CN105013433A - Method for preparing nanometer titanate adsorbent by modifying pig manure with acetic acid - Google Patents
Method for preparing nanometer titanate adsorbent by modifying pig manure with acetic acid Download PDFInfo
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Abstract
The invention relates to a method for preparing a nanometer titanate adsorbent by modifying pig manure with acetic acid. The method comprises the following steps of: 1) taking fresh pig manure, adjusting the water ratio, adding glacial acetic acid in the quality ratio of the pig manure to the glacial acetic acid being 1:04-0.8, mashing and homogenating the pig manure and the glacial acetic acid, adding a hydrogen peroxide solution according to the proportion of 1:0.1-0.3, continuously mashing and homogenating the pig manure, the glacial acetic acid and the hydrogen peroxide solution, and sealing the pig manure, the glacial acetic acid and the hydrogen peroxide solution for 24 hours so as to obtain modified pig manure glue with acetic acid; 2) under continuous stirring, dropwise adding tetrabutyl titanate to the modified pig manure glue with the acetic acid so as to obtain pig manure glue containing titanium; 3) adding an alkaline-earth metal compound in proportion to the pig manure glue containing titanium, stirring the alkaline-earth metal compound and the pig manure glue for reaction, and drying the reacted alkaline-earth metal compound and the reacted pig manure glue so as to prepare titanium-alkaline-earth metal-pig manure xerogel; and 4) calcining the xerogel so as to obtain the nanometer titanate adsorbent. The method disclosed by the invention utilizes the acetic acid for modifying the pig manure, realizes the resource utilization of the pig manure, and reduces the preparation cost of the nanometer titanate.
Description
Technical field
The invention belongs to environmental protection technical field, comprise the utilization of feces of livestock and poultry and the preparation of material for water treatment.Relate to a kind of method that acetic acid modification pig manure prepares Nano titanate adsorbent.Specifically, be utilize acetic acid modified to pig manure, for sol-gal process synthesis of nano titanate adsorbent.
Technical background
China is traditional big country of raising pigs.In recent years, the pig industry of China, from the dispersion cultivation of traditional peasant household, was rapidly to scale, intensive and industrialized development.While pig industry is flourish, the environmental problem that the concentrated discharge of pig manure causes is on the rise.Containing a large amount of organic matters in pig manure, traditional disposal and utilization method makes agricultural fertilizer after compost fermentation process.But in modern breeding process, in order to promote growing of pig, diseases prevention expelling parasite, generally all can add the additive of the elements such as cupric zinc-iron arsenic in feed; Sometimes, in order to prevent epidemic and cure the disease needs in breeding process, also antibiotic can be used, these materials all can excrete with ight soil mostly, thus the harmful substances such as excessive heavy metal are contained sometimes in the pig manure that pig farm is discharged, these harmful substances are difficult to effectively remove in composting fermentation process, if directly used, and can to soil and environment.For these problems, people have developed heavy metal and antibiotic techniques and methods (Lin Daiyan etc., patent of invention 200810071567.2 in some new removal pig manures; Zeng Qingru etc., application number: 201410197618.1; Zhou Jun etc. bioleaching method removes heavy metal and the research of its dewatering of raising in pig manure. and ACTA Scientiae Circumstantiae .201131 (2): 388-394; Zhang Shuqing, large-scale cultivation animal dung harmful components measure and harmless treatment effect, the Chinese Academy of Agricultural Sciences, post-doctoral research work report, 2004).But these methods, due to the not yet extensive use of high in cost of production reason, at present, can't meet the demand of aquaculture to swine manure treatment, and the pig manure of bulk deposition is badly in need of new utilization and process approach.
Pig belongs to Omnivore, containing more than 50% organic (comprising crude protein, free amino acid and cellulose etc.) in the pig manure of pig farm discharge, material in food, after the gastral digestion process of pig, character there occurs certain change, these compositions all have stronger complexing power to metal ion, by acetic acid to its further carboxylated process, improve the complexing of each component in ight soil, dispersion and gel-formation power, these performances can be applied in complexing sol-gel method synthesis.
