CN103120926A - Method for improving water fluorine adsorbing capacity of activated alumina through microwave modification - Google Patents
Method for improving water fluorine adsorbing capacity of activated alumina through microwave modification Download PDFInfo
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- CN103120926A CN103120926A CN2011103702303A CN201110370230A CN103120926A CN 103120926 A CN103120926 A CN 103120926A CN 2011103702303 A CN2011103702303 A CN 2011103702303A CN 201110370230 A CN201110370230 A CN 201110370230A CN 103120926 A CN103120926 A CN 103120926A
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Abstract
The invention relates to a method for improving water fluorine adsorbing performance of activated alumina subjected to microwave modification. The modification method comprises the following steps of: a, dipping activated alumina to a 1-2 mol/L NaCl solution according to a solid-to-liquid ratio of 1:2, and shaking the solution at an intermediate speed for 24h at a normal temperature or performing water bath on the solution at a high temperature (being greater than or equal to 80 DEG C) for 3h; b, repeatedly washing the obtained solution by purified water for 6-7 times until no milky white suspension occurs, and drying the obtained product for 24h at 120 DEG C; c, uniformly laying the processed activated alumina in a glassware (the thickness of which is less than or equal to 6mm), and heating the glassware with high fire (at microwave output power of 800W) in a microwave oven for 10 minutes; and d, cooling the activated alumina taken out of the microwave oven at a normal temperature to obtain the microwave modified activated alumina. The modification method provided by the invention has the advantages of simplicity and safety of operation, low manufacturing cost, short period and obvious effect.
Description
Technical field
The invention belongs to the optimisation technique field of the de-fluoridation adsorbent in water treatment procedure.Method is simple, safety, and exploitativeness is strong, and is with low cost, is applicable to laboratory operation, can further explore commercial production conditions.
Background technology
In China's drinking water standard (GB5749-2006) regulation drinking water, fluorinated volume must not surpass 1mg/L.Human body long-term drinking high-fluorine water can cause fluorine poisoning, shows as fluorine dental plaque, fluorosis of bone.The absorption method defluorination is the most widely used method of present water treatment defluorination process, and adsorbent mainly contains activated alumina, bone black and zeolite, and wherein, activated alumina is used widely with its good adsorption capacity and mechanical performance.Common industrial activated alumina defluorination finite capacity carries out modification through certain method to it, can greatly improve its Fluoride-Absorption Capacity.
The Wang Peng of Harbin Institute of Technology (number of patent application 200410013583.8), (number of patent applications 200710052639.4) such as the Zhang Huiling of Wuhan University Of Technology is combined commercial alumina with microwave technique, improve its catalytic performance.The Li Zhenyu of Tsing-Hua University, Sun Qing etc., utilize microwave method to prepare activated magnesia in the laboratory, static defluorination capacity is 13.11-13.29mg/g (Li Zhenyu, Deng. microwave irradiation prepares the experimental study [J] of activated magnesia defluorinating agent, inorganic chemicals industry, 2009,11 (4): 11-14).At present, in water treatment field, also rarely found with the bibliographical information that improves its Fluoride-Absorption Capacity about utilizing the microwave modification activated alumina.
Summary of the invention
The object of the present invention is to provide a kind of activated alumina method of modifying simple to operate, easy to implement, cheap, with short production cycle, to improve the ability of fluorine ion in its adsorbed water.
In order to realize above-mentioned target, the method for modifying of activated alumina is as follows: a. takes the industrial activated alumina that the 50g particle diameter is 1-3mm, by solid-to-liquid ratio 1: 2, impregnated in the 100mL pure water, puts into shaking table, and it is 150rpm that rotating speed is set, and shakes 24h under 30 ℃; B. repeatedly rinses 6-7 time with pure water after taking out, until the appearance of agalasisa white suspension thing is placed in baking oven, dry 24h under 120 ℃; C. the activated alumina uniform spreading after getting 10g and processing is placed in the high fire heating of micro-wave oven 10 minutes in culture dish; D. take out, normal temperature is cooling, namely obtains pure water dipping-microwave modification activated alumina.
