the deep treatment method of fluorinated water.Adsorbent can be inserted packed column, adopt the Dynamic Adsorption mode, easy and simple to handle, defluorination effect is comparatively stable, and cost is lower, has become the most widely defluorinating process of present domestic and international application.
The quality of defluorination effect mainly is subjected to the restriction of sorbing material.Sorbing material commonly used mainly comprises: contain aluminium adsorbent (such as activated alumina), carbonaceous material (such as activated carbon, bone black, CNT), biological species (such as shitosan), natural minerals class and based on some modified adsorbents that these materials are done, wherein obtaining generally sure is Defluorination of Formation Mater By Adsorption On Activated Alumina agent and material modified.But that these adsorbents exist is expensive, adsorption capacity is low or the problem such as adsorbent stripping.
Summary of the invention
Technical problem to be solved by this invention provides a kind of aluminium modified hydrotalcite de-fluoridation adsorbent preparation method, overcomes existing expensive, the defectives such as adsorption capacity is low, adsorbent stripping of de-fluoridation adsorbent.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of aluminium modified hydrotalcite de-fluoridation adsorbent preparation method may further comprise the steps:
1) hydrotalcite powder and aluminate or meta-aluminate are formulated as reaction system with the quality proportioning of 1000:0.27~54, heating also keeps reaction temperature at 60~95 ℃, react under the stirring condition, wherein said aluminate and meta-aluminate are with the Mass Calculation of aluminium element;
2) reaction is complete, separates obtaining solid product, and washing oven dry, calcining namely make the modified hydrotalcite de-fluoridation adsorbent.
The invention has the beneficial effects as follows: adopt method of the present invention to prepare adsorbent to fluorine tool good adsorption usefulness, can realize that fluorine-containing source water is treated and reach drinking water standard and separating property is good.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described hydrotalcite powder comprises the natural water talcum or/and artificial synthetic hydrotalcite.
Further, the described lower reaction time of stirring condition of step 1) is 1~10 hour.
Further, step 2) described calcining is 100~350 ℃
Further, step 2) described calcination time is 1~5 hour,
The specific embodiment
With the following Examples principle of the present invention and feature are described, institute gives an actual example and only is used for explaining the present invention, is not be used to limiting scope of the present invention.
Embodiment 1
A kind of aluminium modified hydrotalcite of the present invention de-fluoridation adsorbent preparation method, may further comprise the steps: with natural water talcum and artificial synthetic hydrotalcite and aluminate or meta-aluminate take the weight proportion of 1000:0.27 as preparing reaction system, heating also keeps reaction temperature at 60 ℃, the lower reaction time of stirring condition is 1 hour, and wherein said aluminate and meta-aluminate are with the Mass Calculation of aluminium element; React complete, separate obtaining solid product, the washing oven dry 100 ℃ of calcinings 4 hours, namely makes the modified hydrotalcite de-fluoridation adsorbent.
Embodiment 2
A kind of aluminium modified hydrotalcite of the present invention de-fluoridation adsorbent preparation method, may further comprise the steps: with natural water talcum and aluminate or meta-aluminate take the weight proportion of 1000:10 as the preparation reaction system, heating also keeps reaction temperature at 70 ℃, the lower reaction time of stirring condition is 2 hours, and wherein said aluminate and meta-aluminate are with the Mass Calculation of aluminium element); React complete, separate obtaining solid product, the washing oven dry 150 ℃ of calcinings 3 hours, namely makes the modified hydrotalcite de-fluoridation adsorbent.
Embodiment 3
A kind of aluminium modified hydrotalcite of the present invention de-fluoridation adsorbent preparation method, may further comprise the steps: with artificial synthetic hydrotalcite and aluminate or meta-aluminate take the weight proportion of 1000:1 as the preparation reaction system, heating also keeps reaction temperature at 65 ℃, the lower reaction time of stirring condition is 5 hours, and wherein said aluminate and meta-aluminate are with the Mass Calculation of aluminium element; React complete, separate obtaining solid product, the washing oven dry 250 ℃ of calcinings 2 hours, namely makes the modified hydrotalcite de-fluoridation adsorbent.
