CN105032338A - Method of preparing nano calcium titanate by aging and modifying sheep manure with quick lime - Google Patents
Method of preparing nano calcium titanate by aging and modifying sheep manure with quick lime Download PDFInfo
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- CN105032338A CN105032338A CN201510134251.3A CN201510134251A CN105032338A CN 105032338 A CN105032338 A CN 105032338A CN 201510134251 A CN201510134251 A CN 201510134251A CN 105032338 A CN105032338 A CN 105032338A
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Abstract
A method of preparing nano calcium titanate by aging and modifying sheep manure with quick lime includes the following steps: a) preparing fresh sheep manure into manure slurry and mashing and homogenizing the manure slurry for 20-40 min; b) adding the quick lime to the manure slurry and continuously mashing and homogenizing the manure slurry for 20-40 min; c) sealing the manure slurry and performing temperature-maintained aging reaction at 60-90 DEG C for 20-24 h to obtain homogenized calcified sheep manure gum; d) adding tetrabutyl titanate dropwisely to the calcified sheep manure gum under a continuous stirring condition, mixing the mixture uniformly and performing a stirring reaction completely; e) heating the mixture to 80-100 DEG C, maintaining the temperature and stirring and evaporating the mixture, drying the mixture at 105 DEG C to obtain titanium-calcium-sheep manure dried gel; and f) calcining the titanium-calcium-sheep manure dried gel at 650-950 DEG C in air for 5-7 h to obtain the nano calcium titanate. In the invention, with the sheep manure as an additive, the nano calcium titanate is low in cost, is strong in adsorption capability on heavy metal and is high in adsorption capacity.
Description
Technical field
The invention belongs to environmental protection technical field, particularly a kind of method utilizing quick lime slaking modification sheep excrement to prepare nano barium titanate calcium.
Background technology
Sheep is that people provide the milk of high-quality, meat and fur, but sheep excrement brings pollution also to our environment band.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 barium titanate calcium is a kind of stable high-performance heavy metal absorbent (east, Hou Ping, chemical journal, 67 volume 12 phase: p1336-1342 in 2009; DongZhang, Chun-liZhang, PinZhou, JournalofHazardousMaterials, 2011,186 volume 2-3 phases, p971 – 977), being generally with calcium nitrate and butyl titanate for calcium and titanium source, is complexing and dispersant with citric acid, acetic acid, alcohols etc., adopts the synthesis of sol-gel calcination method.But the method material used, reagent price are all very high, and the cost of the nano barium titanate calcium of synthesis is high, limit its application in practice.
Summary of the invention
Object of the present invention, is to provide a kind of method utilizing quick lime slaking modification sheep excrement to prepare nano barium titanate calcium, 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 quick lime slaking modification sheep excrement to prepare a method for nano barium titanate calcium, it is characterized in that, comprise following processing step:
(1), fresh sheep excrement is got, adjustment moisture content is 90-92%, making excrement slurry, smash homogenate 20-40min to pieces, is 1:0.05-0.3 preparing quick lime by excrement slurry and Lime Quality ratio, quick lime is added in excrement slurry, continue to smash homogenate 20-40min to pieces, airtight, under 60-90 DEG C of condition, be incubated slaking reaction 20-24h, obtain homogeneous calcification sheep excrement glue, for subsequent use;
(2) be, that 1:1 gets butyl titanate by calcium and titanium mol ratio, under Keep agitation condition, be added dropwise in the calcification sheep excrement glue obtained in step (1), mix, stirring reaction is complete, is heated to 80-100 DEG C, after insulated and stirred evaporation, dry under 105 DEG C of conditions, make titanium-calcium-sheep argol gel, for subsequent use;
(3), by the titanium-calcium-sheep argol gel of preparation in step (2) under 650-950 DEG C of condition, calcine 5-7h in air atmosphere, to obtain final product.
Described in above-mentioned steps (1) smash homogenate to pieces time, smash speed of agitator >=5000r/min to pieces.
This method is broken by mechanical force, utilize calcium oxide to cellulose in sheep excrement, lignin, the composition such as protein and colloidal substance, carry out modification, various compositions in sheep excrement, react in maturing process at calcium oxide and water, cellulose and lignin expand, permeability improves, specific area increases, macromolecular chain end group group hydroxylating, improve dispersiveness and the complexing power of sheep excrement, calcium ion fully contacts with the multicomponent in excrement and is combined into more stable complex compound simultaneously, dispersion evenly, react with butyl titanate again, the calcium titanate precursor generated is more even, cellulose in sheep excrement and lignin also play the effect of template simultaneously.