Perhaps step is: a. takes the industrial activated alumina that the 50g particle diameter is 1-3mm, and by solid-to-liquid ratio 1: 2, impregnated in 100mL concentration was in the NaCl solution of 0.5-6mol/L, puts into shaking table, and it is 150rpm that rotating speed is set, and shakes 24h under 30 ℃; B. repeatedly rinses 6-7 time with pure water after taking out, until the appearance of agalasisa white suspension thing is placed in baking oven, dry 24h under 120 ℃; C. get 10g with 1 or 2mol/L NaCl solution-treated after the activated alumina uniform spreading in culture dish, be placed in the high fire heating of micro-wave oven 10 minutes; D. take out, normal temperature is cooling, namely obtains NaCl dipping-microwave modification activated alumina.
Perhaps step is: a. takes the industrial activated alumina that the 50g particle diameter is 1-3mm, presses solid-to-liquid ratio 1: 2, and impregnated in 100mL concentration is in the NaCl solution of 1mol/L, puts into water-bath and heats 3h, and bath temperature is 40 ℃, 60 ℃, 80 ℃; B. repeatedly rinses 6-7 time with pure water after taking out, until the appearance of agalasisa white suspension thing is placed in baking oven, dry 24h under 120 ℃; C. get activated alumina uniform spreading after 80 ℃ of processing of 10g in culture dish, be placed in the high fire heating of micro-wave oven 10 minutes; D. take out, normal temperature is cooling, namely obtains NaCl water-bath-microwave modification activated alumina.
The micro-wave oven model of using is the KJ23C-AN2 of U.S..The instrument design parameter is: rated input power 1300W, microwave output power 800W, microwave operational frequencies 2450MHz, roasting power 1000W.Adopt the high fire screen of micro-wave oven in the present invention.
Method for optimizing is: a. takes the industrial activated alumina that the 50g particle diameter is 1-3mm, and by solid-to-liquid ratio 1: 2, impregnated in 100mL concentration was in the NaCl solution of 2mol/L, shakes 24h under 30 ℃; B. repeatedly rinses 6-7 time with pure water after taking out, until the appearance of agalasisa white suspension thing is placed in baking oven, dry 24h under 120 ℃; C. the activated alumina uniform spreading after getting 10g and processing is placed in the high fire heating of micro-wave oven 10 minutes in culture dish; D. take out, normal temperature is cooling, namely obtains 2mol/L NaCl dipping-microwave modification activated alumina.
Activated alumina is a kind of white spherical material of porous, and specific area is large, has defect lattice.Industrial, often be used to catalyst, decolorizer, drier etc.Water treatment field, activated alumina are most widely used defluorinating agents.Its defluorination principle is considered to two aspects usually: the one, and huge surface area, the duct inner surface of special tool; The 2nd, lattice defect.It carries out modification common available aluminium salt, molysite, manganese salt pair, but cost is quite high, and may cause the problem of heavy metal secondary pollution.Use NaCl to carry out modification to activated alumina in the present invention, obtained certain effect, then used micro-wave oven to its further modification.By test data as can be known, use microwave modification can improve activated alumina to the adsorbance of fluorine.What wherein defluorination effect was best is combination " 2mol/L NaCl dipping-microwave modification activated alumina ", and activated alumina is through modification, and its 3h adsorbance can improve 89.6%, 24h adsorbance can improve 48.5%; What defluorination effect took second place is combination " 1mol/L NaCl, 80 ℃ of water-bath-microwave modification activated aluminas ", and its 3h adsorbance can improve 69.2%, 24h adsorbance can improve 42.2%.
Description of drawings
Fig. 1 is the adsorbance contrast of activated alumina to fluorine under different method of modifying.Wherein, the main modifying process of embodiment 1-13 is described as follows:
1---microwave 10min;
2---0.5mol/L NaCl, concussion 24h;
3---1mol/L NaCl, concussion 24h;
4---2mol/L NaCl, concussion 24h;
5---4mol/L NaCl, concussion 24h;
6---6mol/L NaCl, concussion 24h;
7---1mol/L NaCl, concussion 24h, microwave 10min;
8---2mol/L NaCl, concussion 24h, microwave 10min;
9---1mol/L NaCl, 40 ℃ of water-bath 3h;
10---1mol/L NaCl, 60 ℃ of water-bath 3h;
11---1mol/L NaCl, 80 ℃ of water-bath 3h;
12---1mol/LNaCl, 80 ℃ of water-bath 3h, microwave 10min;
13---without special modified measures.