Embodiment 4
A kind of aluminium modified hydrotalcite de-fluoridation adsorbent preparation method, may further comprise the steps: with natural water talcum and artificial synthetic hydrotalcite and aluminate or meta-aluminate take the weight proportion of 1000:30 as preparing reaction system, heating also keeps reaction temperature at 80 ℃, the lower reaction time of stirring condition is 7 hours, and wherein said aluminate and meta-aluminate are with the Mass Calculation of aluminium element; React complete, separate obtaining solid product, the washing oven dry 350 ℃ of calcinings 1 hour, namely makes the modified hydrotalcite de-fluoridation adsorbent.
Embodiment 5
A kind of aluminium modified hydrotalcite of the present invention de-fluoridation adsorbent preparation method, may further comprise the steps: with natural water talcum and artificial synthetic hydrotalcite and aluminate or meta-aluminate take the weight proportion of 1000:54 as preparing reaction system, heating also keeps reaction temperature at 95 ℃, the lower reaction time of stirring condition is 9 hours, and wherein said aluminate and meta-aluminate are with the Mass Calculation of aluminium element; React complete, separate obtaining solid product, the washing oven dry 300 ℃ of calcinings 2 hours, namely makes the modified hydrotalcite de-fluoridation adsorbent.
Embodiment 6
A kind of aluminium modified hydrotalcite of the present invention de-fluoridation adsorbent preparation method, may further comprise the steps: with natural water talcum and artificial synthetic hydrotalcite and aluminate or meta-aluminate take the weight proportion of 1000:40 as preparing reaction system, heating also keeps reaction temperature at 75 ℃, the lower reaction time of stirring condition is 6 hours, and wherein said aluminate and meta-aluminate are with the Mass Calculation of aluminium element; React complete, separate obtaining solid product, the washing oven dry 200 ℃ of calcinings 3 hours, namely makes the modified hydrotalcite de-fluoridation adsorbent.
Embodiment 7
A kind of aluminium modified hydrotalcite of the present invention de-fluoridation adsorbent preparation method, may further comprise the steps: with natural water talcum and artificial synthetic hydrotalcite and aluminate or meta-aluminate take the weight proportion of 1000:35 as preparing reaction system, heating also keeps reaction temperature at 95 ℃, the lower reaction time of stirring condition is 7.5 hours, and wherein said aluminate and meta-aluminate are with the Mass Calculation of aluminium element; React complete, separate obtaining solid product, the washing oven dry 220 ℃ of calcinings 3.5 hours, namely makes the modified hydrotalcite de-fluoridation adsorbent.
Embodiment 8
A kind of aluminium modified hydrotalcite of the present invention de-fluoridation adsorbent preparation method, may further comprise the steps: with natural water talcum and artificial synthetic hydrotalcite and aluminate or meta-aluminate take the weight proportion of 1000:45 as preparing reaction system, heating also keeps reaction temperature at 95 ℃, the lower reaction time of stirring condition is 8 hours, and wherein said aluminate and meta-aluminate are with the Mass Calculation of aluminium element; React complete, separate obtaining solid product, the washing oven dry 180 ℃ of calcinings 4.5 hours, namely makes the modified hydrotalcite de-fluoridation adsorbent.
Embodiment 9
A kind of aluminium modified hydrotalcite of the present invention de-fluoridation adsorbent preparation method, may further comprise the steps: with natural water talcum and artificial synthetic hydrotalcite and aluminate or meta-aluminate take the weight proportion of 1000:5 as preparing reaction system, heating also keeps reaction temperature at 65 ℃, the lower reaction time of stirring condition is 6 hours, and wherein said aluminate and meta-aluminate are with the Mass Calculation of aluminium element; React complete, separate obtaining solid product, the washing oven dry 200 ℃ of calcinings 2.5 hours, namely makes the modified hydrotalcite de-fluoridation adsorbent.
