CN104857915A - Method for preparing porous titanate adsorbent by using sludge - Google Patents

Method for preparing porous titanate adsorbent by using sludge Download PDF

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CN104857915A
CN104857915A CN201510134130.9A CN201510134130A CN104857915A CN 104857915 A CN104857915 A CN 104857915A CN 201510134130 A CN201510134130 A CN 201510134130A CN 104857915 A CN104857915 A CN 104857915A
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titaniferous
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earth metal
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CN104857915B (en
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张东
张璐瑶
王敏
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Huludao from Shi He De environmental protection equipment Co., Ltd.
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Shenyang Ligong University
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Abstract

The invention relates to a method for preparing a porous titanate adsorbent by using sludge. The process steps comprise: taking sludge, adjusting the water content of the sludge to 87-92%, placing into a mashing homogenizing machine, carrying out mashing homogenizing for 10-20 min to obtain a homogenized mud slurry, slowly adding titanium tetrachloride to the homogenized mud slurry in a dropwise manner under a continuous stirring condition, carrying out a sealing thermal insulation stirring reaction for 30-120 min at a temperature of 60-80 DEG C after completing the adding so as to obtain a titanium-containing gelatinous material, taking alkaline earth metal carbonate powder and adding to the titanium-containing gelatinous material, uniformly mixing, stirring, adjusting the pH value to 2.5-4 with ammonia water, carrying out stirring evaporation, drying at a temperature of 100-110 DEG C to prepare a titanium-alkaline earth metal-containing mud dry gel, placing the titanium-alkaline earth metal-containing mud dry gel into an electric furnace, calcining for 4-6 h at a temperature of 650-1000 DEG C in an air atmosphere, and naturally cooling to a room temperature in the furnace to obtain the finished product. According to the present invention, the sludge is directly utilized to synthesize the porous titanate so as to reduce the synthesis cost of the porous titanate adsorbent, and the porous titanate heavy metal adsorption material with characteristics of low cost and high performance is prepared.

Description

A kind of method utilizing mud to prepare porous titanate adsorbent
Technical field
The invention belongs to environmental protection technical field, relate to the utilization of city domestic sewage treatment plant excess sludge and the preparation of material for water treatment, particularly a kind of method utilizing mud to prepare porous titanate adsorbent.
Background technology
Along with the development of urbanization, urban population is increased sharply, and city domestic sewage discharge capacity is increasing, and these sanitary sewage biodegradabilities are good, and each city has all built the sewage treatment plant based on biochemical process, achieve the qualified discharge of sewage.But sewage treatment plant disposes of sewage in process, can produce a large amount of excess sludges, these moisture percentage in sewage sludge high (75% ~ 99%), content of organics is high, perishable.Containing the organic matter with potential value in mud, nitrogen, phosphorus, potassium and various trace element, also containing the heavy metal such as the pathogenic organisms such as parasitic ovum, pathogenic microorganism and copper, zinc, chromium, and the difficult degradation poisonous and harmful substance such as Polychlorinated biphenyls, bioxin, if do not dealt carefully with, easily cause secondary pollution.
The process of mud is a difficult problem for water treatment field always, and at present, the processing method for excess sludge mainly contains the methods such as Land_use change, sanitary landfills and burning.These method costs are high, there is Environmental security hidden danger.Dewater exceptionally in mud, containing a large amount of organic matters, these organic matters, based on the residual body of biology, are rich in protein, and a lot of compositions are wherein all valuable resources.Thus, actively inquire into the method for comprehensive utilization of mud, turning waste into wealth, is the best outlet of sludge treatment.
POROUS TITANIUM hydrochlorate is the high-performance heavy metal absorbent of first stability, generally all adopts via sol-gel template method to synthesize (east, Wang Min, Tan Yuling, chemical journal, 16 phases, p1641-1648 in 2010; DongZhang, Chun-li Zhang, Pin Zhou, Journal of Hazardous Materials, 2011,186 volume 2-3 phases, p971 – 977).The method respectively with butyl titanate and alkali salt for titanium and alkaline earth metal source, with citric acid, oleic acid, acetic acid and triethanolamine for complexing agent and catalyst, take alcohol reagent as dispersant, add the pore-foaming agents such as hydrogen peroxide or mould material again, obtain homogeneous titanate Gel Precursor by sol-gel technique, obtain porous titanate adsorbent through high-temperature calcination.The maximum problem of the method is expensive reagents used, and the titanate cost of synthesis is very high, which has limited the application in practice of porous titanate adsorbent.