The specific embodiment
A kind of method of microwave modification activated alumina: a. takes the industrial activated alumina that the 50g particle diameter is 1-3mm, by solid-to-liquid ratio 1: 2, impregnated in the 100mL pure water, puts into shaking table, and it is 150rpm that rotating speed is set, and shakes 24h under 30 ℃; B. repeatedly rinses 6-7 time with pure water after taking out, until the appearance of agalasisa white suspension thing is placed in baking oven, dry 24h under 120 ℃; C. the activated alumina uniform spreading after getting 10g and processing is placed in the high fire heating of micro-wave oven 10 minutes in culture dish; D. take out, normal temperature is cooling, namely obtains pure water dipping-microwave modification activated alumina.
A kind of method of NaCl modified activated aluminum oxide: a. takes the industrial activated alumina that the 50g particle diameter is 1-3mm, pressed solid-to-liquid ratio 1: 2, impregnated in 100mL concentration is in the NaCl solution of 0.5mol/L, puts into shaking table, it is 150rpm that rotating speed is set, and shakes 24h under 30 ℃; B. repeatedly rinses 6-7 time with pure water after taking out, until the appearance of agalasisa white suspension thing is placed in baking oven, dry 24h under 120 ℃; C. take out, normal temperature is cooling, namely obtains 0.5mol/L NaCl dipping modified activated aluminum oxide.
A kind of method of NaCl modified activated aluminum oxide: except the NaCl solution with the 0.5mol/L in 1mol/L NaCl solution replacement embodiment 2, other are identical with embodiment 2.
A kind of method of NaCl modified activated aluminum oxide: except the NaCl solution with the 0.5mol/L in 2mol/L NaCl solution replacement embodiment 2, other are identical with embodiment 2.
Embodiment 5
A kind of method of NaCl modified activated aluminum oxide: except the NaCl solution with the 0.5mol/L in 4mol/L NaCl solution replacement embodiment 2, other are identical with embodiment 2.
Embodiment 6
A kind of method of NaCl modified activated aluminum oxide: except the NaCl solution with the 0.5mol/L in 6mol/L NaCl solution replacement embodiment 2, other are identical with embodiment 2.
Embodiment 7
A kind of method of NaCl-microwave modification activated alumina: get the activated alumina 10g that embodiment 3 processed, uniform spreading is on culture dish, and the high fire of micro-wave oven heated 10 minutes.
Embodiment 8
A kind of method of NaCl-microwave modification activated alumina: get the activated alumina 10g that embodiment 4 processed, uniform spreading is on culture dish, and the high fire of micro-wave oven heated 10 minutes.
Embodiment 9
A kind of method of heating water bath modified activated aluminum oxide: a. takes the industrial activated alumina that the 50g particle diameter is 1-3mm, presses solid-to-liquid ratio 1: 2, and impregnated in 100mL concentration is in the NaCl solution of 1mol/L, puts into water-bath and heats 3h, and bath temperature is 40 ℃; B. repeatedly rinses 6-7 time with pure water after taking out, until the appearance of agalasisa white suspension thing is placed in baking oven, dry 24h under 120 ℃; C. get activated alumina uniform spreading after 80 ℃ of processing of 10g in culture dish, be placed in the high fire heating of micro-wave oven 10 minutes; D. take out, normal temperature is cooling, namely obtains NaCl water-bath-microwave modification activated alumina.
A kind of method of heating water bath modified activated aluminum oxide: except 40 ℃ that replace in embodiment 9 with 60 ℃, other are identical with embodiment 9.
A kind of method of heating water bath modified activated aluminum oxide: except 40 ℃ that replace in embodiment 9 with 80 ℃, other are identical with embodiment 9.
The method of a kind of NaCl water-bath-microwave modification activated alumina: get the activated alumina 10g that embodiment 11 processed, uniform spreading is on culture dish, and the high fire of micro-wave oven heated 10 minutes.
Unmodified activated alumina preparation method: a. takes the industrial activated alumina that the 50g particle diameter is 1-3mm, by solid-to-liquid ratio 1: 2, impregnated in the 100mL pure water, puts into shaking table, and it is 150rpm that rotating speed is set, and shakes 24h under 30 ℃; B. repeatedly rinses 6-7 time with pure water after taking out, until the appearance of agalasisa white suspension thing is placed in baking oven, dry 24h under 120 ℃; C. take out, normal temperature is cooling, namely obtains pure water-microwave modification activated alumina.
Confirmatory experiment: the activated alumina of preparing with specific embodiment 1-13 carries out the fluoride waste experiment, and step is as follows.
