CN104857922A - Method for preparing nanometer titanate adsorbent through acetic acid modification on sheep manure - Google Patents
Method for preparing nanometer titanate adsorbent through acetic acid modification on sheep manure Download PDFInfo
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Abstract
The invention relates to a method for preparing a nanometer titanate adsorbent through acetic acid modification on sheep manure. The process steps comprise: taking fresh sheep manure to prepare a manure slurry, adding glacial acetic acid to the manure slurry, carrying out mashing homogenizing for 30-60 min, sealing, carrying out thermal insulation for 16-24 h at a temperature of 60-80 DEG C to obtain a homogenized acetic acid modification sheep manure gel, slowly adding tetrabutyl titanate to the obtained acetic acid modification sheep manure gel in a dropwise manner under a continuous stirring condition, stirring for 20-30 min after completing the adding to obtain a titanium-containing sheep manure gel, taking an alkaline earth metal compound, adding to the titanium-containing sheep manure gel, carrying out uniform stirring and mixing, heating to a temperature of 80-90 DEG C, carrying out thermal insulation stirring reaction, evaporating to completely remove the water, drying at a temperature of 100-110 DEG C to prepare a titanium-alkaline earth metal-sheep manure dry gel, and calcining the prepared titanium-alkaline earth metal-sheep manure dry gel for 4-6 h at a temperature of 650-1000 DEG C in an air atmosphere to obtain the finished product. According to the present invention, the acetic acid is utilized to modify the sheep manure and the modified sheep manure is utilized as the auxiliary agent to prepare the nanometer titanate adsorbent, such that the sheep manure is utilized and treated while the porous titanate heavy metal adsorption material with characteristics of low cost and high performance is prepared.
Description
Technical field
The invention belongs to environmental protection technical field, particularly a kind of acetic acid modification sheep excrement prepares the method for Nano titanate adsorbent.
Background technology
In recent years, China's sheep husbandry developed rapidly.But, no matter be grassland, pasture supports, or the modernization cultivation of scale livestock farming, the discharge of sheep excrement brings very large pressure to environment, and pollution problem highlights increasingly.For the process of sheep excrement, traditional method is ferment making agricultural fertilizer.But traditional compost fermentation method cycle is long, and Nutrient Availability is low, and nutrient easily runs off, contaminated environment.Sheep is Herbivore, and ight soil is dry and carefully, be rich in cellulose, lignin, protein, the available precious resources such as each seed amino acid and colloidal substance in sheep excrement.In recent years, the report of more existing sheep excrement method of comprehensive utilization, as: for the flocculation aid (Peng Jiang Rui Xu in morning is graceful, ZL201210484952.6) of waste water control; Prepare disinfectant and liquid ammonium K composite fertilizer (Liu Wei etc., ZL 201310251712.6); Preventing and fixing sand (Chen Wenye etc., application number 201310748256.6) etc.But, sheep excrement is had no report for the synthesis of the research of heavy-metal adsorption material.
Nano titanate is the high-performance heavy metal absorbent of first stability, general is all adopt the synthesis of sol-gel calcination method, that is: be raw material with butyl titanate and alkali salt, using citric acid, oleic acid, acetic acid, polyvinyl alcohol and ethanol etc. as dispersant, complexing agent and catalyst, adopt sol gel process to prepare titanate gel, high-temperature calcination obtains a Nano titanate (east, Hou Ping, chemistry journal, 2009,67 volume 12 phase: p1336-1342; Zhang Dong, Wang Min, Tan Yuling, chemical journal, 16 phases, p1641-1648 in 2010; Dong Zhang, Chun-li Zhang, Pin Zhou, Journal of Hazardous Materials, 2011,186 volume 2-3 phases, p971 – 977).The Nano titanate sorbing material function admirable of the method synthesis, but material used, reagent price are all very high, and the cost of the Nano titanate of synthesis is very high, the application in practice of restriction Nano titanate adsorbent.
Summary of the invention
Object of the present invention, is to provide a kind of method that acetic acid modification sheep excrement prepares Nano titanate adsorbent, and this method production technology is simple, and cost is low, solves the pollution problem of sheep excrement simultaneously.
