CN104096547B - A kind of efficiently humic acid fluorine ion absorber - Google Patents
A kind of efficiently humic acid fluorine ion absorber Download PDFInfo
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Abstract
The invention discloses a kind of efficiently humic acid fluorine ion absorber, its raw material to include by weight：35 38 parts of humic acid, 45 parts of iron chloride, 28 32 parts of aluminium chloride, 45 parts of manganese chloride, 68 72 parts of zirconium chloride, 7 10 parts of calcium chloride, 49 52 parts of mixed coal powder, 55 60 parts of sodium hydroxide solution.Iron-aluminum-manganese zirconium calcium mixed solution is obtained by zirconium chloride, iron chloride, aluminium chloride, manganese chloride, calcium chloride are soluble in water successively, humic acid addition sodium hydroxide solution is obtained into alkaline sodium humate solution, stir alkaline sodium humate solution and add iron-aluminum-manganese zirconium calcium mixed solution, adjustment pH value carries out being filtrated to get solid mixture；After solid mixture is washed, heating high-pressure drying obtains metal oxide-humic complex；Mixed coal powder and metal oxide-humic complex are stirred to obtain efficient humic acid fluorine ion absorber.Raw material sources of the present invention are extensive, and preparation technology is simple, and adsorption capacity is high, and fluorine removing rate is high, so as to substantially reduce cost.
Description
Technical field
The present invention relates to fluorine ion adsorption technology field, more particularly to a kind of efficiently humic acid fluorine ion absorber.
Background technology
A kind of fluorine trace element essential as human body, appropriate fluorine can not only take care of one's teeth, and to bone
Formation and metabolism play the role of important reduction carious tooth incidence, excitability conduction, alcium and phosphor metabolization also to nervous system, first shape
Gland function, cell enzyme system and reproductive process are all helpful.But the fluorine of long-term excess intake can produce various fluorine poisoning symptoms,
Den tal fluorosis, fluorosis of bone, meat fiber may be caused to degenerate, or even osteocarcinoma.Therefore, the intake of fluorine is strictly controlled to health
It is significant.
At present, high-fluorine water purification method mainly has absorption method, the precipitation method, membrane separation process, electrocoagulation, ion-exchange
Deng absorption method has the advantages that simple to operate, cost is cheap, is conveniently easy to get so that absorption method is suitable for scattered high-fluorine water source
The removal of fluorine, the economical and effective the most in numerous drinking water defluorination methods.But traditional adsorbent such as activated alumina etc. is deposited
In the problem such as adsorption capacity is low, practical application is influenceed.
Humic acid is the polymer that nature is widely present, and it has the property of colloid and loose " sponge
Shape " structure, it is set to produce huge surface area and surface energy., can be with containing hydroxyl, carboxyl isoreactivity group in humic acid molecule
Ion exchange, complex reaction and adsorption effect occur for underwater gold category ion, and hydrogen bond also occurs with the stronger material of electronegativity
Suction-operated.In addition, humic acid is also easy to produce gelling under pH reductions or additional electrolyte conditions.By above-mentioned effect, corruption can be made
Phytic acid and the metal ion added are compound, and the compound formed will assign humic acid new function, so as to according to difference
Need to be prepared into the various composites for having specific function.Therefore, the metallic compound and humic acid that will there is affinity with fluorine
It is compound, a kind of novel absorption material is prepared into, it is excellent to reflect wide source, cheap, selectivity height, fluorine removing rate height etc.
Point, developing this kind of new defluorination absorbing material has larger practical value.
The content of the invention
Technical problem existing for basic background technology, the present invention proposes a kind of efficiently humic acid fluorine ion absorber, former
Expect wide material sources, preparation technology is simple, and adsorption capacity is high, and fluorine removing rate is high, so as to substantially reduce cost.
