CN104857923A - Method for preparing porous titanate sorbent by using poultry manure - Google Patents
Method for preparing porous titanate sorbent by using poultry manure Download PDFInfo
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- CN104857923A CN104857923A CN201510134217.6A CN201510134217A CN104857923A CN 104857923 A CN104857923 A CN 104857923A CN 201510134217 A CN201510134217 A CN 201510134217A CN 104857923 A CN104857923 A CN 104857923A
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Abstract
The invention relates to a method for preparing a porous titanate sorbent by using poultry manure. The process steps comprise: (1) taking fresh poultry manure, adjusting the water content, and carrying out mashing homogenizing to obtain a gelatineous manure slurry; (2) weighing titanium tetrachloride according to a ratio of 1:0.1-1, adding to the manure slurry prepared in the step (1), uniformly stirring, carrying out heating boiling, and cooling to a room temperature to obtain a titanium-containing manure gel; (3) weighing alkaline earth metal carbonate powder according to a molar ratio of the alkaline earth metal to the titanium of 1:1, adding to the titanium-containing manure gel prepared in the step (2), uniformly stirring, and drying to prepare a titanium-alkaline earth metal-manure dry gel; and (4) calcining the titanium-alkaline earth metal-manure dry gel prepared in the step (3) to obtain the porous titanate sorbent for removal of heavy metals in water. According to the present invention, the poultry manure is utilized to synthesize the porous titanate sorbent, the new low-cost porous titanate sorbent synthesis method is obtained, and the new way is provided for the resource utilization of the poultry manure.
Description
Technical field
The invention belongs to environmental protection technical field, relate to a kind of method utilizing brid guano to prepare porous titanate adsorbent.Specifically, be the method utilizing brid guano, titanium tetrachloride and alkaline earth metal carbonate to prepare POROUS TITANIUM Barbiturates heavy-metal adsorption material.
Technical background
The meat that bird provides and egg are the main sources that the mankind obtain high-quality animal protein.China is traditional poultry cultivation and consumption big country, and in recent years, along with the development of bird aquaculture, the environmental problem that the concentrated discharge of poultry dung causes is on the rise.The digestion power of bird is very poor, and in feed, the nutriment such as most of protein excretes with ight soil, and a large amount of brid guano provides hotbed not only to the growth of pathogeny bacterium and maggot fly, and the corrupt pernicious gas contaminated air decomposing the stench discharged.Traditional treatment method of poultry manure is by making agricultural fertilizer after compost fermentation, composting process not only the cycle long, sweat can discharge a large amount of mephitis, and organic matter easily runs off and enters water body, causes the pollution of air and water.In modern breeding process, in order to improve the yield and quality of birds, beasts and eggs and poultry, the metallic elements such as copper zinc, iron, manganese can be added in feed.Meanwhile, in order to diseases prevention and treatment, plant also often can use antibiotic etc, and these materials all can be discharged with ight soil mostly, is difficult to effectively remove in traditional composting fermentation process, if directly used, and can to soil and environment.In recent years, people have developed some new brid guano disposal and utilization technology (Zhu Qubo etc., ZL 201010233989.2; Open very civilian, patent of invention, application number: 201210561028.3; Wang Yuqin, the pollution of brid guano and control, Chinese livestock and poultry kind industry, 2014.07).But the utilization of these methods to brid guano is limited, a lot of plants brid guano is piled up, contaminated environment.
POROUS TITANIUM hydrochlorate is high-performance heavy metal absorbent (east, Wang Min, Tan Yuling, chemical journal, 16 phases, the p1641-1648 in 2010 of first stability; Dong Zhang, Chun-liZhang, Pin Zhou, Journal of Hazardous Materials, 2011,186 volume 2-3 phases, p971 – 977).At present, the most frequently used method of synthesizing porous titanate adopts the reagent such as citric acid, acetic acid, triethanolamine and alcohols as complexing, catalysis and dispersant, hydrogen peroxide etc. are pore-foaming agent, with butyl titanate and alkaline earth nitrate for titanium and alkaline earth metal source, add template or mould material, obtain in conjunction with the synthesis of collosol and gel calcining technology.The material that these methods are used and reagent price all very high, the cost of the POROUS TITANIUM hydrochlorate of synthesis is very high, restriction porous titanate adsorbent application in practice.