The technical scheme adopted is:
Acetic acid modification sheep excrement prepares a method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
(1), fresh sheep excrement is got, adjustment moisture content is 82-94%, making excrement slurry, be placed in and smash to pieces in refiner, is that 1:0.3-1 gets glacial acetic acid by excrement slurry and glacial acetic acid mass ratio, glacial acetic acid is added in excrement slurry, smash homogenate 30-60min to pieces, airtight, under 60-80 DEG C of condition, be incubated 16-24h, obtain homogeneous acetic acid modification sheep excrement glue, for subsequent use;
(2) be, that 1:0.25-1 gets butyl titanate by sheep excrement glue and butyl titanate mass ratio, under Keep agitation condition, butyl titanate is slowly added dropwise in the acetic acid modification sheep excrement glue obtained in step (1), after dripping off, continue to stir 20-30min, obtain titaniferous sheep excrement glue, for subsequent use;
(3) be, that 1:1 takes alkaline earth metal compound by alkaline-earth metal and titanium mol ratio, join in titaniferous sheep excrement glue obtained in step (2), be uniformly mixed, be heated to 80-90 DEG C of insulated and stirred reaction, after evaporating water, in 100-110 DEG C of oven dry, make titanium-alkaline-earth metal-sheep argol gel, for subsequent use;
(4) titanium-alkaline-earth metal-sheep argol gel, by step (3) prepared, under 650-1000 DEG C of condition, is calcined 4-6h in air atmosphere, to be obtained final product.
Above-mentioned steps smashs mixing speed >=5000r/min to pieces in (1).
In above-mentioned steps (3), alkaline earth metal compound is the one in calcium nitrate, magnesium nitrate, barium nitrate, strontium nitrate, calcium carbonate, brium carbonate, strontium carbonate and dolomite dust, agstone.
Particle diameter≤25 micron of calcium carbonate, brium carbonate, strontium carbonate and dolomite dust, agstone in above-mentioned alkaline earth metal compound.
The invention has the advantages that:
The present invention utilizes acetic acid to the modification of sheep excrement, and utilize modification sheep excrement to be auxiliary agent, prepare Nano titanate adsorbent, to utilize and while process sheep excrement, divide preparation a kind of low cost, high performance POROUS TITANIUM Barbiturates heavy-metal adsorption material, manufacturing process of the present invention is simple, easy to operate, uses cost of material lower, be suitable for extensive use, there is good economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is the XRD spectrum of porous calcium titanate 1 in embodiment 2.
Fig. 2 is the stereoscan photograph of porous calcium titanate 1 in embodiment 2.
Detailed description of the invention
Embodiment 1
Acetic acid modification sheep excrement prepares a method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
(1), fresh sheep excrement is got, adjustment moisture content is 88-92%, making excrement slurry, be placed in and smash to pieces in refiner, is that 1:0.5-0.8 gets glacial acetic acid by excrement slurry and glacial acetic acid mass ratio, glacial acetic acid is added in excrement slurry, smash homogenate 30-60min to pieces, airtight, under 60-80 DEG C of condition, be incubated 16-24h, obtain homogeneous acetic acid modification sheep excrement glue, for subsequent use;
(2) be, that 1:0.25-0.8 gets butyl titanate by sheep excrement glue and butyl titanate mass ratio, under Keep agitation condition, butyl titanate is slowly added dropwise in the acetic acid modification sheep excrement glue obtained in step (1), after dripping off, continue to stir 20-30min, obtain titaniferous sheep excrement glue, for subsequent use;
(3) be, that 1:1 takes alkaline earth metal compound by alkaline-earth metal and titanium mol ratio, join in titaniferous sheep excrement glue obtained in step (2), be uniformly mixed, be heated to 80-90 DEG C of insulated and stirred reaction, after evaporating water, in 100-110 DEG C of oven dry, make titanium-alkaline-earth metal-sheep argol gel, for subsequent use;
(4) titanium-alkaline-earth metal-sheep argol gel, by step (3) prepared, under 650-1000 DEG C of condition, is calcined 4-6h in air atmosphere, to be obtained final product.
Embodiment 2
Acetic acid modification sheep excrement prepares a method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 88%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:0.5, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 60min to pieces, airtight, under 60 DEG C of conditions, be incubated 24h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 149g agstone, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 90 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium titanate calcium 1.
Above-mentioned agstone is containing calcium carbonate 99%, and particle diameter is 25 microns.