1, laboratory apparatus
Hua Lida HZ-2111KB constant temperature oscillator (granary, Jiangsu Hua Lida experimental facilities Co., Ltd), electric drying oven with forced convection (Shanghai Yiheng Scientific Instruments Co., Ltd), phoenix FOO1508 type fluoride ion selective electrode (U.S. VanLondon-pHoenix), Hana HI98185A type pH/ORP/ISE instrument (Italian HANNA)
2, experiment material
The activated alumina of embodiment 1-13, the fluorinated water of 10mg/L are (in F-, KF standard reserving solution with 1000ppm, dilution obtains), TISAB I (230mL acetic acid, 232g NaCl, 16g CDTA, 150g NaOH are settled to 4L, and are 5.25 with 5mol/L NaOH adjusting pH)
3, experimental procedure
Take the 1g activated alumina, be placed in the plastic bottle of 200mL, add the 100mL10mg/L fluorinated water, be placed in 30 ℃ of isothermal vibrations of shaking table, 3h and 24h sampling, measure wherein F-concentration after the reaction beginning.The adsorbance q of calculated activity aluminium oxide to fluorine according to the following formula
t(mg/kg):
q
t＝(C
0-C
t)V/m
Wherein, C
0---F-concentration in solution before reaction is 10mg/L
Ct---F-concentration in etching solution during t, unit is mg/L
V---liquor capacity is 0.1L
M---adsorbent mass is 0.001kg
Therefore following formula can be written as:
q
t＝(10-C
t)×100
q
t：mg/kg
4, experimental result
The adsorbance contrast of various modified activated aluminum oxides as shown in Figure 1.As can be seen from Figure 1, used the embodiment 1 of microwave modification, 8, No. 12 methods, gained modified activated aluminum oxide absorption F-best results, and associative list 1 can find out that the raising of 3h adsorbance is respectively 66.9%, 89.6%, 69.2%.Therefore, modification embodiment 8 is optimum implementation, and 8 or 12 all can be used as alternative.
The contrast of defluorination adsorbance after the modification of table 1 activated alumina
* annotate: in table, data calculate with comparative example 13, i.e. defluorination adsorbance before and after modification increases percentage, and computing formula is as follows
Percentage=(q
it-q
13t)/q
13t
q
itBe the activated alumina t adsorbance constantly of embodiment 1-12, i=1-12, t=3h or 24h;
q
13tBe activated alumina (unmodified) the t adsorbance constantly of embodiment 13, t=3h or 24h.
Claims (6)
1. the method for a microwave modification activated alumina, it is characterized in that its modification procedure is: a. impregnated in activated alumina in pure water or NaCl solution by solid-to-liquid ratio at 1: 2, middling speed concussion 24h or heating water bath 3h under normal temperature; B. repeatedly rinses 6-7 time with pure water after taking out, until the appearance of agalasisa white suspension thing, dry 24h under 120 ℃; C. the activated alumina uniform spreading after processing is placed in the high fire heating of micro-wave oven 10 minutes in glassware; D. take out, normal temperature is cooling, namely obtains the microwave modification activated alumina.
2. the method for microwave modification activated alumina according to claim 1, the design parameter that it is characterized in that preparation process is: a. takes the industrial activated alumina that the 50g particle diameter is 1-3mm, pressed solid-to-liquid ratio 1: 2, impregnated in the 100mL pure water, put into shaking table, it is 150rpm that rotating speed is set, and shakes 24h under 30 ℃; B. repeatedly rinses 6-7 time with pure water after taking out, until the appearance of agalasisa white suspension thing is placed in baking oven, dry 24h under 120 ℃; C. the activated alumina uniform spreading after getting 10g and processing is placed in the high fire heating of micro-wave oven 10 minutes in culture dish; D. take out, normal temperature is cooling, namely obtains pure water dipping-microwave modification activated alumina.
3. the method for microwave modification activated alumina according to claim 1, the design parameter that it is characterized in that preparation process is: a. takes the industrial activated alumina that the 50g particle diameter is 1-3mm, pressed solid-to-liquid ratio 1: 2, impregnated in 100mL concentration is in the NaCl solution of 0.5-6mol/L, put into shaking table, it is 150rpm that rotating speed is set, and shakes 24h under 30 ℃; B. repeatedly rinses 6-7 time with pure water after taking out, until the appearance of agalasisa white suspension thing is placed in baking oven, dry 24h under 120 ℃; C. get the activated alumina uniform spreading of 10g after with 1-2mol/L NaCl solution-treated in culture dish, be placed in the high fire heating of micro-wave oven 10 minutes; D. take out, normal temperature is cooling, namely obtains NaCl dipping-microwave modification activated alumina.