Summary of the invention
Object of the present invention, is to provide a kind of method utilizing mud to prepare porous titanate adsorbent, and this method production technology is simple, utilizes mud to manufacture a kind of cost low, high performance heavy-metal adsorption material.
The technical scheme adopted is:
Utilize mud to prepare a method for porous titanate adsorbent, it is characterized in that, comprise following processing step:
(1) get mud, the moisture content of adjustment mud is 87-92%, puts into and smashs refiner to pieces, smash homogenate 10-20min to pieces, obtain homogenizing slurry, for subsequent use;
(2) be that 1:0.2 – 1 gets titanium tetrachloride by mud and titanium tetrachloride mass ratio, under Keep agitation condition, titanium tetrachloride is slowly added dropwise in the homogenizing slurry obtained in step (1), after dripping, under 60-80 DEG C of condition, sealed thermal insulating stirring reaction 30-120min, obtains titaniferous jelly, for subsequent use;
(3) be that 1:1 takes alkaline earth metal carbonate powder by alkaline-earth metal and titanium mol ratio, join in titaniferous jelly obtained in step (2), mix, stir, be 2.5-4 with ammoniacal liquor adjust pH, stir evaporate to dryness, finally dry under 100-110 DEG C of condition, make titaniferous-dry glue of alkaline-earth metal-mud, for subsequent use;
(4) titaniferous-dry glue of alkaline-earth metal-mud of preparation in step (3) is placed in electric furnace, under 650-1000 DEG C of condition, calcines 4-6h in air atmosphere, naturally cool to room temperature in stove, to obtain final product.
Smashing Homogenization time in above-mentioned steps (1) to pieces is 10-20min.
Above-mentioned steps (1) mud, when smashing homogenate to pieces, smashs homogenate speed of agitator >=4000 rev/min to pieces.
In above-mentioned steps (3), alkaline earth metal carbonate powder is one or more in Paris white, brium carbonate powder, strontium carbonate powder, dolomite dust, agstone and calcite in powder.
Particle diameter≤25 micron of alkaline earth metal carbonate powder in above-mentioned steps (3).
In above-mentioned steps (3), mixing time is 20-40min.
Said method process also make use of mud, and reduce the synthesis cost of porous nano titanate adsorbent, providing 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 simultaneously.In titanium tetrachloride and sludge reaction process, can generate hydrochloric acid, hydrochloric acid can, to organics modifications such as the protein in mud, make mud have complexing, dispersion and gel-formation power, necessary auxiliary agent when can substitute titanate synthesis completely.Unnecessary hydrochloric acid and the carbonate reaction of alkaline-earth metal, dissolved carbon hydrochlorate, the carbon dioxide simultaneously produced, plays pore effect.The inorganic constituents such as the heavy metal in mud are stayed in titanate adsorbent admittedly, and these materials are entrained in titanate, play the effect of the adsorption capacity improving titanate.
The invention has the advantages that:
The present invention directly utilizes the synthesizing porous titanate of mud, reduce the synthesis cost of porous titanate adsorbent, there is provided titanium source with the titanium tetrachloride that price is lower, 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, mud processed simultaneously, solve the problem of mud environmental pollution, turn waste into wealth, there is good economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is the XRD spectrum of porous calcium titanate 1 in embodiment 2.
Fig. 2 is the stereoscan photograph of porous calcium titanate 1 in embodiment 2.
Detailed description of the invention
Embodiment 1
Utilize mud to prepare a method for porous titanate adsorbent, it is characterized in that, comprise following processing step:
(1) get mud, the moisture content of adjustment mud is 88-91%, puts into and smashs refiner to pieces, smash homogenate 10-20min to pieces, obtain homogenizing slurry, for subsequent use;
(2) be that 1:0.4 – 0.8 gets titanium tetrachloride by mud and titanium tetrachloride mass ratio, under Keep agitation condition, titanium tetrachloride is slowly added dropwise in the homogenizing slurry obtained in step (1), after dripping, under 60-80 DEG C of condition, sealed thermal insulating stirring reaction 60-90min, obtains titaniferous jelly, for subsequent use;
(3) be that 1:1 takes alkaline earth metal carbonate powder by alkaline-earth metal and titanium mol ratio, join in titaniferous jelly obtained in step (2), mix, stir, be 2.5-4 with ammoniacal liquor adjust pH, stir evaporate to dryness, finally dry under 100-110 DEG C of condition, make titaniferous-dry glue of alkaline-earth metal-mud, for subsequent use;
(4) titaniferous-dry glue of alkaline-earth metal-mud of preparation in step (3) is placed in electric furnace, under 850 DEG C of conditions, calcines 4-6h in air atmosphere, naturally cool to room temperature in stove, to obtain final product.
