CN101693191A - Preparation method of meerschaum adsorbent capable of catalyzing oxidized regeneration - Google Patents
Preparation method of meerschaum adsorbent capable of catalyzing oxidized regeneration Download PDFInfo
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- CN101693191A CN101693191A CN200910114476A CN200910114476A CN101693191A CN 101693191 A CN101693191 A CN 101693191A CN 200910114476 A CN200910114476 A CN 200910114476A CN 200910114476 A CN200910114476 A CN 200910114476A CN 101693191 A CN101693191 A CN 101693191A
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Abstract
The invention discloses a preparation method of a meerschaum adsorbent capable of catalyzing oxidized regeneration, which comprises the following steps: firstly uniformly mixing 40-60 meshes of meerschaum after high temperature modification in a cobalt nitrate and ferric nitrate solution, then adjusting the pH value of the solution, immersing, flushing with distilled water until the solution is colorless, drying and finally calcining for more than 1 hour at the temperature of 450-750 DEG C to obtain the product. The meerschaum adsorbent capable of catalyzing oxidized regeneration has simple preparation process, low cost, difficult poisoning and inactivation, strong adsorption capacity for poisonous refractory biodegradation organic substances and extensive processed wastewater varieties. The adsorbent capable of catalyzing oxidized regeneration has greatly improved degradation ratio for the poisonous refractory biodegradation organic substances under high temperature airflow or air as compared with the degradation ratio for cobalt dioxide and ferric oxide without meerschaum load, the degradation ratio can reach 50-90 percent, and the invention overcomes the limitations that a conventional adsorbent can not be regenerated or recycled and the adsorbent has no catalytic capability.
Description
Technical field
The present invention relates to adsorbent, but specifically be a kind of preparation method of meerschaum adsorbent of catalyzing oxidized regeneration.
Background technology
In China, annual discharged volume of industrial waste water reaches 40,000,000,000 tons, and the section that half is arranged in the seven big water systems of the whole nation is by organic pollution or heavy metal pollution, and 86% section, city water pollution exceeds standard.At present, energy-saving and emission-reduction work is the important means of keeping economic sustainable fast development and the healthy and safe existence of human settlements, promotes energetically in all trades and professions.A large amount of synthetic organic pesticides, dyestuff, organic cyanide, polycyclic aromatic hydrocarbon, heterocycle compound, chlorinated aromatic compound, plasticizer etc. are poisonous, the material of bio-refractory and contain in the waste water that heavily contaminated manufacturing enterprise produced such as agricultural chemicals, printing and dyeing, petrochemical industry, coking, pharmacy, papermaking, processing to this class waste water now still lacks economy and practical efficiently treatment process, and this will aggravate the pollution of environment and seriously hinder sustainable economic development.
Handle the adsorption treatment method that this class technology poisonous, bio-refractory waste water mainly contains physics at present, traditional adsorbent mainly contains active carbon, and adsorbance is big, and the processing cycle is short, and selectivity is little, but the price height, and the required energy consumption of regenerating is big, is difficult to regeneration cycle and uses; Slag and cinder belong to twice laid, and treatment effeciency is low, are difficult to regeneration cycle and use, and produce secondary pollution.
Summary of the invention
The objective of the invention is in order to overcome conventional adsorbent production cost height, can not regeneration cycle use and adsorbent self does not possess the limitation of catalytic capability, and a kind of tool catalytic performance and reproducible preparation method of meerschaum adsorbent are provided.It is not only good to the organic degradation rate of poisonous bio-refractory under high temperature gas flow and air that but this preparation method has the catalyzing oxidized regeneration adsorbent, but repetitive cycling is used, because catalytic action also reduces and needed temperature and time when having reduced oxidizing process, save energy consumption, reduce cost.