4. the method for microwave modification activated alumina according to claim 1, the design parameter that it is characterized in that preparation process is: a. takes the industrial activated alumina that the 50g particle diameter is 1-3mm, pressed solid-to-liquid ratio 1: 2, impregnated in 100mL concentration is in the NaCl solution of 1mol/L, put into water-bath and heat 3h, bath temperature is respectively 40 ℃, 60 ℃, 80 ℃; B. repeatedly rinses 6-7 time with pure water after taking out, until the appearance of agalasisa white suspension thing is placed in baking oven, dry 24h under 120 ℃; C. get activated alumina uniform spreading after 80 ℃ of processing of 10g in culture dish, be placed in the high fire heating of micro-wave oven 10 minutes; D. take out, normal temperature is cooling, namely obtains NaCl water-bath-microwave modification activated alumina.
5. according to claim 1,2,3,4 described micro-wave oven models are beautiful KJ23C-AN2, the instrument design parameter is: rated input power 1300W, microwave output power 800W, microwave operational frequencies 2450MHz, roasting power 1000W.Adopt the high fire screen of micro-wave oven in the present invention.
6. 2,3, the 4 described methods of utilizing the microwave modification activated alumina according to claim 1,, the method for optimizing that it is characterized in that it is: a. takes the industrial activated alumina that the 50g particle diameter is 1-3mm, pressed solid-to-liquid ratio 1: 2, impregnated in 100mL concentration is in the NaCl solution of 2mol/L, shakes 24h under 30 ℃; B. repeatedly rinses 6-7 time with pure water after taking out, until the appearance of agalasisa white suspension thing is placed in baking oven, dry 24h under 120 ℃; C. the activated alumina uniform spreading after getting 10g and processing is placed in the high fire heating of micro-wave oven 10 minutes in culture dish; D. take out, normal temperature is cooling, namely obtains 2mol/L NaCl dipping-microwave modification activated alumina.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103537254A (en) * | 2013-11-08 | 2014-01-29 | 天津工业大学 | Basalt fiber felt-loaded aluminum oxide defluorination and adsorption material and preparation method thereof |
| CN108341440A (en) * | 2018-03-02 | 2018-07-31 | 北京利华消防工程有限公司 | The method of water treatment agent, preparation method and water treatment agent processing fire demand water |
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| JPS5230054A (en) * | 1975-08-30 | 1977-03-07 | Nikkei Giken:Kk | Method of removing fluorine in waste water |
| CN1559670A (en) * | 2004-02-26 | 2005-01-05 | 哈尔滨工业大学 | Preparation method of modified aluminium oxide catalyst used in micro wave induced oxidation process |
| CN101116819A (en) * | 2007-07-05 | 2008-02-06 | 武汉科技大学 | Microwave inducing catalyst and method for preparing the same |
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2011
- 2011-11-21 CN CN2011103702303A patent/CN103120926A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5230054A (en) * | 1975-08-30 | 1977-03-07 | Nikkei Giken:Kk | Method of removing fluorine in waste water |
| CN1559670A (en) * | 2004-02-26 | 2005-01-05 | 哈尔滨工业大学 | Preparation method of modified aluminium oxide catalyst used in micro wave induced oxidation process |
| CN101116819A (en) * | 2007-07-05 | 2008-02-06 | 武汉科技大学 | Microwave inducing catalyst and method for preparing the same |
Non-Patent Citations (1)
| Title |
|---|
| ERIC DADUSH, ET AL.: "Microwave activation of alumina and its use as a catalyst in synthetic reactions", 《JOURNAL OF CHEMICAL RESEARCH》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103537254A (en) * | 2013-11-08 | 2014-01-29 | 天津工业大学 | Basalt fiber felt-loaded aluminum oxide defluorination and adsorption material and preparation method thereof |
| CN108341440A (en) * | 2018-03-02 | 2018-07-31 | 北京利华消防工程有限公司 | The method of water treatment agent, preparation method and water treatment agent processing fire demand water |
| CN108341440B (en) * | 2018-03-02 | 2021-02-23 | 北京利华消防工程有限公司 | Water treatment agent, preparation method and method for treating fire-fighting water by using water treatment agent |
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Application publication date: 20130529 |