Embodiment 2
Utilize mud to prepare a method for porous titanate adsorbent, it is characterized in that, comprise following processing step:
Get the excess sludge of new discharge, adjustment moisture content is 88.5%, is placed in and smashs to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, obtain homogenizing slurry; Take 1000g homogenizing slurry, under Keep agitation condition, dropwise add 500g titanium tetrachloride, after dripping, in 70 DEG C of sealed thermal insulating stirring reaction 60min, obtain titaniferous jelly, add 267g agstone, mix, stir 30min, be 3 with ammoniacal liquor adjust pH, agitating heating is evaporated, and finally dries under 105 DEG C of conditions, make titaniferous-dry glue of calcium-mud, be placed in cabinet-type electric furnace, under 850 DEG C of conditions, calcining 5h, naturally cools to room temperature in stove, obtains porous calcium titanate 1;
Above-mentioned agstone is containing calcium carbonate 99%, and particle diameter is 25 microns.
Embodiment 3
Utilize mud to prepare a method for porous titanate adsorbent, it is characterized in that, comprise following processing step:
Get the excess sludge of new discharge, adjustment moisture content is 88.5%, is placed in and smashs to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, obtain homogenizing slurry; Take 1000g homogenizing slurry, under Keep agitation condition, dropwise add 750g titanium tetrachloride, after dripping, in 70 DEG C of sealed thermal insulating stirring reaction 60min, obtain titaniferous jelly; Add 400g agstone, mix, stirring 30min, is 3 with ammoniacal liquor adjust pH, agitating heating evaporate to dryness, finally dries under 105 DEG C of conditions, makes titaniferous-dry glue of calcium-mud, is placed in cabinet-type electric furnace, under 850 DEG C of conditions, calcining 5h, naturally cools to room temperature in stove, obtains porous calcium titanate 2;
Above-mentioned agstone is containing calcium carbonate 99%, and particle diameter is 25 microns.
Embodiment 4
Utilize mud to prepare a method for porous titanate adsorbent, it is characterized in that, comprise following processing step:
Get the excess sludge of new discharge, adjustment moisture content is 90%, is placed in and smashs to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, obtain homogenizing slurry; Take 1000g homogenizing slurry, under Keep agitation condition, dropwise add 250g titanium tetrachloride, after dripping, in 70 DEG C of sealed thermal insulating stirring reaction 90min, obtain titaniferous jelly; Add 134g agstone, mix, stirring 30min, is 3 with ammoniacal liquor adjust pH, agitating heating evaporate to dryness, finally dries under 105 DEG C of conditions, makes titaniferous-dry glue of calcium-mud, is placed in cabinet-type electric furnace, under 850 DEG C of conditions, calcining 5h, naturally cools to room temperature in stove, obtains porous calcium titanate 3;
Above-mentioned agstone is containing calcium carbonate 99%, and particle diameter is 25 microns.
Embodiment 5
Utilize mud to prepare a method for porous titanate adsorbent, it is characterized in that, comprise following processing step:
Get the excess sludge of new discharge, adjustment moisture content is 92%, is placed in and smashs to pieces in refiner, with 4000r/min mixing speed, smash homogenate 10min to pieces, obtain homogenizing slurry; Take 1000g homogenizing slurry, under Keep agitation condition, dropwise add 500g titanium tetrachloride, after dripping, in 60 DEG C of sealed thermal insulating stirring reaction 30min, obtain titaniferous jelly; Add 267g agstone, mix, stirring 30min, is 2.5 with ammoniacal liquor adjust pH, agitating heating evaporate to dryness, finally dry under 105 DEG C of conditions, make titaniferous-dry glue of calcium-mud, be placed in cabinet-type electric furnace, under 650 DEG C of conditions, calcining 6h, naturally cools to room temperature in stove, obtains porous calcium titanate 4;
Above-mentioned agstone is containing calcium carbonate 99%, and particle diameter is 25 microns.