Nano titanate is the high-performance heavy metal absorbent of first stability, and synthetic method the most frequently used is at present complexing sol-gel method (east, Hou Ping, chemical journal, 67 volume 12 phase: p1336-1342 in 2009; Zhang Dong, Wang Min, Tan Yuling, chemical journal, 16 phases, p1641-1648 in 2010; Dong Zhang, Chun-li Zhang, Pin Zhou, Journal ofHazardous Materials, 2011,186 volume 2-3 phases, p971 – 977), general is all adopt citric acid, acetic acid and alcohol reagent etc. for auxiliary agent, respectively with butyl titanate and alkaline earth nitrate for raw material, adopt the synthesis of collosol and gel calcination method to obtain.Material used and reagent price all very high, the cost of the Nano titanate of synthesis is very high, restriction Nano titanate adsorbent application in practice.
In order to disposal and utilization pig manure, reduce the synthesis cost of Nano titanate adsorbent simultaneously, acetic acid and hydrogen peroxide is utilized to process pig manure, improve the complexing of pig manure, dispersion and gel-formation power, respectively butyl titanate and alkaline earth metal compound are added again in pig manure slurry, add thermal response, flash to dry glue, high-temperature calcination, obtains Nano titanate adsorbent.The heavy metals such as the copper zinc, iron, manganese contained in pig manure are stayed in Nano titanate adsorbent admittedly, are entrained in these metal ions in titanate lattice, improve the absorption property of Nano titanate.
Summary of the invention
Object of the present invention, be to provide a kind of method that acetic acid modification pig manure prepares Nano titanate adsorbent, the present invention utilizes pig manure for raw material, utilize acetic acid and hydrogen peroxide to pig manure modification, improve the complexing plastic of pig manure and dispersibility, make all auxiliary agents that pig manure can replace in synthesis of nano titanate adsorbent process completely.
The present invention not only increases the adsorption capacity of Nano titanate adsorbent, and technique is simple, and production cost is low.
The technical scheme adopted is:
Utilize acetic acid modification pig manure to prepare a method for Nano titanate adsorbent, it is characterized in that the method comprises the steps:
1, get fresh pig manure, adjustment moisture content, within the scope of 88%-93%, obtains excrement slurry, for subsequent use;
2, it is that 1:0.4-0.8 gets glacial acetic acid that the excrement prepared by step 1 is starched with glacial acetic acid mass ratio, and is added by glacial acetic acid in excrement slurry, smashs homogenate 10-20min to pieces; The excrement prepared by step 1 again starches and hydrogen peroxide mass ratio is that 1:0.1-0.3 adds hydrogen peroxide, continues to smash homogenate 10-20min to pieces, airtight standing 8-24h, obtains acetic acid modification pig manure glue;
3, be 1:0.5 – 1 by acetic acid modification pig manure glue and butyl titanate mass ratio, get butyl titanate, under Keep agitation condition, be slowly added dropwise in the acetic acid modification pig manure glue that step 2 obtains, after dripping off, continue to stir 20-30min, obtain titaniferous pig manure glue;
4, be that 1:1 takes alkaline earth metal compound by alkaline-earth metal and titanium mol ratio, join in the obtained titaniferous pig manure glue of step 3, stir, be heated to 85-95 DEG C, continue insulated and stirred reaction, evaporation, finally dry under 105 DEG C of conditions, make titanium-alkaline-earth metal-pig manure xerogel;
5, titanium-alkaline-earth metal-pig manure xerogel step 4 prepared, in 650-950 DEG C, is calcined 4-6h in air atmosphere, is obtained Nano titanate adsorbent.
Described smash mixing speed to pieces when smashing homogenate to pieces and be not less than 4000r/min.
Described hydrogen peroxide mass concentration is 20-30%.
Described alkaline earth metal compound is one or more in calcium nitrate, magnesium nitrate, barium nitrate, strontium nitrate, calcium carbonate, brium carbonate, strontium carbonate and dolomite, lime stone, calcite.
The particle diameter of described calcium carbonate, brium carbonate, strontium carbonate and dolomite, lime stone, calcite is not more than 25 microns.
Present invention process is simple, and production cost is low, and the energy-absorbing power of the Nano titanate adsorbent produced is strong, makes pig manure get utilization simultaneously, avoids the pollution of pig manure to environment, have very high economy, society and environmental benefit.