The technical scheme that realizes the object of the invention is:
The present invention selects for use cheap, the sepiolite that itself has good rheological characteristic, heat endurance, dispersiveness and mechanical strength is as adsorbing agent carrier, load has the cobalt oxide and the iron oxide of catalytic performance, utilize high temperature modified poisonous, the bio-refractory organic matter of sepiolite absorption, oxidation absorption is poisonous, during the bio-refractory organic matter, the cobalt oxide of load and iron oxide play the concerted catalysis degradation, the simultaneous oxidation reproducing adsorbent has solved the difficult regeneration of adsorbent or the regeneration period is long and adsorbent does not have limitation such as catalyzing and degrading pollutant.
Preparation method of the present invention comprises the steps:
1, sepiolite is high temperature modified;
2, high temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, the pH value of regulating mixed solution is 1-2, soaks then and puts 12h;
3, soak to put and finish the back to wash sepiolite repeatedly with distilled water colourless to solution;
4, calcining was taken out cooling, but is promptly obtained this catalyzing oxidized regeneration adsorbent more than 1 hour in Muffle furnace.
Sepiolite described in the step 1 is high temperature modified to be prior art.
The addition scope of high temperature modified sepiolite is described in the step 2: high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.2-0.8: 10; The addition scope of cobalt nitrate and ferric nitrate is that cobalt nitrate and ferric nitrate mol ratio are 0.5-2.5: 1.
The pH value of described adjusting mixed solution is to be the sulfuric acid solution of 1mol/L with concentration.
Describedly soak that to put be that cobalt ions and iron ion are stated from the high temperature modified sepiolite by the method for ion-exchange and absorption is compound, preparation has the oxidable reproducing adsorbent of strong catalytic capability
Described flushing be will be free cobalt ions and iron ion remove, wash simultaneously to the pH value of solution and be neutrality.
Described temperature of calcining in Muffle furnace is 500-600 ℃.
Orthogonal experiment proves: this Effect Factors for Sythetic Technology has: 1, cobalt nitrate and ferric nitrate mol ratio; 2, high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio; 3, pH value of solution value; 4, soak the time of putting; 5, calcining heat; 6, calcination time, the size of its influence degree are the sepiolite of cobalt nitrate and ferric nitrate mol ratio＞high temperature modified and cobalt nitrate and ferric nitrate mass ratio＞calcining heat＞calcination time＞soak the time of putting＞the pH value of solution value.
The preferred parameter of this technology is that cobalt nitrate and ferric nitrate mol ratio are 2.0: 1, and high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.5: 10, and the pH value of solution value is 2, and soaking the time of putting is 12h, and calcining heat is 600 ℃, and calcination time is 3h.Under the preferred parameter condition, but catalyzing oxidized regeneration adsorbent reactivation rate is 80.26%.
The invention has the beneficial effects as follows that preparation technology is simple, cost is low, has activated catalyst in the time of the high-temperature oxydation adsorbate, and the catalyst of load is difficult for poisoning and deactivation, and to poisonous bio-refractory organic matter high adsorption capacity, it is extensive to handle kind of waste water.But should under high temperature gas flow and air, there be the degradation rate of sepiolite supported cobalt oxide and iron oxide to improve a lot by the catalyzing oxidized regeneration adsorbent to the organic degradation rate of poisonous bio-refractory, degradation rate all can reach 50%-90%, has overcome conventional adsorbent and can not regeneration cycle have used and adsorbent self does not possess the limitation of catalytic capability.But should the catalyzing oxidized regeneration adsorbent not only can repetitive cycling use, abandon the secondary pollution that causes after reducing adsorbents adsorb,, save energy consumption, reduce cost because catalytic action also reduces and needed temperature and time when having reduced oxidizing process.Simultaneously because the used carrier sepiolite itself has excellent properties such as good rheological characteristic, heat endurance, dispersiveness and mechanical strength, for the processing of poisonous bio-refractory organic wastewater provides new environment-friendly materials.