In order to disposal and utilization brid guano, reduce the synthesis cost of porous nano titanate adsorbent simultaneously, utilizing brid guano for auxiliary agent, provide titanium source with the titanium tetrachloride that price is lower, is alkaline earth metal source with the carbonate of the alkaline-earth metal such as lime stone, dolomite, calcium carbonate, brium carbonate.Utilize the hydrochloric acid that titanium tetrachloride and ight soil course of reaction generate, by adding thermal response, to the organic activation modification in ight soil, improve dispersiveness and the complexing power of organic principle in ight soil, unnecessary hydrochloric acid and the carbonate reaction of alkaline-earth metal, dissolved carbon hydrochlorate, the carbon dioxide simultaneously produced, plays pore effect.
Summary of the invention
The object of this is to propose a kind of recycling of brid guano and the preparation method of POROUS TITANIUM hydrochlorate sorbing material, and the present invention utilizes all auxiliary agents in brid guano replacement synthesizing titanate adsorbent process, and produce simple, synthesis cost is low.
The technical scheme adopted is:
Utilize brid guano to prepare a method for porous titanate adsorbent, it is characterized in that this method comprises the following steps:
1, get fresh brid guano, adjust moisture content to reach 82-92%, smash homogenate to pieces, smash mixer revolution >=5000 turn, point to pieces, smashing the homogenate time to pieces is 30-60min, obtains homogeneous excrement slurry, for subsequent use;
2, the excrement slurry prepared by step 1, under Keep agitation condition, add titanium tetrafluoride, excrement slurry is 1:0.1-1 with the mass ratio of titanium tetrafluoride, after dripping off, continue to be heated with stirring to boiling, keep the skin wet in time to water content 82-92%, keep slight boiling condition stirring reaction 1-4 hour, continue to stir, cool to room temperature, obtains titaniferous excrement glue;
3, be that 1:1 takes alkaline earth metal carbonate powder by alkaline-earth metal and titanium mol ratio, join in the obtained titaniferous excrement glue of step 2, mix, stirring reaction, heating evaporate to dryness, dry under 105 DEG C of conditions, make titanium-alkaline-earth metal-argol gel;
4, titanium-alkaline-earth metal-argol gel step 3 prepared is placed in electric furnace, in 650-1000 DEG C, calcines 4-6h in air atmosphere, cool to room temperature, obtains porous titanate adsorbent.
Above-mentioned brid guano comprises the fresh excreta of chicken, duck, goose, quail, pigeon.
Above-mentioned alkaline earth metal compound powder is one or more in calcium carbonate, brium carbonate, strontium carbonate, dolomite, lime stone, calcite.
The particle diameter of above-mentioned alkaline earth metal compound powder is not more than 25 microns.
Advantage of the present invention:
The present invention utilizes brid guano for auxiliary agent, provides titanium source with the titanium tetrachloride that price is lower, is alkaline earth metal source with the carbonate of the alkaline-earth metal such as lime stone, dolomite, calcium carbonate, brium carbonate.Utilize the hydrochloric acid that titanium tetrachloride and ight soil course of reaction generate, by adding thermal response, to the organic activation modification in ight soil, improve dispersiveness and the complexing power of organic principle in ight soil, unnecessary hydrochloric acid and the carbonate reaction of alkaline-earth metal, dissolved carbon hydrochlorate, the carbon dioxide simultaneously produced, plays pore effect.Therefore the present invention has good economic and social benefit.
Accompanying drawing explanation
Fig. 1 is the SEM photo of porous acid calcium 3 in embodiment 3; Fig. 2 is the XRD spectrum of porous acid calcium 3 in embodiment 3.
Detailed description of the invention
Embodiment 1: utilize chicken manure and lime stone to prepare porous calcium titanate 1
Get fresh chicken manure, adjustment moisture content is 82%, is placed in and smashs to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, obtains homogeneous excrement slurry.Get 1000g homogeneous excrement slurry, under Keep agitation condition, dropwise add 190g titanium tetrachloride, after dripping, continue to be heated with stirring to boiling, keep the skin wet, keep slight boiling condition, stirring reaction 2h, continue to stir, cool to room temperature, obtains titaniferous excrement glue.Take 101g agstone, add in titaniferous excrement glue, stirring reaction 30min, add thermal agitation evaporation, dry under 105 DEG C of conditions, make titanium-calcium-argol gel.Titanium-calcium-argol gel is placed in cabinet-type electric furnace, in 850 DEG C, in air atmosphere, calcines 6h, in stove, naturally cool to room temperature, obtain porous calcium titanate 1.