Accompanying drawing explanation
Accompanying drawing 1 is the XRD spectrum of nano barium titanate calcium 3 in embodiment 3.
Detailed description of the invention
Embodiment 1: utilize pig manure and lime stone to prepare nano barium titanate calcium 1
Get fresh pig manure, adjustment moisture content, 88%, mixes, gets 1000g, add 800g glacial acetic acid, be placed in and smash to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, add 100g hydrogen peroxide again, continue to smash homogenate 15min to pieces, airtight placement 24h, obtain homogeneous acetic acid modification pig manure glue; Take 1000g acetic acid modification pig manure glue, under Keep agitation condition, slowly drip 500g butyl titanate, after dripping off, continue to stir 30min, obtain titaniferous pig manure glue; Take 149g agstone, join in titaniferous pig manure glue, stir, be heated to 90 DEG C, continue insulated and stirred reaction, evaporation, finally dry under 105 DEG C of conditions, make titanium-calcium-pig manure xerogel; By titanium-calcium-pig manure xerogel in 800 DEG C, calcine 6h in air atmosphere, in stove, naturally cool to room temperature, obtain nano barium titanate calcium adsorbent 1.
Embodiment 2: utilize pig manure and lime stone to prepare nano barium titanate calcium 2
Get fresh pig manure, adjustment moisture content, 89%, mixes, gets 1000g pig manure, add 400g glacial acetic acid, be placed in and smash to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, add 300g hydrogen peroxide again, continue to smash homogenate 15min to pieces, airtight placement 24h, obtain homogeneous acetic acid modification pig manure glue; Take 1000g acetic acid modification pig manure glue, under Keep agitation condition, slowly drip 1000g butyl titanate, after dripping off, continue to stir 30min, obtain titaniferous pig manure glue; Take 298g agstone, join in titaniferous pig manure glue, stir, be heated to 90 DEG C, continue insulated and stirred reaction, evaporation, finally dry under 105 DEG C of conditions, make titanium-calcium-pig manure xerogel; By titanium-calcium-pig manure xerogel in 700 DEG C, calcine 6h in air atmosphere, in stove, naturally cool to room temperature, obtain nano barium titanate calcium adsorbent 2.
Embodiment 3: utilize pig manure and calcium nitrate to prepare nano barium titanate calcium 3
Get fresh pig manure, adjustment moisture content, 90%, mixes, gets 1000g pig manure, add 500g glacial acetic acid, be placed in and smash to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, add 200g hydrogen peroxide again, continue to smash homogenate 15min to pieces, airtight placement 24h, obtain homogeneous acetic acid modification pig manure glue; Take 1000g acetic acid modification pig manure glue, under Keep agitation condition, slowly drip 600g butyl titanate, after dripping off, continue to stir 30min, obtain titaniferous pig manure glue; Take 417g calcium nitrate, join in titaniferous pig manure glue, stir, be heated to 90 DEG C, continue insulated and stirred reaction, evaporation, finally dry under 105 DEG C of conditions, make titanium-calcium-pig manure xerogel; By titanium-calcium-pig manure xerogel in 800 DEG C, calcine 6h in air atmosphere, in stove, naturally cool to room temperature, obtain nano barium titanate calcium adsorbent 3.
Embodiment 4: utilize pig manure and calcium nitrate to prepare nano barium titanate calcium 4
Get fresh pig manure, adjustment moisture content, 91%, mixes, gets 1000g pig manure, add 700g glacial acetic acid, be placed in and smash to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, add 400g hydrogen peroxide again, continue to smash homogenate 15min to pieces, airtight placement 24h, obtain homogeneous acetic acid modification pig manure glue; Take 1000g acetic acid modification pig manure glue, under Keep agitation condition, slowly drip 800g butyl titanate, after dripping off, continue to stir 30min, obtain titaniferous pig manure glue; Take 555g calcium nitrate, join in titaniferous pig manure glue, stir, be heated to 90 DEG C, continue insulated and stirred reaction, evaporation, finally dry under 105 DEG C of conditions, make titanium-calcium-pig manure xerogel; By titanium-calcium-pig manure xerogel in 650 DEG C, calcine 6h in air atmosphere, in stove, naturally cool to room temperature, obtain nano barium titanate calcium adsorbent 4.