A kind of efficiently humic acid fluorine ion absorber, its raw material proposed by the present invention include by weight：Humic acid 35-38
Part, iron chloride 4-5 parts, aluminium chloride 28-32 parts, manganese chloride 4-5 parts, zirconium chloride 68-72 parts, calcium chloride 7-10 parts, mixed coal powder
49-52 parts, 1.2-1.5mol/L sodium hydroxide solution 55-60 parts；Wherein, mixed coal powder is prepared according to following technique：
12-15 parts coal dust is added in 42-48 parts 8.5-8.8mol/L hydrochloric acid solution, temperature is risen to 83-86 DEG C and with 130-
150rpm mixing speed stirring 1.5-1.8h, then cools the temperature to after being stored at room temperature 8-10h and filters, then solid to filtering gained
Body carries out heating high-pressure drying 20-23min and obtains drying solid coal dust, and the temperature for heating high-pressure drying is 50-55 DEG C, and heating adds
It is 8-10Pa to press dry dry pressure；By 40-50 part drying solids coal dust, 20-24 parts activated carbon, 16-20 part sepiolite powders with 87-
93rpm mixing speed stirring 1.7-2h obtains mixed coal powder；
In the preparation process of efficient humic acid fluorine ion absorber, by zirconium chloride, iron chloride, aluminium chloride, manganese chloride, chlorine
Change that calcium is soluble in water successively obtains iron-aluminum-manganese zirconium calcium mixed solution；Humic acid addition sodium hydroxide solution is obtained into alkaline humic acid
Sodium solution, alkaline sodium humate solution is stirred, iron-aluminum-manganese zirconium calcium mixed solution is added in whipping process, with stirring for 57-60rpm
Speed stirring 1.4-2.1h is mixed, then after pH value is adjusted to 6.5-7.5 and stands 4-6h, carries out being filtrated to get solid mixture；
After solid mixture is washed with clear water, heating high-pressure drying 30-35min obtains metal oxide-humic complex, wherein heating adds
Dry temperature is pressed dry as 55-65 DEG C, the pressure for heating high-pressure drying is 0.03-0.05kPa；By mixed coal powder and humic acid metal
Complex compound is placed in mixer, and obtaining efficient humic acid fluorine ion with 225-230rpm mixing speed stirring 0.8-1.2h adsorbs
Agent.
Preferably, mixed coal powder is 800-900 mesh.
Preferably, its raw material includes by weight：Humic acid 36-37 parts, iron chloride 4.2-4.4 parts, aluminium chloride 29-31
Part, manganese chloride 4.6-4.8 parts, zirconium chloride 69-70 parts, calcium chloride 8-9 parts, 800-900 mesh mixed coal powder 50-51 parts, 1.2-
1.5mol/L sodium hydroxide solution 56-59 parts.
Preferably, mixed coal powder is prepared according to following technique：13-14 parts coal dust is added into 44-46 parts 8.5-
In 8.8mol/L hydrochloric acid solution, temperature is risen to 84-85 DEG C and 1.6-1.7h is stirred with 135-140rpm mixing speed, is connect
Cool the temperature to be stored at room temperature 8.3-9.2h after filter, then to filtering gained solid carry out heat high-pressure drying 21-22min obtain
To drying solid coal dust, the temperature for heating high-pressure drying is 52-54 DEG C, and the pressure for heating high-pressure drying is 8.5-9.5Pa；Will
42-48 part drying solids coal dust, 22-23 parts activated carbon, 17-19 parts sepiolite powder stir 1.8- with 89-90rpm mixing speed
1.9h obtains 800-900 mesh mixed coal powders.
Preferably, in the preparation process of efficient humic acid fluorine ion absorber, by zirconium chloride, iron chloride, aluminium chloride, chlorine
Change manganese, calcium chloride is soluble in water successively obtains iron-aluminum-manganese zirconium calcium mixed solution；Humic acid addition sodium hydroxide solution is obtained into alkali
Property sodium humate solution, stir alkaline sodium humate solution, in whipping process add iron-aluminum-manganese zirconium calcium mixed solution, with 58-
59rpm mixing speed stirring 1.5-1.8h, then pH value is adjusted to 7 and after standing 4.6-5.2h, carry out being filtrated to get solid
Mixture；After solid mixture is washed with clear water, heating high-pressure drying 32-34min obtains metal oxide-humic complex, wherein
The temperature for heating high-pressure drying is 58-62 DEG C, and the pressure for heating high-pressure drying is 0.04kPa；By 800-900 mesh mixed coal powder with
Metal oxide-humic complex is placed in mixer, and efficient humic acid is obtained with 227-229rpm mixing speed stirring 0.9-1.1h
Fluorine ion absorber.