Embodiment 6
Utilize mud to prepare a method for porous titanate adsorbent, it is characterized in that, comprise following processing step:
Get the excess sludge of new discharge, adjustment moisture content is 87%, is placed in and smashs to pieces in refiner, with 4000r/min mixing speed, smash homogenate 20min to pieces, obtain homogenizing slurry; Take 1000g homogenizing slurry, under Keep agitation condition, dropwise add 400g titanium tetrachloride, after dripping, in 80 DEG C of sealed thermal insulating stirring reaction 120min, obtain titaniferous jelly; Add 196g dolomite dust, mix, stirring 30min, is 4 with ammoniacal liquor adjust pH, agitating heating evaporate to dryness, finally dry under 110 DEG C of conditions, make titaniferous-calcium/dry glue of magnesium-mud, be placed in cabinet-type electric furnace, under 1000 DEG C of conditions, calcining 4h, naturally cools to room temperature in stove, obtains porous calcium titanate/magnesium compound adsorbent 1;
Above-mentioned dolomite dust is containing calcium carbonate 55.36%, and magnesium carbonate 44.10%, particle diameter is 23 microns.
Embodiment 7
Utilize mud to prepare a method for porous titanate adsorbent, it is characterized in that, comprise following processing step:
Get the excess sludge of new discharge, adjustment moisture content is 91%, is placed in and smashs to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, obtain homogenizing slurry; Take 1000g homogenizing slurry, under Keep agitation condition, dropwise add 800g titanium tetrachloride, after dripping, in 70 DEG C of sealed thermal insulating stirring reaction 80min, obtain titaniferous jelly; Add 392g dolomite dust, mix, stirring 30min, is 3 with ammoniacal liquor adjust pH, agitating heating evaporate to dryness, finally dry under 105 DEG C of conditions, make titaniferous-calcium/dry glue of magnesium-mud, be placed in cabinet-type electric furnace, under 850 DEG C of conditions, calcining 5h, naturally cools to room temperature in stove, obtains porous calcium titanate/magnesium compound adsorbent 2;
Above-mentioned dolomite dust is containing calcium carbonate 55.36%, and magnesium carbonate 44.10%, particle diameter is 23 microns.
Embodiment 8
Utilize mud to prepare a method for porous titanate adsorbent, it is characterized in that, comprise following processing step:
Get the excess sludge of new discharge, adjustment moisture content is 92%, is placed in and smashs to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, obtain homogenizing slurry; Take 1000g homogenizing slurry, under Keep agitation condition, dropwise add 1000g titanium tetrachloride, after dripping, in 70 DEG C of sealed thermal insulating stirring reaction 30min, obtain titaniferous jelly; Add 1045g brium carbonate powder, mix, stirring 30min, is 3 with ammoniacal liquor adjust pH, agitating heating evaporate to dryness, finally dries under 105 DEG C of conditions, makes titaniferous-dry glue of barium-mud, is placed in cabinet-type electric furnace, under 850 DEG C of conditions, calcining 5h, naturally cools to room temperature in stove, obtains porous barium titanate;
Above-mentioned brium carbonate is technical grade, content 99.5%, and particle diameter is 23 microns.
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 2-8, 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 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.
η = ( C 0 - C e ) C 0 × 100 % - - - ( 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 2-8 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 25 24.37 97.48
Porous calcium titanate 2 24.12 22.98 95.26
Porous calcium titanate 3 23.90 23.06 96.49
Porous calcium titanate 4 19.65 18.17 92.46
Porous calcium titanate magnesium 1 25 24.91 99.64
Porous calcium titanate magnesium 2 24.23 24.14 99.61
Porous barium titanate 13.052 13.17 100.91
After wash-out, can reuse after POROUS TITANIUM hydrochlorate is washed to neutrality.