The specific embodiment
Embodiment 1
Preparation of adsorbent method of the present invention comprises the steps:
1, sepiolite is high temperature modified: 700 ℃ of calcining 1-5h get final product in Muffle furnace;
2, high temperature modified back 40-60 purpose sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, addition is that high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.2: 10, cobalt nitrate and ferric nitrate mol ratio are 0.5: 1, the pH value of regulating mixed solution is 1-2, soaks then and puts 12h;
3, soak to put and finish the back to wash sepiolite repeatedly with distilled water colourless to solution;
4, in Muffle furnace, calcine 3h under 550 ℃, take out cooling, but promptly obtain the adsorbent of catalyzing oxidized regeneration.
The test of adsorption capacity:
Getting the 15g adsorbent internal diameter of packing into is 22mm, and height is in the adsorption and high temperature airflow post of 400mm, is the flow velocity suction adsorption column of 116mL/h with peristaltic pump with the flow velocity with the crystal violet solution of 500mg/L, adopts and falls stream absorption.When go out water concentration greater than former crystal violet solution concentration 5% the time stop into water, prove that dyestuff has been adsorbed agent absorption.
The test of power of regeneration:
Under the situation of adsorption column overcoat heating, utilize high temperature gas flow to purge adsorbent again, the air velocity that air compressor is emitted is 1.5L/min, and air constantly purges adsorbent, and tail gas flows out from the gas outlet that can revolve capping.Constant temperature time is that 30min makes adsorbent reactivation after the temperature of heating jacket reaches established temperature, and then the method for testing of adsorption capacity tests, and test result is that adsorbent regeneration rate is 63.60%.
Embodiment 2
High temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, addition is that high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.5: 10, and all the other are with embodiment 1.According to surveying and determination, the absorption regeneration rate of adsorbent is 62.21%.
Embodiment 3
High temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, addition is that high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.2: 10, and cobalt nitrate and ferric nitrate mol ratio are 2.5: 1, and all the other are with embodiment 1.According to surveying and determination, the absorption regeneration rate of adsorbent is 72.03%.
Embodiment 4
High temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, addition is that high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.8: 10, cobalt nitrate and ferric nitrate mol ratio are 2.5: 1, all the other are with embodiment 1, according to surveying and determination, the absorption regeneration rate of adsorbent is 72.77%.
Embodiment 5
High temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, addition is that high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.2: 10, cobalt nitrate and ferric nitrate mol ratio are 1.5: 1, calcine 3h down for 500 ℃ in Muffle furnace, and all the other are with embodiment 1.According to surveying and determination, the absorption regeneration rate of adsorbent is 73.44%.
Embodiment 6
High temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, addition is that high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.2: 10, cobalt nitrate and ferric nitrate mol ratio are 1.5: 1, calcine 3h down for 600 ℃ in Muffle furnace, and all the other are with embodiment 1.According to surveying and determination, the absorption regeneration rate of adsorbent is 64.32%.
Embodiment 7
High temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, addition is that high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.8: 10, cobalt nitrate and ferric nitrate mol ratio are 1.5: 1, calcine 3h down for 500 ℃ in Muffle furnace, and all the other are with embodiment 1.According to surveying and determination, the absorption regeneration rate of adsorbent is 70.15%.
Embodiment 8
High temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, addition is that high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.8: 10, cobalt nitrate and ferric nitrate mol ratio are 1.5: 1, calcine 3h down for 600 ℃ in Muffle furnace, and all the other are with embodiment 1.According to surveying and determination, the absorption regeneration rate of adsorbent is 68.48%.
Embodiment 9
High temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, addition is that high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.5: 10,500 ℃ of calcining 3h down in Muffle furnace, and all the other are with embodiment 1.According to surveying and determination, the absorption regeneration rate of adsorbent is 63.17%.
Embodiment 10
High temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, addition is that high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.5: 10, cobalt nitrate and ferric nitrate mol ratio are 2.5: 1, calcine 3h down for 500 ℃ in Muffle furnace, and all the other are with embodiment 1.According to surveying and determination, the absorption regeneration rate of adsorbent is 76.52%.