The present invention using humic acid in the basic conditions can with metal ion occur complex reaction, and zirconium chloride, iron chloride,
Aluminium chloride, manganese chloride, calcium chloride cause zirconium ion, iron ion, aluminium ion, manganese ion, calcium ion and hydrogen-oxygen in the basic conditions
Radical ion combines to form colloid, ultimately forms humic acid-ZrO2-Fe2O3-Al2O3-MnO2- CaO aquogel polymers；Pass through again
Filter and washing, reduce the impurity in aquogel polymer, improve the purity of gelatin polymer；, will by heating high-pressure drying
Moisture in aquogel polymer further reduces, and forms the humic acid-ZrO with tridimensional network2-Fe2O3-Al2O3-
MnO2- CaO aeroge complexs, make the mechanical strength of the present invention be strengthened；And mixed coal powder both has higher porosity
Adsorption can be carried out to fluorine ion in water, containing substantial amounts of hydroxyl, carboxyl, amino again can be in water with huge specific surface area
Fluorine ion carries out Hydrogen Binding Adsorption, after mixed coal powder and the blending of aeroge complex, substantially increases the present invention to fluorine ion
Adsorption capacity and selectivity.Raw material sources of the present invention are extensive, and preparation technology is simple, and adsorption capacity is high, and fluorine removing rate is high, so as to big
Reduce cost greatly.
Embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of efficiently humic acid fluorine ion absorber, its raw material proposed by the present invention include by weight：35 parts of humic acid,
5 parts of iron chloride, 28 parts of aluminium chloride, 5 parts of manganese chloride, 68 parts of zirconium chloride, 10 parts of calcium chloride, 900 49 parts of mesh mixed coal powders,
55 parts of 1.5mol/L sodium hydroxide solution；Wherein 900 mesh mixed coal powder preparation methods are as follows：15 parts of coal dusts are added 42 parts
In 8.8mol/L hydrochloric acid solution, temperature is risen to 83 DEG C and 1.5h is stirred with 150rpm mixing speed, then drops temperature
Filtered to after being stored at room temperature 10h, then heating high-pressure drying 20min is carried out to filtering gained solid and obtains drying solid coal dust, added
The temperature of hot high-pressure drying is 50 DEG C, and the pressure for heating high-pressure drying is 10Pa；By 40 parts of drying solid coal dusts, 24 parts of activity
Charcoal, 16 parts of sepiolite powders obtain 900 mesh mixed coal powders with 93rpm mixing speed stirring 1.7h；
In the preparation process of efficient humic acid fluorine ion absorber, by zirconium chloride, iron chloride, aluminium chloride, manganese chloride, chlorine
Change that calcium is soluble in water successively obtains iron-aluminum-manganese zirconium calcium mixed solution；Humic acid addition sodium hydroxide solution is obtained into alkaline humic acid
Sodium solution, alkaline sodium humate solution is stirred, iron-aluminum-manganese zirconium calcium mixed solution is added in whipping process, with 57rpm stirring
Speed stirs 2.1h, then pH value is adjusted to 6.5 and after standing 6h, carries out being filtrated to get solid mixture；By solid mixture
After being washed with clear water, heating high-pressure drying 30min obtains metal oxide-humic complex, wherein the temperature of heating high-pressure drying is 65
DEG C, the pressure for heating high-pressure drying is 0.03kPa；900 mesh mixed coal powders and metal oxide-humic complex are placed in mixer,
Efficient humic acid fluorine ion absorber is obtained with 230rpm mixing speed stirring 0.8h.