Claims (10)

1. utilize mud to prepare a method for porous titanate adsorbent, it is characterized in that, comprise following processing step:
(1) get mud, the moisture content of adjustment mud is 87-92%, puts into and smashs refiner to pieces, smash homogenate 10-20min to pieces, obtain homogenizing slurry, for subsequent use;
(2) be that 1:0.2 – 1 gets titanium tetrachloride by mud and titanium tetrachloride mass ratio, under Keep agitation condition, titanium tetrachloride is slowly added dropwise in the homogenizing slurry obtained in step (1), after dripping, under 60-80 DEG C of condition, sealed thermal insulating stirring reaction 30-120min, obtains titaniferous jelly, for subsequent use;
(3) be that 1:1 takes alkaline earth metal carbonate powder by alkaline-earth metal and titanium mol ratio, join in titaniferous jelly obtained in step (2), mix, stir, be 2.5-4 with ammoniacal liquor adjust pH, stir evaporate to dryness, finally dry under 100-110 DEG C of condition, make titaniferous-dry glue of alkaline-earth metal-mud, for subsequent use;
(4) titaniferous-dry glue of alkaline-earth metal-mud of preparation in step (3) is placed in electric furnace, under 650-1000 DEG C of condition, calcines 4-6h in air atmosphere, naturally cool to room temperature in stove, to obtain final product.
2. a kind of method utilizing mud to prepare porous titanate adsorbent according to claim 1, is characterized in that: described step (1) mud, when smashing homogenate to pieces, is smashed homogenate speed of agitator to pieces and is not less than 4000 revs/min.
3. a kind of method utilizing mud to prepare porous titanate adsorbent according to claim 1, is characterized in that: in described step (3), alkaline earth metal carbonate powder is one or more in Paris white, brium carbonate powder, strontium carbonate powder, dolomite dust, agstone and calcite in powder.
4. a kind of method utilizing mud to prepare porous titanate adsorbent according to claim 1, is characterized in that: in described step (3), the particle diameter of alkaline earth metal carbonate powder is not more than 25 microns.
5. a kind of method utilizing mud to prepare porous titanate adsorbent according to claim 1, is characterized in that, comprise following processing step:
(1) get mud, the moisture content of adjustment mud is 88-91%, puts into and smashs refiner to pieces, smash homogenate 10-20min to pieces, obtain homogenizing slurry, for subsequent use;
(2) be that 1:0.4 – 0.8 gets titanium tetrachloride by mud and titanium tetrachloride mass ratio, under Keep agitation condition, titanium tetrachloride is slowly added dropwise in the homogenizing slurry obtained in step (1), after dripping, under 60-80 DEG C of condition, sealed thermal insulating stirring reaction 60-90min, obtains titaniferous jelly, for subsequent use;
(3) be that 1:1 takes alkaline earth metal carbonate powder by alkaline-earth metal and titanium mol ratio, join in titaniferous jelly obtained in step (2), mix, stir, be 2.5-4 with ammoniacal liquor adjust pH, stir evaporate to dryness, finally dry under 100-110 DEG C of condition, make titaniferous-dry glue of alkaline-earth metal-mud, for subsequent use;
(4) titaniferous-dry glue of alkaline-earth metal-mud of preparation in step (3) is placed in electric furnace, under 850 DEG C of conditions, calcines 4-6h in air atmosphere, naturally cool to room temperature in stove, to obtain final product.
6. a kind of method utilizing mud to prepare porous titanate adsorbent according to claim 1, is characterized in that, comprise following processing step:
Get the excess sludge of new discharge, adjustment moisture content is 88.5%, is placed in and smashs to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, obtain homogenizing slurry; Take 1000g homogenizing slurry, under Keep agitation condition, dropwise add 500g titanium tetrachloride, after dripping, in 70 DEG C of sealed thermal insulating stirring reaction 60min, obtain titaniferous jelly, add 267g agstone, mix, stir 30min, be 3 with ammoniacal liquor adjust pH, agitating heating is evaporated, and finally dries under 105 DEG C of conditions, make titaniferous-dry glue of calcium-mud, be placed in cabinet-type electric furnace, under 850 DEG C of conditions, calcining 5h, naturally cools to room temperature in stove, obtains porous calcium titanate 1;
Above-mentioned agstone is containing calcium carbonate 99%, and particle diameter is 25 microns.
