CN105013432A - Method for preparing nanometer titanate adsorbent by utilizing ammoniation sheep manure - Google Patents
Method for preparing nanometer titanate adsorbent by utilizing ammoniation sheep manure Download PDFInfo
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Abstract
The invention relates to a method for preparing a nanometer titanate adsorbent by utilizing ammoniation sheep manure. The method comprises the following steps of: taking fresh sheep manure, making sheep manure starch, mashing and homogenating the sheep manure starch, adding an ammonia solution to the sheep manure starch, continuously mashing and homogenating the sheep manure starch in which the ammonia solution is added for 20-30 minutes, sealing the mashed and homogenated sheep manure starch, and performing heat preservation under the condition of 60-90 DEG C for 20-24 hours so as to obtain homogenized ammoniation sheep manure glue; under the condition of continuous stirring, dropwise adding tetrabutyl titanate to the ammoniation sheep manure glue slowly, and uniformly stirring the tetrabutyl titanate and the ammoniation sheep manure glue so as to obtain sheep manure glue containing titanium; adding a saturated water solution of the alkaline-earth metal compounds to the prepared sheep manure glue containing the titanium, and uniformly mixing the saturated water solution and the sheep manure glue to obtain a mixture; completely performing a stirring reaction, performing heating to 80-90 DEG C, baking the heated mixture at 105 DEG C after performing heat preservation, stirring and evaporation, making titanium-alkaline-earth metal-sheep manure xerogel, and calcining the titanium-alkaline-earth metal-sheep manure xerogel in atmosphere for 5-7 hours under the condition of 650-950 DEG C. According to the method disclosed by the invention, sheep manure glue is used for replacing sol gel to prepare all auxiliaries used for preparing a nanometer titanate type adsorbent, and a multihole titanate heavy metal adsorbing material which is low in cost and high in performance is prepared.
Description
Technical field
The invention belongs to environmental protection technical field, particularly a kind of method utilizing ammonification sheep excrement to prepare Nano titanate adsorbent.
Background technology
Rapidly, while we provide the milk of high-quality, meat and fur, the discharge of sheep excrement brings very large pressure also to our environment to the development of China sheep husbandry.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 the method for comprehensive utilization that more existing sheep excrement are new, 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., ZL201310251712.6); 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, polyethylene glycol 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 utilizing ammonification sheep excrement to prepare 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:
Utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
(1), fresh sheep excrement is got, adjustment moisture content is 87-90%, makes excrement slurry, is placed in and smashs to pieces in refiner, smash homogenate 20-30min to pieces, by excrement slurry and ammoniacal liquor mass ratio be the ammoniacal liquor that 1:0.05-0.5 gets that mass concentration is 25-28%, ammoniacal liquor is added excrement starch in, continue to smash homogenate 20-30min to pieces, airtight, under 60-90 DEG C of condition, be incubated 20-24h, obtain homogeneous ammonification sheep excrement glue, for subsequent use;
(2) be, that 1:0.1-2 gets butyl titanate by ammonification sheep excrement glue and butyl titanate mass ratio, under Keep agitation condition, butyl titanate is slowly added dropwise in the ammonification sheep excrement glue that step (1) obtains, stirs, 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, alkaline earth metal compound is added water and is mixed with saturated aqueous solution, join in titaniferous sheep excrement glue obtained in step (2), mix, stirring reaction is complete, is heated to 80-90 DEG C, after insulated and stirred evaporation, in 105 DEG C of oven dry, make titanium-alkaline-earth metal-sheep argol gel, for subsequent use;
(4), by the titanium-alkaline-earth metal-sheep argol gel of preparation in step (3) under 650-950 DEG C of condition, calcine 5-7h in air atmosphere, to obtain final product.
When smashing homogenate to pieces in above-mentioned steps (1), smash mixing speed >=5000r/min to pieces.
In above-mentioned steps (3), alkaline earth metal compound is calcium chloride, magnesium chloride, barium chloride or strontium chloride.
The invention has the advantages that:
All auxiliary agents used when the present invention replaces sol-gal process to prepare nano barium titanate salt adsorbent with sheep excrement glue, to utilize and while process sheep excrement, prepare 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, use 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 nano barium titanate calcium 4 in embodiment 4.