The agstone used in the present embodiment is 99% containing calcium carbonate, particle diameter 25 microns.
Embodiment 2: utilize chicken manure and lime stone to prepare porous calcium titanate 2
Get fresh chicken manure, adjustment moisture content is 85.6%, is placed in and smashs to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, obtains homogeneous excrement slurry.Get 1000g homogeneous excrement slurry, under Keep agitation condition, dropwise add 190g titanium tetrachloride, after dripping, continue to be heated with stirring to boiling, keep the skin wet, keep slight boiling condition, stirring reaction 3h, continue to stir, cool to room temperature, obtains titaniferous excrement glue.Taking 101g particle diameter is 25 microns, and weldering calcium titanate is the agstone of 99%, adds in titaniferous excrement glue, stirring reaction 30min, adds thermal agitation evaporation, dries, make titanium-calcium-argol gel under 105 DEG C of conditions.Titanium-calcium-argol gel is placed in cabinet-type electric furnace, in 850 DEG C, in air atmosphere, calcines 6h, in stove, naturally cool to room temperature, obtain porous calcium titanate 2.
The agstone used in the present embodiment is 99% containing calcium carbonate, particle diameter 25 microns.
Embodiment 3: utilize chicken manure and lime stone to prepare porous calcium titanate 3
Get fresh chicken manure, adjustment moisture content is 85.6%, is placed in and smashs to pieces in refiner, with 5000r/min mixing speed, smash homogenate 60min to pieces, obtains homogeneous excrement slurry.Get 1000g homogeneous excrement slurry, under Keep agitation condition, dropwise add 380g titanium tetrachloride, after dripping, continue to be heated with stirring to boiling, keep the skin wet, keep slight boiling condition, stirring reaction 1h, continue to stir, cool to room temperature, obtains titaniferous excrement glue.Take 202g agstone, add in titaniferous excrement glue, stirring reaction 30min, add thermal agitation evaporation, dry under 105 DEG C of conditions, make titanium-calcium-argol gel.Titanium-calcium-argol gel is placed in cabinet-type electric furnace, in 850 DEG C, in air atmosphere, calcines 6h, in stove, naturally cool to room temperature, obtain porous calcium titanate 3.
The agstone used in the present embodiment is 99% containing calcium carbonate, particle diameter 25 microns.
Embodiment 4: utilize chicken manure and lime stone to prepare porous calcium titanate 4
Get fresh chicken manure, adjustment moisture content is 88%, is placed in and smashs to pieces in refiner, with 5000r/min mixing speed, smash homogenate 40min to pieces, obtains homogeneous excrement slurry; Get 1000g homogeneous excrement slurry, under Keep agitation condition, dropwise add 760g titanium tetrachloride, after dripping, continue to be heated with stirring to boiling, keep the skin wet, keep slight boiling condition, stirring reaction 2h, continue to stir, cool to room temperature, obtains titaniferous excrement glue.Take 405g agstone, add in titaniferous excrement glue, stirring reaction 30min, add thermal agitation evaporation, dry under 105 DEG C of conditions, make titanium-calcium-argol gel.Titanium-calcium-argol gel is placed in cabinet-type electric furnace, in 850 DEG C, in air atmosphere, calcines 6h, in stove, naturally cool to room temperature, obtain porous calcium titanate 4.
The agstone used in the present embodiment is 99% containing calcium carbonate, particle diameter 25 microns.
Embodiment 5: utilize chicken manure and the standby porous calcium titanate/magnesium compound adsorbent 1 of dolomite
Get fresh chicken manure, adjustment moisture content is 91%, is placed in and smashs to pieces in refiner, with 6000r/min mixing speed, smash homogenate 30min to pieces, obtains homogeneous excrement slurry; Get 1000g homogeneous excrement slurry, under Keep agitation condition, dropwise add 950g titanium tetrachloride, after dripping, continue to be heated with stirring to boiling, keep the skin wet, keep slight boiling condition, stirring reaction 2h, continue to stir, cool to room temperature, obtains titaniferous excrement glue.Take 506g containing calcium carbonate 55.36% dolomite dust, add in titaniferous excrement glue, stirring reaction 30min, add thermal agitation evaporation, dry under 105 DEG C of conditions, make titanium-calcium/magnesium-argol gel.Titanium-calcium/magnesium-argol gel is placed in cabinet-type electric furnace, in 850 DEG C, calcines 6h in air atmosphere, naturally cool to room temperature in stove, obtains porous calcium titanate/magnesium compound adsorbent 1.