Embodiment 5: utilize pig manure and the standby nano barium titanate calcium/magnesium compound adsorbent 1 of dolomite
Get fresh pig manure, adjustment moisture content, 92%, mixes, gets 1000g pig manure, add 400g glacial acetic acid, be placed in and smash to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, add 100g hydrogen peroxide again, continue to smash homogenate 15min to pieces, airtight placement 24h, obtain homogeneous acetic acid modification pig manure glue; Take 1000g acetic acid modification pig manure glue, under Keep agitation condition, slowly drip 1000g butyl titanate, after dripping off, continue to stir 30min, obtain titaniferous pig manure glue; Take 273g dolomite, join in titaniferous pig manure glue, stir, be heated to 90 DEG C, continue insulated and stirred reaction, evaporation, finally dry under 105 DEG C of conditions, make titanium-calcium/magnesium-pig manure xerogel; By titanium-calcium/magnesium-pig manure xerogel in 750 DEG C, calcine 6h in air atmosphere, in stove, naturally cool to room temperature, obtain nano barium titanate calcium/magnesium compound adsorbent 1.
Embodiment 6: utilize pig manure and the standby nano barium titanate calcium/magnesium compound adsorbent 2 of dolomite
Get fresh pig manure, adjustment moisture content, 93%, mixes, gets 1000g pig manure, add 800g glacial acetic acid, be placed in and smash to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, add 200g hydrogen peroxide again, continue to smash homogenate 15min to pieces, airtight placement 24h, obtain homogeneous acetic acid modification pig manure glue; Take 1000g acetic acid modification pig manure glue, under Keep agitation condition, slowly drip 500g butyl titanate, after dripping off, continue to stir 30min, obtain titaniferous pig manure glue; Take 137g dolomite, join in titaniferous pig manure glue, stir, be heated to 90 DEG C, continue insulated and stirred reaction, evaporation, finally dry under 105 DEG C of conditions, make titanium-calcium/magnesium-pig manure xerogel; By titanium-calcium/magnesium-pig manure xerogel in 850 DEG C, calcine 6h in air atmosphere, in stove, naturally cool to room temperature, obtain nano barium titanate calcium/magnesium compound adsorbent 2.
Embodiment 7: utilize pig manure and brium carbonate to prepare nano barium phthalate
Get fresh pig manure, add water, adjustment moisture content is 93%, mix, get 1000g pig manure, add 400g glacial acetic acid, be placed in and smash to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, then add 100g hydrogen peroxide, continue to smash homogenate 15min to pieces, airtight placement 8h, obtains homogeneous acetic acid modification pig manure glue; Take 1000g acetic acid modification pig manure glue, under Keep agitation condition, slowly drip 700g butyl titanate, after dripping off, continue to stir 30min, obtain titaniferous pig manure glue; Take 408g brium carbonate, join in titaniferous pig manure glue, stir, be heated to 90 DEG C, continue insulated and stirred reaction, evaporation, finally dry under 105 DEG C of conditions, make titanium-barium-pig manure xerogel; By titanium-barium-pig manure xerogel in 950 DEG C, calcine 6h in air atmosphere, in stove, naturally cool to room temperature, obtain nano barium phthalate adsorbent.
The agstone used in embodiment is 99% containing calcium carbonate, particle diameter 25 microns; Calcium nitrate (CaNO
34H
2o) be AR; The dolomite dust used is containing calcium carbonate 55.36%, and containing magnesium carbonate 44.10%, particle diameter is 25 microns; Brium carbonate is technical grade, content 99.5%, particle diameter 23 microns.
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 1-7, 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 adsorbent 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 1-7
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 (%) | |
| Calcium titanate 1 | 24.21 | 23.45 | 96.86 |
| Calcium titanate 2 | 22.60 | 22.38 | 99.02 |
| Calcium titanate 3 | 25 | 24.22 | 96.88 |
| Calcium titanate 4 | 25 | 25.04 | 100.16 |
| Calcium titanate magnesium 1 | 21.01 | 20.77 | 98.85 |
| Calcium titanate magnesium 2 | 23.41 | 21.58 | 92.20 |
| Barium titanate | 18.27 | 17.62 | 96.43 |
After wash-out, can reuse after Nano titanate is washed to neutrality.