Detailed description of the invention
Embodiment 1
Utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 87%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by sheep excrement and ammoniacal liquor mass ratio 1:0.05, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 163g anhydrous calcium chloride, be dissolved in the 200mL warm water of 40 DEG C, be mixed with containing calcium solution, add in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 1;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
Embodiment 2
Utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 88%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.1, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 22h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 163g anhydrous calcium chloride, be dissolved in the 200mL warm water of 40 DEG C, be mixed with containing calcium solution, add in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 2;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
Embodiment 3
Utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 89%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.2, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 163g anhydrous calcium chloride, be dissolved in the 200mL warm water of 40 DEG C, be mixed with containing calcium solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 3;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
Embodiment 4
Utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 90%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.3, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 60 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 163g anhydrous calcium chloride, be dissolved in the 200mL warm water of 40 DEG C, be mixed with containing calcium solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 4;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
Embodiment 5
Utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 89%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.4, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 163g anhydrous calcium chloride, be dissolved in the 200mL warm water of 40 DEG C, be mixed with containing calcium solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 5;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
Embodiment 6
Utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 88%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.5, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 163g anhydrous calcium chloride, be dissolved in the 200mL warm water of 40 DEG C, be mixed with containing calcium solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 6;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
Embodiment 7
Utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 89%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.3, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, DEG C sealed thermal insulating 24h under 90 conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 100g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 33g anhydrous calcium chloride, be dissolved in the 50mL warm water of 40 DEG C, be mixed with containing calcium solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 7;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
Embodiment 8
Utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 90%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.3, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 300g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 98g anhydrous calcium chloride, be dissolved in the 100mL warm water of 40 DEG C, be mixed with containing calcium solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 8;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
Embodiment 9
Utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 90%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.3, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 163g anhydrous calcium chloride, be dissolved in the 200mL warm water of 40 DEG C, be mixed with containing calcium solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 80 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 950 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 9;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
Embodiment 10
Utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 89%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.3, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 1000g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 326g anhydrous calcium chloride, be dissolved in the 300mL warm water of 40 DEG C, be mixed with containing calcium solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 10;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
Embodiment 11
Utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 89%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.3, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 2000g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 652g anhydrous calcium chloride, be dissolved in the 600mL warm water of 40 DEG C, be mixed with containing calcium solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 11;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
Embodiment 12
Utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 89%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.3, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 200g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 144g barium chloride, be dissolved in the 400mL warm water of 40 DEG C, be mixed with baric solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-barium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium phthalate;
Above-mentioned barium chloride (BaCl
2h
2o) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
The absorption property of nano barium titanate salt pair lead
In order to investigate the absorption property of the Nano titanate heavy metal obtained in embodiment 1-12, 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 1-12
The regenerability of material
Nano titanate after absorption, washes 3 times, adds 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 | 24.93 | 23.87 | 95.7 |
| Nano barium titanate calcium 2 | 25 | 24.16 | 96.6 |
| Nano barium titanate calcium 3 | 25 | 23.83 | 95.3 |
| Nano barium titanate calcium 4 | 25 | 24.59 | 98.4 |
| Nano barium titanate calcium 5 | 24.71 | 24.11 | 97.6 |
| Nano barium titanate calcium 6 | 24.17 | 24.29 | 100.5 |
| Nano barium titanate calcium 7 | 24.67 | 23.84 | 96.7 |
| Nano barium titanate calcium 8 | 25 | 23.96 | 95.8 |
| Nano barium titanate calcium 9 | 24.83 | 24.68 | 99.4 |
| Nano barium titanate calcium 10 | 25 | 24.12 | 96.5 |
| Nano barium titanate calcium 11 | 23.52 | 22.53 | 95.8 |
| Nano barium phthalate | 24.38 | 23.81 | 97.7 |
After wash-out, can reuse after Nano titanate is washed to neutrality.