Embodiment 3
Acetic acid modification sheep excrement prepares a method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 90%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:0.8, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, airtight, under 60 DEG C of conditions, be incubated 24h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 700g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 208g agstone, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 80 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium titanate calcium 2;
Above-mentioned agstone is containing calcium carbonate 99%, and particle diameter is 25 microns.
Embodiment 4
Acetic acid modification sheep excrement prepares a method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 92%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:0.5, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, airtight, under 60 DEG C of conditions, be incubated 24h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 250g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 75g agstone, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 80 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium titanate calcium 3;
Above-mentioned agstone is containing calcium carbonate 99%, and particle diameter is 25 microns.
Embodiment 5
Acetic acid modification sheep excrement prepares a method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 92%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:0.8, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, airtight, under 60 DEG C of conditions, be incubated 16h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 800g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 238g agstone, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 85 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 800 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium titanate calcium 4;
Above-mentioned agstone is containing calcium carbonate 99%, and particle diameter is 25 microns.
Embodiment 6
Acetic acid modification sheep excrement prepares a method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 90%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:0.5, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, airtight, under 80 DEG C of conditions, be incubated 18h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 400g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 278g calcium nitrate, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 80-90 DEG C of insulated and stirred reaction, after evaporating water, dry under 105 DEG C of conditions, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium titanate calcium 5;
Above-mentioned calcium nitrate (CaNO
34H
2o) be AR.
Embodiment 7
Acetic acid modification sheep excrement prepares a method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 85%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:1, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, airtight, under 60 DEG C of conditions, be incubated 24h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 800g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 555g calcium nitrate, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 90 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium titanate calcium 6;
Above-mentioned calcium nitrate (CaNO
34H
2o) be AR.
Embodiment 8
Acetic acid modification sheep excrement prepares a method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 88%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:0.7, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, airtight, under 60 DEG C of conditions, be incubated 24h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 400g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 278g calcium nitrate tetrahydrate powder, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 90 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium titanate calcium 7.
Embodiment 9
Acetic acid modification sheep excrement prepares a method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 88%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:0.8, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, airtight, under 60 DEG C of conditions, be incubated 24h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 600g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 164g dolomite dust, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 90 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-calcium/magnesium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium titanate calcium/magnesium compound adsorbent 1;
Above-mentioned dolomite dust is containing calcium carbonate 55.36%, and containing magnesium carbonate 44.10%, particle diameter is 25 microns.
Embodiment 10
Acetic acid modification sheep excrement prepares a method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 92%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:0.4, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, airtight, under 60 DEG C of conditions, be incubated 24h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 1000g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 274g dolomite dust, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 80 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-calcium/magnesium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium titanate calcium/magnesium compound adsorbent 2;
Above-mentioned dolomite dust is containing calcium carbonate 55.36%, and containing magnesium carbonate 44.10%, particle diameter is 25 microns.
Embodiment 11
Acetic acid modification sheep excrement prepares a method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 94%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:0.3, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, airtight, under 60 DEG C of conditions, be incubated 24h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 900g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 525g brium carbonate powder, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 90 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-barium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium phthalate;
Above-mentioned brium carbonate is technical grade, content 99.5%, and particle diameter is 23 microns.
Nano titanate powder is to the absorption property of lead
In order to investigate the absorption property of the Nano titanate heavy metal obtained in embodiment 2-11, get the standard liquid containing 25mg lead, in 150mL scale calibrated tool plug conical flask, adjust the pH value of solution to 5,50mL scale is settled to water, add the Nano titanate of 0.1g, be placed on oscillator, with 200r/min speed, vibration absorption 20min, centrifugation, surveys the content of heavy metal lead in supernatant with Atomic absorption, calculate clearance by formula (1).The results are shown in Table 1.
In formula: η is plumbous clearance (%); C
0for initial concentration (mg/L); C
efor equilibrium concentration (mg/L).