Claims (5)
1. acetic acid modification pig manure prepares a method for Nano titanate adsorbent, it is characterized in that the method comprises the steps:
(1), get fresh pig manure, adjustment moisture content, within the scope of 88%-93%, obtains excrement slurry, for subsequent use;
(2), by step 1 prepare excrement slurry with glacial acetic acid mass ratio be that 1:0.4-0.8 gets glacial acetic acid, and glacial acetic acid is added excrement slurry in, smash homogenate 10-20min to pieces; The excrement prepared by step 1 again starches and hydrogen peroxide mass ratio is that 1:0.1-0.3 adds hydrogen peroxide, continues to smash homogenate 10-20min to pieces, airtight standing 8-24h, obtains acetic acid modification pig manure glue;
(3) be, that 1:0.5 – 1 gets butyl titanate by acetic acid modification pig manure glue and butyl titanate mass ratio, under Keep agitation condition, be slowly added dropwise in the acetic acid modification pig manure glue that step 2 obtains, after dripping off, continue to stir 20-30min, obtain titaniferous pig manure glue;
(4) be, that 1:1 takes alkaline earth metal compound by alkaline-earth metal and titanium mol ratio, join in the obtained titaniferous pig manure glue of step 3, stir, be heated to 85-95 DEG C, continue insulated and stirred reaction, evaporation, last dry under 105 DEG C of conditions, make titanium-alkaline-earth metal-pig manure xerogel;
(5) titanium-alkaline-earth metal-pig manure xerogel, by step 4 prepared, in 650-950 DEG C, is calcined 4-6h in air atmosphere, is obtained Nano titanate adsorbent.
2. a kind of acetic acid modification pig manure according to claim 1 prepares the method for Nano titanate adsorbent, smashs mixing speed to pieces and be not less than 4000r/min when it is characterized in that step (2) smashs homogenate to pieces.
3. a kind of acetic acid modification pig manure according to claim 1 prepares the method for Nano titanate adsorbent, it is characterized in that the hydrogen peroxide mass concentration that step (2) uses is 20-30%.
4. according to claim 1, described a kind of acetic acid modification pig manure prepares the method for Nano titanate adsorbent, it is characterized in that alkaline earth metal compound that step (4) is selected is one or more in calcium nitrate, magnesium nitrate, barium nitrate, strontium nitrate, calcium carbonate, brium carbonate, strontium carbonate and dolomite, lime stone, calcite.
5. a kind of acetic acid modification pig manure according to claim 4 prepares the method for Nano titanate adsorbent, it is characterized in that: the particle diameter of described calcium carbonate, brium carbonate, strontium carbonate and dolomite, lime stone, calcite is not more than 25 microns.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106986673A (en) * | 2017-02-28 | 2017-07-28 | 沈阳理工大学 | A kind of method that utilization feces of livestock and poultry prepares soilless culture haydite and nutrient solution |
| CN107043291A (en) * | 2017-02-28 | 2017-08-15 | 沈阳理工大学 | A kind of method that utilization feces of livestock and poultry prepares the soil remediation bag with fertilizer slow-released function |
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| 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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| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106986673A (en) * | 2017-02-28 | 2017-07-28 | 沈阳理工大学 | A kind of method that utilization feces of livestock and poultry prepares soilless culture haydite and nutrient solution |
| CN107043291A (en) * | 2017-02-28 | 2017-08-15 | 沈阳理工大学 | A kind of method that utilization feces of livestock and poultry prepares the soil remediation bag with fertilizer slow-released function |
| CN106986673B (en) * | 2017-02-28 | 2021-05-11 | 沈阳理工大学 | Method for preparing ceramsite and nutrient solution for soilless culture by using livestock and poultry manure |
| CN107043291B (en) * | 2017-02-28 | 2021-05-11 | 沈阳理工大学 | Method for preparing soil remediation bag with fertilizer slow-release function by using livestock and poultry manure |
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Application publication date: 20151104 |