The invention has the advantages that:
The present invention utilizes sheep excrement for auxiliary agent, the nano barium titanate calcium of preparation, and cost is low, the high adsorption capacity of heavy metal, adsorption capacity is large, and 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 3 in embodiment 3.
Detailed description of the invention
Embodiment 1
Utilize quick lime slaking modification sheep excrement to prepare a method for nano barium titanate calcium, it is characterized in that, comprise following processing step:
Get the fresh sheep excrement 200g that adjustment moisture content is 90%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then add 10g quick lime, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtains homogeneous calcification sheep excrement glue; Under Keep agitation condition, in calcification sheep excrement glue, dropwise add 60.7g butyl titanate, stir, be heated to 90 DEG C, dry under 105 DEG C of conditions after stirring reaction evaporate to dryness, be placed in cabinet-type electric furnace, under 650 DEG C of conditions, calcining 6h, obtains nano barium titanate calcium 1;
Above-mentioned quick lime is AR, and butyl titanate is chemically pure reagent.
Embodiment 2
Utilize quick lime slaking modification sheep excrement to prepare a method for nano barium titanate calcium, it is characterized in that, comprise following processing step:
Get the fresh sheep excrement 200g that adjustment moisture content is 91%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then add 20g quick lime, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtains homogeneous calcification sheep excrement glue; Under Keep agitation condition, in calcification sheep excrement glue, dropwise add 121.4g butyl titanate, stir, be heated to 90 DEG C, dry under 105 DEG C of conditions after stirring reaction evaporate to dryness, be placed in cabinet-type electric furnace, under 650 DEG C of conditions, calcining 6h, obtains nano barium titanate calcium 2;
Above-mentioned quick lime is AR, and butyl titanate is chemically pure reagent.
Embodiment 3
Utilize quick lime slaking modification sheep excrement to prepare a method for nano barium titanate calcium, it is characterized in that, comprise following processing step:
Get the fresh sheep excrement 200g that adjustment moisture content is 92%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then add 40g quick lime, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtains homogeneous calcification sheep excrement glue; Under Keep agitation condition, in calcification sheep excrement glue, dropwise add 242.8g butyl titanate, stir, be heated to 90 DEG C, dry under 105 DEG C of conditions after stirring reaction evaporate to dryness, be placed in cabinet-type electric furnace, under 650 DEG C of conditions, calcining 6h, obtains nano barium titanate calcium 3;
Above-mentioned quick lime is AR, and butyl titanate is chemically pure reagent.
Embodiment 4
Utilize quick lime slaking modification sheep excrement to prepare a method for nano barium titanate calcium, it is characterized in that, comprise following processing step:
Get the fresh sheep excrement 200g that adjustment moisture content is 92%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then add 60g quick lime, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtains homogeneous calcification sheep excrement glue; Under Keep agitation condition, in calcification sheep excrement glue, dropwise add 364.2g butyl titanate, stir, be heated to 90 DEG C, dry under 105 DEG C of conditions after stirring reaction evaporate to dryness, be placed in cabinet-type electric furnace, under 650 DEG C of conditions, calcining 6h, obtains nano barium titanate calcium 4;
Above-mentioned quick lime is AR, and butyl titanate is chemically pure reagent.
Embodiment 5
Utilize quick lime slaking modification sheep excrement to prepare a method for nano barium titanate calcium, it is characterized in that, comprise following processing step:
Get the fresh sheep excrement 200g that adjustment moisture content is 92%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then add 40g quick lime, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtains homogeneous calcification sheep excrement glue; Under Keep agitation condition, in calcification sheep excrement glue, dropwise add 242.8g butyl titanate, stir, be heated to 90 DEG C, dry under 105 DEG C of conditions after stirring reaction evaporate to dryness, be placed in cabinet-type electric furnace, under 800 DEG C of conditions, calcining 6h, obtains nano barium titanate calcium 5;
Above-mentioned quick lime is AR, and butyl titanate is chemically pure reagent.