Embodiment 2
A kind of efficiently humic acid fluorine ion absorber, its raw material proposed by the present invention include by weight：37 parts of humic acid,
4.2 parts of iron chloride, 31 parts of aluminium chloride, 4.6 parts of manganese chloride, 70 parts of zirconium chloride, 8 parts of calcium chloride, 800 51 parts of mesh mixed coal powders,
59 parts of 1.3mol/L sodium hydroxide solution；Wherein 800 mesh mixed coal powder preparation methods are as follows：12 parts of coal dusts are added 48 parts
In 8.5mol/L hydrochloric acid solution, temperature is risen to 86 DEG C and 1.8h is stirred with 130rpm mixing speed, then drops temperature
Filtered to after being stored at room temperature 8h, then heating high-pressure drying 23min is carried out to filtering gained solid and obtains drying solid coal dust, heated
The temperature of high-pressure drying is 55 DEG C, and the pressure for heating high-pressure drying is 8Pa；By 50 parts of drying solid coal dusts, 20 parts of activated carbons, 20
Part sepiolite powder obtains 800 mesh mixed coal powders with 87rpm mixing speed stirring 2h；
In the preparation process of efficient humic acid fluorine ion absorber, by zirconium chloride, iron chloride, aluminium chloride, manganese chloride, chlorine
Change that calcium is soluble in water successively obtains iron-aluminum-manganese zirconium calcium mixed solution；Humic acid addition sodium hydroxide solution is obtained into alkaline humic acid
Sodium solution, alkaline sodium humate solution is stirred, iron-aluminum-manganese zirconium calcium mixed solution is added in whipping process, with 59rpm stirring
Speed stirs 1.5h, then pH value is adjusted to 7 and after standing 5.2h, carries out being filtrated to get solid mixture；By solid mixture
After being washed with clear water, heating high-pressure drying 32min obtains metal oxide-humic complex, wherein the temperature of heating high-pressure drying is 62
DEG C, the pressure for heating high-pressure drying is 0.04kPa；800 mesh mixed coal powders and metal oxide-humic complex are placed in mixer,
Efficient humic acid fluorine ion absorber is obtained with 227rpm mixing speed stirring 1.1h.
Embodiment 3
A kind of efficiently humic acid fluorine ion absorber, its raw material proposed by the present invention include by weight：38 parts of humic acid,
4 parts of iron chloride, 32 parts of aluminium chloride, 4 parts of manganese chloride, 72 parts of zirconium chloride, 7 parts of calcium chloride, 850 52 parts of mesh mixed coal powders, 1.2mol/
60 parts of L sodium hydroxide solution；Wherein 850 mesh mixed coal powder preparation methods are as follows：13 parts of coal dusts are added into 46 parts of 8.6mol/L
Hydrochloric acid solution in, temperature is risen to 85 DEG C and 1.7h is stirred with 135rpm mixing speed, it is quiet then to cool the temperature to room temperature
Filtered after putting 8.3h, then heating high-pressure drying 22min is carried out to filtering gained solid and obtains drying solid coal dust, heating pressurization is dry
Dry temperature is 52 DEG C, and the pressure for heating high-pressure drying is 9.5Pa；By 42 parts of drying solid coal dusts, 23 parts of activated carbons, 17 parts of seas
Afrodite powder obtains 850 mesh mixed coal powders with 90rpm mixing speed stirring 1.8h；
In the preparation process of efficient humic acid fluorine ion absorber, by zirconium chloride, iron chloride, aluminium chloride, manganese chloride, chlorine
Change that calcium is soluble in water successively obtains iron-aluminum-manganese zirconium calcium mixed solution；Humic acid addition sodium hydroxide solution is obtained into alkaline humic acid
Sodium solution, alkaline sodium humate solution is stirred, iron-aluminum-manganese zirconium calcium mixed solution is added in whipping process, with 58rpm stirring
Speed stirs 1.8h, then pH value is adjusted to 7 and after standing 4.6h, carries out being filtrated to get solid mixture；By solid mixture
After being washed with clear water, heating high-pressure drying 34min obtains metal oxide-humic complex, wherein the temperature of heating high-pressure drying is 58
DEG C, the pressure for heating high-pressure drying is 0.04kPa；850 mesh mixed coal powders and metal oxide-humic complex are placed in mixer,
Efficient humic acid fluorine ion absorber is obtained with 229rpm mixing speed stirring 0.9h.