Adopt the adsorbent Adsorption of fluoride experiment effect data of a kind of aluminium modified hydrotalcite de-fluoridation adsorbent preparation method preparation of activated alumina and embodiment 1 to 8 preparation to see Table 1.Wherein, be to be under 6.5 ± 0.1 conditions fluorine adsorption isotherm to be carried out Langmuir adsorption isotherm the Fitting Calculation to obtain with adsorbent at 20 ℃ of temperature, pH to the fluorine saturated adsorption capacity.
Comparative example: the experiment effect that adopts the activated alumina Adsorption of fluoride.
Table 1: the adsorbent adsorption effect of a kind of aluminium modified hydrotalcite de-fluoridation adsorbent preparation method preparation of activated alumina and embodiment 1 to 9 preparation relatively
Figure BDA00002624658400051
Conclusion: the de-fluoridation adsorbent defluoridation efficacy of the present invention's preparation is better than present commercially available adsorbent activity aluminium oxide.
The above only is preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (5)

1. an aluminium modified hydrotalcite de-fluoridation adsorbent preparation method is characterized in that, may further comprise the steps:
1) hydrotalcite powder and aluminate or meta-aluminate are formulated as reaction system with the weight proportion of 1000:0.27~54, heating also keeps reaction temperature at 60~95 ℃, react under the stirring condition, wherein said aluminate and meta-aluminate are with the Mass Calculation of aluminium element;
2) reaction is complete, separates obtaining solid product, and washing oven dry, calcining namely make the modified hydrotalcite de-fluoridation adsorbent.
2. described a kind of aluminium modified hydrotalcite de-fluoridation adsorbent preparation method according to claim 1 is characterized in that, the hydrotalcite powder comprises the natural water talcum or/and artificial synthetic hydrotalcite.
3. described a kind of aluminium modified hydrotalcite de-fluoridation adsorbent preparation method according to claim 1 and 2 is characterized in that the described lower reaction time of stirring condition of step 1) is 1~10 hour.
4. described a kind of aluminium modified hydrotalcite de-fluoridation adsorbent preparation method according to claim 1 and 2 is characterized in that step 2) described calcining is 100~350 ℃.
5. described a kind of aluminium modified hydrotalcite de-fluoridation adsorbent preparation method according to claim 1 and 2 is characterized in that step 2) described calcination time is 1~5 hour.
CN2012105605567A 2012-12-20 2012-12-20 Preparation method of aluminum modified hydrotalcite fluoride-removal adsorbent Pending CN103055803A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5941037A (en) * 1997-11-21 1999-08-24 W. R. Grace & Co.-Conn Oxygen scavenging hydrotalcite and compositions containing same
CN1287967A (en) * 1999-09-14 2001-03-21 北京化工大学 Surface preparation of layered dihydroxy composite metal oxide powder
CN1579937A (en) * 2003-07-31 2005-02-16 北京化工大学 Method for preparing nano-level magnesium-aluminium hydrotalcite using bittern as raw material
CN102674512A (en) * 2012-05-02 2012-09-19 中国科学院生态环境研究中心 Composite flocculant for treating anionic dye wastewater and preparation method for composite flocculant

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5941037A (en) * 1997-11-21 1999-08-24 W. R. Grace & Co.-Conn Oxygen scavenging hydrotalcite and compositions containing same
CN1287967A (en) * 1999-09-14 2001-03-21 北京化工大学 Surface preparation of layered dihydroxy composite metal oxide powder
CN1579937A (en) * 2003-07-31 2005-02-16 北京化工大学 Method for preparing nano-level magnesium-aluminium hydrotalcite using bittern as raw material
CN102674512A (en) * 2012-05-02 2012-09-19 中国科学院生态环境研究中心 Composite flocculant for treating anionic dye wastewater and preparation method for composite flocculant

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Application publication date: 20130424