Claims (10)
1. utilize ammonification sheep excrement to prepare a method for Nano titanate adsorbent, it is characterized in that, comprise following processing step:
(1), fresh sheep excrement is got, adjustment moisture content is 87-90%, makes excrement slurry, is placed in and smashs to pieces in refiner, smash homogenate 20-30min to pieces, by excrement slurry and ammoniacal liquor mass ratio be the ammoniacal liquor that 1:0.05-0.5 gets that mass concentration is 25-28%, ammoniacal liquor is added excrement starch in, continue to smash homogenate 20-30min to pieces, airtight, under 60-90 DEG C of condition, be incubated 20-24h, obtain homogeneous ammonification sheep excrement glue, for subsequent use;
(2) be, that 1:0.1-2 gets butyl titanate by ammonification sheep excrement glue and butyl titanate mass ratio, under Keep agitation condition, butyl titanate is slowly added dropwise in the ammonification sheep excrement glue that step (1) obtains, stirs, 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, alkaline earth metal compound is added water and is mixed with saturated aqueous solution, join in titaniferous sheep excrement glue obtained in step (2), mix, stirring reaction is complete, is heated to 80-90 DEG C, after insulated and stirred evaporation, in 105 DEG C of oven dry, make titanium-alkaline-earth metal-sheep argol gel, for subsequent use;
(4), by the titanium-alkaline-earth metal-sheep argol gel of preparation in step (3) under 650-950 DEG C of condition, calcine 5-7h in air atmosphere, to obtain final product.
2. a kind of method utilizing ammonification sheep excrement to prepare Nano titanate adsorbent according to claim 1, is characterized in that: when smashing homogenate to pieces in described step (1), smash mixing speed >=5000r/min to pieces.
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 calcium chloride, magnesium chloride, barium chloride or strontium chloride.
4. a kind of method utilizing ammonification sheep excrement to prepare Nano titanate adsorbent according to claim 1, is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 87%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by sheep excrement and ammoniacal liquor mass ratio 1:0.05, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 163g anhydrous calcium chloride, be dissolved in the 200mL warm water of 40 DEG C, be mixed with containing calcium solution, add in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 1;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
5. a kind of method utilizing ammonification sheep excrement to prepare Nano titanate adsorbent according to claim 1, is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 88%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.1, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 22h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 163g anhydrous calcium chloride, be dissolved in the 200mL warm water of 40 DEG C, be mixed with containing calcium solution, add in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 2;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
6. a kind of method utilizing ammonification sheep excrement to prepare Nano titanate adsorbent according to claim 1, is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 89%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.2, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 163g anhydrous calcium chloride, be dissolved in the 200mL warm water of 40 DEG C, be mixed with containing calcium solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 3;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
7. a kind of method utilizing ammonification sheep excrement to prepare Nano titanate adsorbent according to claim 1, is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 90%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.3, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 60 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 163g anhydrous calcium chloride, be dissolved in the 200mL warm water of 40 DEG C, be mixed with containing calcium solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 4;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
8. a kind of method utilizing ammonification sheep excrement to prepare Nano titanate adsorbent according to claim 1, is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 90%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.3, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 300g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 98g anhydrous calcium chloride, be dissolved in the 100mL warm water of 40 DEG C, be mixed with containing calcium solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 8;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
9. a kind of method utilizing ammonification sheep excrement to prepare Nano titanate adsorbent according to claim 1, is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 90%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.3, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 500g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 163g anhydrous calcium chloride, be dissolved in the 200mL warm water of 40 DEG C, be mixed with containing calcium solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 80 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-calcium-sheep argol gel, be placed in cabinet-type electric furnace, under 950 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium titanate calcium 9;
Above-mentioned anhydrous calcium chloride (CaCl
2) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
10. a kind of method utilizing ammonification sheep excrement to prepare Nano titanate adsorbent according to claim 1, is characterized in that, comprise following processing step:
Get fresh sheep excrement, adjustment moisture content is 89%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then get ammoniacal liquor by excrement and ammoniacal liquor mass ratio 1:0.3, ammoniacal liquor is added in sheep excrement, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 90 DEG C of conditions, obtain homogeneous ammonification sheep excrement glue; Take 1000g ammonification sheep excrement glue, under Keep agitation condition, dropwise add 200g butyl titanate, after dripping, continue stirring reaction 30min, obtain titaniferous sheep excrement glue; Take 144g barium chloride, be dissolved in the 400mL warm water of 40 DEG C, be mixed with baric solution, join in titaniferous sheep excrement glue, stirring reaction 30min, be heated to 90 DEG C, dry under 105 DEG C of conditions after continuing insulated and stirred evaporate to dryness, make titanium-barium-sheep argol gel, be placed in cabinet-type electric furnace, under 700 DEG C of conditions, in air atmosphere, calcine 6h, obtain nano barium phthalate;
Above-mentioned barium chloride (BaCl
2h
2o) be AR; Ammoniacal liquor is pure for analyzing, mass concentration (NH
3) be 26%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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