Embodiment 4
A kind of efficiently humic acid fluorine ion absorber, its raw material proposed by the present invention include by weight：36 parts of humic acid,
4.4 parts of iron chloride, 29 parts of aluminium chloride, 4.8 parts of manganese chloride, 69 parts of zirconium chloride, 9 parts of calcium chloride, 870 50 parts of mesh mixed coal powders,
56 parts of 1.4mol/L sodium hydroxide solution；Wherein 870 mesh mixed coal powder preparation methods are as follows：14 parts of coal dusts are added 44 parts
In 8.6mol/L hydrochloric acid solution, temperature is risen to 84 DEG C and 1.6h is stirred with 140rpm mixing speed, then drops temperature
Filtered to after being stored at room temperature 9.2h, then heating high-pressure drying 21min is carried out to filtering gained solid and obtains drying solid coal dust, added
The temperature of hot high-pressure drying is 54 DEG C, and the pressure for heating high-pressure drying is 8.5Pa；By 48 parts of drying solid coal dusts, 22 parts of activity
Charcoal, 19 parts of sepiolite powders obtain 870 mesh mixed coal powders with 89rpm mixing speed stirring 1.9h；
In the preparation process of efficient humic acid fluorine ion absorber, by zirconium chloride, iron chloride, aluminium chloride, manganese chloride, chlorine
Change that calcium is soluble in water successively obtains iron-aluminum-manganese zirconium calcium mixed solution；Humic acid addition sodium hydroxide solution is obtained into alkaline humic acid
Sodium solution, alkaline sodium humate solution is stirred, iron-aluminum-manganese zirconium calcium mixed solution is added in whipping process, with 60rpm stirring
Speed stirs 1.4h, then pH value is adjusted to 7.5 and after standing 4h, carries out being filtrated to get solid mixture；By solid mixture
After being washed with clear water, heating high-pressure drying 35min obtains metal oxide-humic complex, wherein the temperature of heating high-pressure drying is 55
DEG C, the pressure for heating high-pressure drying is 0.05kPa；870 mesh mixed coal powders and metal oxide-humic complex are placed in mixer,
Efficient humic acid fluorine ion absorber is obtained with 225rpm mixing speed stirring 1.2h.
To embodiment 1-4 carry out performance test, with the patent of Application No. 201410214579.1 with it is a kind of efficiently it is honest and clean
Valency fluorine ion absorber is the first control group, and activated alumina is the second control group, and hydroxyl ash phosphorus stone is the 3rd control group, as a result
It is as shown in the table：
| Detection project | Embodiment 1-4 average values | First control group | Second control group | 3rd control group |
| Adsorption capacity (mg/g) | 12±1 | 8 | 3 | 2 |
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (4)
1. a kind of efficiently humic acid fluorine ion absorber, it is characterised in that its raw material includes by weight：Humic acid 35-38 parts,
Iron chloride 4-5 parts, aluminium chloride 28-32 parts, manganese chloride 4-5 parts, zirconium chloride 68-72 parts, calcium chloride 7-10 parts, mixed coal powder 49-
52 parts, 1.2-1.5mol/L sodium hydroxide solution 55-60 parts；Wherein, mixed coal powder is prepared according to following technique：Will
12-15 parts coal dust is added in 42-48 parts 8.5-8.8mol/L hydrochloric acid solution, and temperature is risen into 83-86 DEG C and with 130-
150rpm mixing speed stirring 1.5-1.8h, then cools the temperature to after being stored at room temperature 8-10h and filters, then solid to filtering gained
Body carries out heating high-pressure drying 20-23min and obtains drying solid coal dust, and the temperature for heating high-pressure drying is 50-55 DEG C, and heating adds
It is 8-10Pa to press dry dry pressure；By 40-50 part drying solids coal dust, 20-24 parts activated carbon, 16-20 part sepiolite powders with 87-
93rpm mixing speed stirring 1.7-2h obtains mixed coal powder；
In the preparation process of efficient humic acid fluorine ion absorber, by zirconium chloride, iron chloride, aluminium chloride, manganese chloride, calcium chloride
It is soluble in water successively to obtain iron-aluminum-manganese zirconium calcium mixed solution；It is molten that humic acid addition sodium hydroxide solution is obtained into alkaline sodium humate
Liquid, alkaline sodium humate solution is stirred, iron-aluminum-manganese zirconium calcium mixed solution is added in whipping process, with 57-60rpm stirring speed
Degree stirring 1.4-2.1h, then after pH value is adjusted to 6.5-7.5 and stands 4-6h, carry out being filtrated to get solid mixture；Will be solid
After body mixture is washed with clear water, heating high-pressure drying 30-35min obtains metal oxide-humic complex, wherein heating pressurization is dry
Dry temperature is 55-65 DEG C, and the pressure for heating high-pressure drying is 0.03-0.05kPa；By mixed coal powder and humic acid metal complex
Thing is placed in mixer, and efficient humic acid fluorine ion absorber is obtained with 225-230rpm mixing speed stirring 0.8-1.2h；
Mixed coal powder is 800-900 mesh.