7. a kind of method utilizing mud to prepare porous titanate adsorbent according to claim 1, is characterized in that, comprise following processing step:
Get the excess sludge of new discharge, adjustment moisture content is 90%, is placed in and smashs to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, obtain homogenizing slurry; Take 1000g homogenizing slurry, under Keep agitation condition, dropwise add 250g titanium tetrachloride, after dripping, in 70 DEG C of sealed thermal insulating stirring reaction 90min, obtain titaniferous jelly; Add 134g agstone, mix, stirring 30min, is 3 with ammoniacal liquor adjust pH, agitating heating evaporate to dryness, finally dries under 105 DEG C of conditions, makes titaniferous-dry glue of calcium-mud, is placed in cabinet-type electric furnace, under 850 DEG C of conditions, calcining 5h, naturally cools to room temperature in stove, obtains porous calcium titanate 3;
Above-mentioned agstone is containing calcium carbonate 99%, and particle diameter is 25 microns.
8. a kind of method utilizing mud to prepare porous titanate adsorbent according to claim 1, is characterized in that, comprise following processing step:
Get the excess sludge of new discharge, adjustment moisture content is 92%, is placed in and smashs to pieces in refiner, with 4000r/min mixing speed, smash homogenate 10min to pieces, obtain homogenizing slurry; Take 1000g homogenizing slurry, under Keep agitation condition, dropwise add 500g titanium tetrachloride, after dripping, in 60 DEG C of sealed thermal insulating stirring reaction 30min, obtain titaniferous jelly; Add 267g agstone, mix, stirring 30min, is 2.5 with ammoniacal liquor adjust pH, agitating heating evaporate to dryness, finally dry under 105 DEG C of conditions, make titaniferous-dry glue of calcium-mud, be placed in cabinet-type electric furnace, under 650 DEG C of conditions, calcining 6h, naturally cools to room temperature in stove, obtains porous calcium titanate 4;
Above-mentioned agstone is containing calcium carbonate 99%, and particle diameter is 25 microns.
9. a kind of method utilizing mud to prepare porous titanate adsorbent according to claim 1, is characterized in that, comprise following processing step:
Get the excess sludge of new discharge, adjustment moisture content is 87%, is placed in and smashs to pieces in refiner, with 4000r/min mixing speed, smash homogenate 20min to pieces, obtain homogenizing slurry; Take 1000g homogenizing slurry, under Keep agitation condition, dropwise add 400g titanium tetrachloride, after dripping, in 80 DEG C of sealed thermal insulating stirring reaction 120min, obtain titaniferous jelly; Add 196g dolomite dust, mix, stirring 30min, is 4 with ammoniacal liquor adjust pH, agitating heating evaporate to dryness, finally dry under 110 DEG C of conditions, make titaniferous-calcium/dry glue of magnesium-mud, be placed in cabinet-type electric furnace, under 1000 DEG C of conditions, calcining 4h, naturally cools to room temperature in stove, obtains porous calcium titanate/magnesium compound adsorbent 1;
Above-mentioned dolomite dust is containing calcium carbonate 55.36%, and magnesium carbonate 44.10%, particle diameter is 23 microns.
10. a kind of method utilizing mud to prepare porous titanate adsorbent according to claim 1, is characterized in that, comprise following processing step:
Get the excess sludge of new discharge, adjustment moisture content is 87%, is placed in and smashs to pieces in refiner, with 4000r/min mixing speed, smash homogenate 15min to pieces, obtain homogenizing slurry; Take 1000g homogenizing slurry, under Keep agitation condition, dropwise add 1000g titanium tetrachloride, after dripping, in 70 DEG C of sealed thermal insulating stirring reaction 30min, obtain titaniferous jelly; Add 1045g brium carbonate powder, mix, stirring 30min, is 3 with ammoniacal liquor adjust pH, agitating heating evaporate to dryness, finally dries under 105 DEG C of conditions, makes titaniferous-dry glue of barium-mud, is placed in cabinet-type electric furnace, under 850 DEG C of conditions, calcining 5h, naturally cools to room temperature in stove, obtains porous barium titanate;
Above-mentioned brium carbonate is technical grade, content 99.5%, and particle diameter is 23 microns.
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Publication number Priority date Publication date Assignee Title
CN106962249A (en) * 2017-02-28 2017-07-21 沈阳理工大学 A kind of method that utilization excess sludge prepares multifunction manual reef
CN106962249B (en) * 2017-02-28 2021-05-11 沈阳理工大学 Method for preparing multifunctional artificial reef by using excess sludge

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