The dolomite dust used in the present embodiment is containing calcium carbonate 55.36%, and magnesium carbonate 44.10%, particle diameter is 25 microns.
Embodiment 6: utilize chicken manure and the standby porous calcium titanate/magnesium compound adsorbent 2 of dolomite
Get fresh chicken manure, adjustment moisture content is 89.7%, is placed in and smashs to pieces in refiner, with 6000r/min mixing speed, smash homogenate 30min to pieces, obtains homogeneous excrement slurry; Get 1000g homogeneous excrement slurry, under Keep agitation condition, dropwise add 570g titanium tetrachloride, after dripping, continue to be heated with stirring to boiling, keep the skin wet, keep slight boiling condition, stirring reaction 3h, continue to stir, cool to room temperature, obtains titaniferous excrement glue.Take 279g containing calcium carbonate 55.36% dolomite dust, add in titaniferous excrement glue, stirring reaction 30min, add thermal agitation evaporation, dry under 105 DEG C of conditions, make titanium-calcium/magnesium-argol gel.Titanium-calcium/magnesium-argol gel is placed in cabinet-type electric furnace, in 850 DEG C, calcines 6h in air atmosphere, naturally cool to room temperature in stove, obtains porous calcium titanate/magnesium compound adsorbent 2.
The dolomite dust used in the present embodiment is containing calcium carbonate 55.36%, and magnesium carbonate 44.10%, particle diameter is 25 microns.
Embodiment 7: utilize duck excrement and lime stone to prepare porous calcium titanate 5
Get fresh duck excrement, adjustment moisture content is 90.5%, is placed in and smashs to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, obtains homogeneous excrement slurry; Get 1000g homogeneous excrement slurry, under Keep agitation condition, dropwise add 190g titanium tetrachloride, after dripping, continue to be heated with stirring to boiling, keep the skin wet, keep slight boiling condition, stirring reaction 3h, continue to stir, cool to room temperature, obtains titaniferous excrement glue.Take 101g agstone, add in titaniferous excrement glue, stirring reaction 30min, add thermal agitation evaporation, dry under 105 DEG C of conditions, make titanium-calcium-argol gel.Titanium-calcium-argol gel is placed in cabinet-type electric furnace, in 850 DEG C, in air atmosphere, calcines 6h, in stove, naturally cool to room temperature, obtain porous calcium titanate 5.
The agstone used in the present embodiment is 99% containing calcium carbonate, particle diameter 25 microns.
Embodiment 8: utilize chicken manure and brium carbonate to prepare porous barium titanate
Get fresh chicken manure, adjustment moisture content is 92%, is placed in and smashs to pieces in refiner, with 5000r/min mixing speed, smash homogenate 30min to pieces, obtains homogeneous excrement slurry; Get 1000g homogeneous excrement slurry, under Keep agitation condition, dropwise add 190g titanium tetrachloride, after dripping, continue to be heated with stirring to boiling, keep the skin wet, keep slight boiling condition, stirring reaction 3h, continue to stir, cool to room temperature, obtains titaniferous excrement glue.Take 199g brium carbonate powder, add in titaniferous excrement glue, stirring reaction 30min, add thermal agitation evaporation, dry under 105 DEG C of conditions, make titanium-barium-argol gel.Titanium-barium-argol gel is placed in cabinet-type electric furnace, in 850 DEG C, in air atmosphere, calcines 6h, in stove, naturally cool to room temperature, obtain porous barium titanate.
The particle diameter of brium carbonate powder used in the present embodiment is 23 microns, content 99.5%.