Embodiment 6
Utilize quick lime slaking modification sheep excrement to prepare a method for nano barium titanate calcium, it is characterized in that, comprise following processing step:
Get the fresh sheep excrement 200g that adjustment moisture content is 92%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then add 40g quick lime, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtains homogeneous calcification sheep excrement glue; Under Keep agitation condition, in calcification sheep excrement glue, dropwise add 242.8g butyl titanate, stir, be heated to 90 DEG C, dry under 105 DEG C of conditions after stirring reaction evaporate to dryness, be placed in cabinet-type electric furnace, under 950 DEG C of conditions, calcining 6h, obtains nano barium titanate calcium 6;
Above-mentioned quick lime is AR, and butyl titanate is chemically pure reagent.
Nano barium titanate calcium is to the absorption property of lead
In order to investigate the absorption property of the nano barium titanate calcium heavy metal obtained in embodiment 1-6, 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 nano barium titanate calcium prepared in table 1 embodiment 1-6 is to the removal capacity of lead
The regenerability of material
Nano barium titanate calcium 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 | 24.64 | 22.99 | 93.3 |
| Nano barium titanate calcium 2 | 24.82 | 24.68 | 99.4 |
| Nano barium titanate calcium 3 | 25 | 23.94 | 95.8 |
| Nano barium titanate calcium 4 | 24.38 | 23.82 | 97.7 |
| Nano barium titanate calcium 5 | 23.92 | 22.75 | 95.1 |
| Nano barium titanate calcium 6 | 21.18 | 20.38 | 96.2 |
After wash-out, can reuse after nano barium titanate calcium is washed to neutrality.
Claims (8)
1. utilize quick lime slaking modification sheep excrement to prepare a method for nano barium titanate calcium, it is characterized in that, comprise following processing step:
(1), fresh sheep excrement is got, adjustment moisture content is 90-92%, making excrement slurry, smash homogenate 20-40min to pieces, is 1:0.05-0.3 preparing quick lime by excrement slurry and Lime Quality ratio, quick lime is added in excrement slurry, continue to smash homogenate 20-40min to pieces, airtight, under 60-90 DEG C of condition, be incubated slaking reaction 20-24h, obtain homogeneous calcification sheep excrement glue, for subsequent use;
(2) be, that 1:1 gets butyl titanate by calcium and titanium mol ratio, under Keep agitation condition, be added dropwise in the calcification sheep excrement glue obtained in step (1), mix, stirring reaction is complete, is heated to 80-100 DEG C, after insulated and stirred evaporation, dry under 105 DEG C of conditions, make titanium-calcium-sheep argol gel, for subsequent use;
(3), by the titanium-calcium-sheep argol gel of preparation in step (2) under 650-950 DEG C of condition, calcine 5-7h in air atmosphere, to obtain final product.
2. a kind of method utilizing quick lime slaking modification sheep excrement to prepare nano barium titanate calcium according to claim 1, is characterized in that: when smashing homogenate to pieces in described step (1), smash speed of agitator >=5000r/min to pieces.
3. a kind of method utilizing quick lime slaking modification sheep excrement to prepare nano barium titanate calcium according to claim 1, is characterized in that, comprise following processing step:
Get the fresh sheep excrement 200g that adjustment moisture content is 90%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then add 10g quick lime, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtains homogeneous calcification sheep excrement glue; Under Keep agitation condition, in calcification sheep excrement glue, dropwise add 60.7g butyl titanate, stir, be heated to 90 DEG C, dry under 105 DEG C of conditions after stirring reaction evaporate to dryness, be placed in cabinet-type electric furnace, under 650 DEG C of conditions, calcining 6h, obtains nano barium titanate calcium 1;
Above-mentioned quick lime is AR, and butyl titanate is chemically pure reagent.
4. a kind of method utilizing quick lime slaking modification sheep excrement to prepare nano barium titanate calcium according to claim 1, is characterized in that, comprise following processing step:
Get the fresh sheep excrement 200g that adjustment moisture content is 91%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then add 20g quick lime, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtains homogeneous calcification sheep excrement glue; Under Keep agitation condition, in calcification sheep excrement glue, dropwise add 121.4g butyl titanate, stir, be heated to 90 DEG C, dry under 105 DEG C of conditions after stirring reaction evaporate to dryness, be placed in cabinet-type electric furnace, under 650 DEG C of conditions, calcining 6h, obtains nano barium titanate calcium 2;
Above-mentioned quick lime is AR, and butyl titanate is chemically pure reagent.