2. efficient humic acid fluorine ion absorber as claimed in claim 1, it is characterised in that its raw material includes by weight：It is rotten
Phytic acid 36-37 parts, iron chloride 4.2-4.4 parts, aluminium chloride 29-31 parts, manganese chloride 4.6-4.8 parts, zirconium chloride 69-70 parts, chlorination
Calcium 8-9 parts, 800-900 mesh mixed coal powder 50-51 parts, 1.2-1.5mol/L sodium hydroxide solution 56-59 parts.
3. efficient humic acid fluorine ion absorber as claimed in claim 1 or 2, it is characterised in that mixed coal powder is according to following work
It is prepared by skill：13-14 parts coal dust is added in 44-46 parts 8.5-8.8mol/L hydrochloric acid solution, temperature is risen to 84-85 DEG C
And 1.6-1.7h is stirred with 135-140rpm mixing speed, then cool the temperature to after being stored at room temperature 8.3-9.2h and filter, then
Heating high-pressure drying 21-22min is carried out to filtering gained solid and obtains drying solid coal dust, the temperature for heating high-pressure drying is
52-54 DEG C, the pressure for heating high-pressure drying is 8.5-9.5Pa；By 42-48 part drying solids coal dust, 22-23 parts activated carbon, 17-
19 parts of sepiolite powders obtain 800-900 mesh mixed coal powders with 89-90rpm mixing speed stirring 1.8-1.9h.
4. efficient humic acid fluorine ion absorber as claimed in claim 1 or 2, it is characterised in that in efficient humic acid fluorine ion
In the preparation process of adsorbent, iron-aluminum-manganese is obtained by zirconium chloride, iron chloride, aluminium chloride, manganese chloride, calcium chloride are soluble in water successively
Zirconium calcium mixed solution；Humic acid addition sodium hydroxide solution is obtained into alkaline sodium humate solution, it is molten to stir alkaline sodium humate
Liquid, iron-aluminum-manganese zirconium calcium mixed solution is added in whipping process, 1.5-1.8h is stirred with 58-59rpm mixing speed, then by PH
Value is adjusted to 7 and after standing 4.6-5.2h, carries out being filtrated to get solid mixture；After solid mixture is washed with clear water, add
Hot high-pressure drying 32-34min obtains metal oxide-humic complex, wherein the temperature of heating high-pressure drying is 58-62 DEG C, heating adds
It is 0.04kPa to press dry dry pressure；800-900 mesh mixed coal powder and metal oxide-humic complex are placed in mixer, with
227-229rpm mixing speed stirring 0.9-1.1h obtains efficient humic acid fluorine ion absorber.
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| CN103962099A (en) * | 2014-05-09 | 2014-08-06 | 中国科学技术大学 | Fluorine removal agent prepared from fly ash, fluorine removal method and application of fluorine removal agent |
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Address after: 242310, Anhui, Xuancheng province Ningguo port town Industrial Zone Jinyang foreign high-tech materials Limited by Share Ltd Applicant after: Jinyang hi tech material Limited by Share Ltd Address before: 242310 provincial eco industrial park, port town, Xuancheng, Ningguo, Anhui Applicant before: Anhui Jinyang Fluorine Chemicals Co., Ltd. |
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| GR01 | Patent grant | ||
| GR01 | Patent grant |