POROUS TITANIUM hydrochlorate is to the absorption property of lead
In order to investigate the absorption property of the POROUS TITANIUM hydrochlorate heavy metal obtained in embodiment 1-8, get the standard liquid containing 25mg lead, in 150mL scale calibrated tool plug conical flask, adjust the pH value of solution to 6,50mL scale is settled to water, add the porous 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 POROUS TITANIUM hydrochlorate prepared in table 1 embodiment 1-8 is to the removal capacity of lead
The regenerability of material
Get the POROUS TITANIUM hydrochlorate 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 (%) | |
| Porous calcium titanate 1 | 21.39 | 20.66 | 96.58 |
| Porous calcium titanate 2 | 25 | 24.38 | 97.52 |
| Porous calcium titanate 3 | 25 | 24.54 | 98.16 |
| Porous calcium titanate 4 | 22.72 | 22.09 | 97.24 |
| Porous calcium titanate magnesium 1 | 19.33 | 19.19 | 99.29 |
| Porous calcium titanate magnesium 2 | 25 | 23.86 | 95.44 |
| Porous calcium titanate 5 | 24.32 | 22.19 | 91.26 |
| Porous barium titanate | 17.08 | 17.02 | 99.63 |
After wash-out, can reuse after POROUS TITANIUM hydrochlorate is washed to neutrality.
Claims (5)
1. utilize brid guano to prepare a method for porous titanate adsorbent, it is characterized in that comprising the steps:
Step one: get fresh brid guano, adjustment moisture content is 82%-92%, smashs more than homogenate 30min to pieces, obtains homogeneous excrement slurry;
Step 2: starching with titanium tetrachloride mass ratio by homogeneous excrement is that 1:0.1-1 gets titanium tetrachloride, under Keep agitation condition, titanium tetrachloride is slowly added dropwise in the homogeneous excrement slurry that step one obtains, after dripping off, continue to be heated with stirring to boiling, supplementing moisture content in time to containing dose rate is 82%-92%, keep slight boiling condition stirring reaction 1-4 hour, continue to stir, cool to room temperature, obtains titaniferous excrement glue;
Step 3: take alkaline earth metal carbonate powder by alkaline-earth metal and titanium mol ratio and 1:1, joins in the obtained titaniferous excrement glue of step 2, mixes, stirring reaction, and heating evaporate to dryness is dry under 105 DEG C of conditions, makes titanium-alkaline-earth metal-argol gel;
Step 4, titanium-alkaline-earth metal-argol gel step 3 prepared is placed in electric furnace, in 650-1000 DEG C, calcines 4-6h in air atmosphere, cool to room temperature, obtains porous titanate adsorbent.
2. a kind of method utilizing brid guano to prepare porous titanate adsorbent according to claim 1, is characterized in that brid guano comprises the fresh excreta of chicken, duck, goose, quail, pigeon.
3., according to claim 1, a kind of described method utilizing brid guano to prepare porous titanate adsorbent, when it is characterized in that step one brid guano smashs homogenate to pieces, smashs speed of agitator to pieces and is not less than 5000 revs/min.
4. according to claim 1, a kind of described method utilizing brid guano to prepare porous titanate adsorbent, the alkaline earth metal compound powder that it is characterized in that described in step 3 is one or more in calcium carbonate, brium carbonate, strontium carbonate, dolomite, lime stone, calcite.
5., according to claim 4, a kind of method utilizing brid guano to prepare porous titanate adsorbent, is characterized in that the particle diameter of described alkaline earth metal compound powder is not more than 25 microns.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101804328A (en) * | 2010-03-31 | 2010-08-18 | 沈阳理工大学 | Titanate porous monolithic adsorbent using straws as template and preparation method thereof |
| 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 |
| JP2015028473A (en) * | 2013-06-28 | 2015-02-12 | 富久 太田 | Base material containing absorbent of radioactive substance released in environment, manufacturing method thereof, method of reducing radioactive substance from radioactive substance pollution polluted water (hereafter polluted water), and device |
-
2015
- 2015-03-26 CN CN201510134217.6A patent/CN104857923A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101804328A (en) * | 2010-03-31 | 2010-08-18 | 沈阳理工大学 | Titanate porous monolithic adsorbent using straws as template and preparation method thereof |
| CN102430382A (en) * | 2011-09-23 | 2012-05-02 | 沈阳理工大学 | Method for preparing porous calcium titanate heavy metal adsorbent |
| JP2015028473A (en) * | 2013-06-28 | 2015-02-12 | 富久 太田 | Base material containing absorbent of radioactive substance released in environment, manufacturing method thereof, method of reducing radioactive substance from radioactive substance pollution polluted water (hereafter polluted water), and device |
| 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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