The removal capacity of the nano barium titanate salt pair lead prepared in table 1 embodiment 2-11
The regenerability of material
Get the Nano titanate after absorption, wash 3 times, add the salpeter solution 10mL of 1mol/L respectively, vibrate wash-out 5min on oscillator, centrifugal, with the content of the lead ion of (or measuring after dilution) in atomic absorption detecting supernatant, calculate wash-out yield and the rate of recovery.The results are shown in Table 2:
Table 2: wash-out recovering state
| Absorption total amount (mg) | Wash-out yield (mg) | The rate of recovery (%) | |
| Nano barium titanate calcium 1 | 25 | 24.28 | 97.12 |
| Nano barium titanate calcium 2 | 25 | 24.15 | 96.6 |
| Nano barium titanate calcium 3 | 25 | 23.86 | 95.44 |
| Nano barium titanate calcium 4 | 25 | 25.32 | 101.28 |
| Nano barium titanate calcium 5 | 25 | 24.38 | 97.52 |
| Nano barium titanate calcium 6 | 24.56 | 23.39 | 95.22 |
| Nano barium titanate calcium 7 | 25 | 25.07 | 100.28 |
| Nano barium titanate calcium magnesium 1 | 25 | 24.64 | 98.56 |
| Nano barium titanate calcium magnesium 2 | 23.82 | 22.96 | 96.41 |
| Nano barium phthalate | 19.08 | 17.31 | 90.73 |
After wash-out, can reuse after Nano titanate is washed to neutrality.
Claims (10)
1. acetic acid modification sheep excrement prepares a method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
(1), fresh sheep excrement is got, adjustment moisture content is 82-94%, making excrement slurry, be placed in and smash to pieces in refiner, is that 1:0.3-1 gets glacial acetic acid by excrement slurry and glacial acetic acid mass ratio, glacial acetic acid is added in excrement slurry, smash homogenate 30-60min to pieces, airtight, under 60-80 DEG C of condition, be incubated 16-24h, obtain homogeneous acetic acid modification sheep excrement glue, for subsequent use;
(2) be, that 1:0.25-1 gets butyl titanate by sheep excrement glue and butyl titanate mass ratio, under Keep agitation condition, butyl titanate is slowly added dropwise in the acetic acid modification sheep excrement glue obtained in step (1), after dripping off, continue to stir 20-30min, obtain titaniferous sheep excrement glue, for subsequent use;
(3) be, that 1:1 takes alkaline earth metal compound by alkaline-earth metal and titanium mol ratio, join in titaniferous sheep excrement glue obtained in step (2), be uniformly mixed, be heated to 80-90 DEG C of insulated and stirred reaction, after evaporating water, in 100-110 DEG C of oven dry, make titanium-alkaline-earth metal-sheep argol gel, for subsequent use;
(4) titanium-alkaline-earth metal-sheep argol gel, by step (3) prepared, under 650-1000 DEG C of condition, is calcined 4-6h in air atmosphere, to be obtained final product.
2. a kind of acetic acid modification sheep excrement according to claim 1 prepares the method for Nano titanate adsorbent, it is characterized in that: described step smashs mixing speed >=5000r/min to pieces in (1).
3. a kind of acetic acid modification sheep excrement according to claim 1 prepares the method for Nano titanate adsorbent, it is characterized in that: in described step (3), alkaline earth metal compound is the one in calcium nitrate, magnesium nitrate, barium nitrate, strontium nitrate, calcium carbonate, brium carbonate, strontium carbonate and dolomite dust, agstone.
4. a kind of acetic acid modification sheep excrement according to claim 1 prepares the method for Nano titanate adsorbent, it is characterized in that: particle diameter≤25 micron of calcium carbonate, brium carbonate, strontium carbonate and dolomite dust, agstone in described alkaline earth metal compound.
5. a kind of acetic acid modification sheep excrement according to claim 1 prepares the method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
(1), fresh sheep excrement is got, adjustment moisture content is 88-92%, makes excrement slurry, is that 1:0.5-0.8 gets glacial acetic acid by excrement slurry and glacial acetic acid mass ratio, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30-60min to pieces, airtight, under 60-80 DEG C of condition, be incubated 16-24h, obtain homogeneous acetic acid modification sheep excrement glue, for subsequent use;
(2) be, that 1:0.25-0.8 gets butyl titanate by sheep excrement glue and butyl titanate mass ratio, under Keep agitation condition, butyl titanate is slowly added dropwise in the acetic acid modification sheep excrement glue obtained in step (1), after dripping off, continue to stir 20-30min, obtain titaniferous sheep excrement glue, for subsequent use;
(3) be, that 1:1 takes alkaline earth metal compound by alkaline-earth metal and titanium mol ratio, join in titaniferous sheep excrement glue obtained in step (2), be uniformly mixed, be heated to 80-90 DEG C of insulated and stirred reaction, after evaporating water, in 100-110 DEG C of oven dry, make titanium-alkaline-earth metal-sheep argol gel, for subsequent use;
(4) titanium-alkaline-earth metal-sheep argol gel, by step (3) prepared, under 650-1000 DEG C of condition, is calcined 4-6h in air atmosphere, to be obtained final product.