5. a kind of method utilizing quick lime slaking modification sheep excrement to prepare nano barium titanate calcium according to claim 1, is characterized in that, comprise following processing step:
Get the fresh sheep excrement 200g that adjustment moisture content is 92%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then add 40g quick lime, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtains homogeneous calcification sheep excrement glue; Under Keep agitation condition, in calcification sheep excrement glue, dropwise add 242.8g butyl titanate, stir, be heated to 90 DEG C, dry under 105 DEG C of conditions after stirring reaction evaporate to dryness, be placed in cabinet-type electric furnace, under 650 DEG C of conditions, calcining 6h, obtains nano barium titanate calcium 3;
Above-mentioned quick lime is AR, and butyl titanate is chemically pure reagent.
6. a kind of method utilizing quick lime slaking modification sheep excrement to prepare nano barium titanate calcium according to claim 1, is characterized in that, comprise following processing step:
Get the fresh sheep excrement 200g that adjustment moisture content is 92%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then add 60g quick lime, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtains homogeneous calcification sheep excrement glue; Under Keep agitation condition, in calcification sheep excrement glue, dropwise add 364.2g butyl titanate, stir, be heated to 90 DEG C, dry under 105 DEG C of conditions after stirring reaction evaporate to dryness, be placed in cabinet-type electric furnace, under 650 DEG C of conditions, calcining 6h, obtains nano barium titanate calcium 4;
Above-mentioned quick lime is AR, and butyl titanate is chemically pure reagent.
7. a kind of method utilizing quick lime slaking modification sheep excrement to prepare nano barium titanate calcium according to claim 1, is characterized in that, comprise following processing step:
Get the fresh sheep excrement 200g that adjustment moisture content is 92%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then add 40g quick lime, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtains homogeneous calcification sheep excrement glue; Under Keep agitation condition, in calcification sheep excrement glue, dropwise add 242.8g butyl titanate, stir, be heated to 90 DEG C, dry under 105 DEG C of conditions after stirring reaction evaporate to dryness, be placed in cabinet-type electric furnace, under 800 DEG C of conditions, calcining 6h, obtains nano barium titanate calcium 5;
Above-mentioned quick lime is AR, and butyl titanate is chemically pure reagent.
8. a kind of method utilizing quick lime slaking modification sheep excrement to prepare nano barium titanate calcium according to claim 1, is characterized in that, comprise following processing step:
Get the fresh sheep excrement 200g that adjustment moisture content is 92%, be placed in and smash to pieces in refiner, with 5000r/min speed, smash homogenate 30min to pieces, then add 40g quick lime, continue to smash homogenate 30min to pieces with identical speed, sealed thermal insulating 24h under 80 DEG C of conditions, obtains homogeneous calcification sheep excrement glue; Under Keep agitation condition, in calcification sheep excrement glue, dropwise add 242.8g butyl titanate, stir, be heated to 90 DEG C, dry under 105 DEG C of conditions after stirring reaction evaporate to dryness, be placed in cabinet-type electric furnace, under 950 DEG C of conditions, calcining 6h, obtains nano barium titanate calcium 6;
Above-mentioned quick lime is AR, and butyl titanate is chemically pure reagent.
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| 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 |
| CN103406091A (en) * | 2013-07-22 | 2013-11-27 | 沈阳理工大学 | Method for preparation of titanate adsorbent from (methyl) acrylic acid production wastewater |
| 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 |
| CN104383906A (en) * | 2014-11-10 | 2015-03-04 | 沈阳理工大学 | Method for preparing porous strontium titanate photocatalyst |
-
2015
- 2015-03-26 CN CN201510134251.3A patent/CN105032338A/en active Pending
Patent Citations (6)
| 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 |
| CN103406091A (en) * | 2013-07-22 | 2013-11-27 | 沈阳理工大学 | Method for preparation of titanate adsorbent from (methyl) acrylic acid production wastewater |
| 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 |
| CN104383906A (en) * | 2014-11-10 | 2015-03-04 | 沈阳理工大学 | Method for preparing porous strontium titanate photocatalyst |
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