6. a kind of acetic acid modification sheep excrement according to claim 1 prepares the method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 88%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:0.5, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 60min to pieces, airtight, under 60 DEG C of conditions, be incubated 24h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 149g agstone, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 90 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium titanate calcium 1;
Above-mentioned agstone is containing calcium carbonate 99%, and particle diameter is 25 microns.
7. a kind of acetic acid modification sheep excrement according to claim 1 prepares the method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 90%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:0.8, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, airtight, under 60 DEG C of conditions, be incubated 24h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 700g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 208g agstone, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 80 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium titanate calcium 2;
Above-mentioned agstone is containing calcium carbonate 99%, and particle diameter is 25 microns.
8. a kind of acetic acid modification sheep excrement according to claim 1 prepares the method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 85%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:1, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, airtight, under 60 DEG C of conditions, be incubated 24h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 800g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 555g calcium nitrate, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 90 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium titanate calcium 6;
Above-mentioned calcium nitrate (CaNO
34H
2o) be AR.
9. a kind of acetic acid modification sheep excrement according to claim 1 prepares the method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 92%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:0.4, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, airtight, under 60 DEG C of conditions, be incubated 24h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 1000g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 274g dolomite dust, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 80 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-calcium/magnesium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium titanate calcium/magnesium compound adsorbent 2;
Above-mentioned dolomite dust is containing calcium carbonate 55.36%, and containing magnesium carbonate 44.10%, particle diameter is 25 microns.
10. a kind of acetic acid modification sheep excrement according to claim 1 prepares the method for Nano titanate adsorbent, it is characterized in that, comprises following processing step:
Get fresh sheep excrement, adjustment moisture content is 94%, make excrement slurry, get glacial acetic acid by excrement slurry with glacial acetic acid mass ratio 1:0.3, glacial acetic acid is added in excrement slurry, be placed in and smash to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, airtight, under 60 DEG C of conditions, be incubated 24h, obtain homogeneous acetic acid modification sheep excrement glue; Take 1000g acetic acid modification sheep excrement glue, under Keep agitation condition, dropwise add 900g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 525g brium carbonate powder, add in titaniferous sheep excrement glue, be uniformly mixed, be heated to 90 DEG C of insulated and stirred reactions, after evaporating water, dry under 105 DEG C of conditions, make titanium-barium-sheep argol gel, be placed in cabinet-type electric furnace, under 750 DEG C of conditions, calcine 6h in air atmosphere, obtain nano barium phthalate;
Above-mentioned brium carbonate is technical grade, content 99.5%, and particle diameter is 23 microns.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7524795B1 (en) * | 2004-02-20 | 2009-04-28 | The United States Of America As Represented By The Secretary Of The Agriculture | Activated carbons from animal manure |
| CN102430382A (en) * | 2011-09-23 | 2012-05-02 | 沈阳理工大学 | Method for preparing porous calcium titanate heavy metal adsorbent |
| CN103406089A (en) * | 2013-07-22 | 2013-11-27 | 沈阳理工大学 | Method for preparation of rime-like titanate by taking organic matters in methacrylic acid wastewater as template agent |
| CN103920479A (en) * | 2014-04-10 | 2014-07-16 | 福建师范大学 | Preparation method and applications of biomass modified TiO2 visible light photocatalyst |
-
2015
- 2015-03-26 CN CN201510134215.7A patent/CN104857922A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7524795B1 (en) * | 2004-02-20 | 2009-04-28 | The United States Of America As Represented By The Secretary Of The Agriculture | Activated carbons from animal manure |
| CN102430382A (en) * | 2011-09-23 | 2012-05-02 | 沈阳理工大学 | Method for preparing porous calcium titanate heavy metal adsorbent |
| CN103406089A (en) * | 2013-07-22 | 2013-11-27 | 沈阳理工大学 | Method for preparation of rime-like titanate by taking organic matters in methacrylic acid wastewater as template agent |
| CN103920479A (en) * | 2014-04-10 | 2014-07-16 | 福建师范大学 | Preparation method and applications of biomass modified TiO2 visible light photocatalyst |
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