Embodiment 11
High temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, addition is that high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.5: 10, cobalt nitrate and ferric nitrate mol ratio are 0.5: 1, calcine 3h down for 600 ℃ in Muffle furnace, and all the other are with embodiment 1.According to surveying and determination, the absorption regeneration rate of adsorbent is 64.88%.
Embodiment 12
High temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, addition is that high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.5: 10, cobalt nitrate and ferric nitrate mol ratio are 2.5: 1, calcine 3h down for 600 ℃ in Muffle furnace, and all the other are with embodiment 1.According to surveying and determination, the absorption regeneration rate of adsorbent is 75.15%.
Embodiment 13
High temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, addition is that high temperature modified sepiolite and cobalt nitrate and ferric nitrate mass ratio are 0.5: 10, and cobalt nitrate and ferric nitrate mol ratio are 1.5: 1, and all the other are with embodiment 1.According to surveying and determination, the absorption regeneration rate of adsorbent is 78.43%.
Claims (7)
1. but the preparation method of meerschaum adsorbent of a catalyzing oxidized regeneration is characterized in that: comprise the steps:
(1) sepiolite is high temperature modified;
(2) high temperature modified sepiolite is joined in the mixed solution of cobalt nitrate and ferric nitrate, the pH value of regulating mixed solution is 1-2, soaks then and puts 12h;
(3) soak to put and finish the back to wash sepiolite repeatedly with distilled water colourless to solution;
(4) calcining was taken out cooling more than 1 hour in Muffle furnace, promptly obtained the regenerable sorbent of tool catalytic oxidation performance.
2. preparation method as claimed in claim 1 is characterized in that: sepiolite that described adding is high temperature modified and cobalt nitrate and ferric nitrate mass ratio are 0.2-0.8: 10.
3. preparation method as claimed in claim 2 is characterized in that: sepiolite that described adding is high temperature modified and cobalt nitrate and ferric nitrate mass ratio are 0.5: 10.
4. preparation method as claimed in claim 1 is characterized in that: described cobalt nitrate and ferric nitrate mol ratio are 0.5-2.5: 1.
5. preparation method as claimed in claim 4 is characterized in that: described cobalt nitrate and ferric nitrate mol ratio are 2.0: 1.
6. preparation method as claimed in claim 1 is characterized in that: the pH value of described adjusting mixed solution is 2.
7. preparation method as claimed in claim 1 is characterized in that: the described 3h that calcines under 500-600 ℃ in Muffle furnace.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104525097A (en) * | 2014-12-02 | 2015-04-22 | 广西师范大学 | Preparation method of Ce-Ni double-metal-loading sepiolite adsorption-catalyst |
| CN106040164A (en) * | 2016-06-27 | 2016-10-26 | 安徽金联地矿科技有限公司 | Water body eutrophication ion attapulgite adsorbent |
| CN109022097A (en) * | 2018-07-09 | 2018-12-18 | 安徽冠建新能源科技有限公司 | A kind of additive improving biology burning matter particle burning degree |
| CN112111977A (en) * | 2020-07-28 | 2020-12-22 | 浙江锶通净新材料有限公司 | Flame-retardant transition metal oxide sepiolite composite material, and preparation method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MX2007003775A (en) * | 2007-03-29 | 2008-10-28 | Mexicano Inst Petrol | Process for preparing multimetallic anionic clays and products thereof. |
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2009
- 2009-10-18 CN CN2009101144767A patent/CN101693191B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104525097A (en) * | 2014-12-02 | 2015-04-22 | 广西师范大学 | Preparation method of Ce-Ni double-metal-loading sepiolite adsorption-catalyst |
| CN104525097B (en) * | 2014-12-02 | 2017-03-15 | 广西师范大学 | A kind of Ce Ni bimetallics load the preparation method of meerschaum adsorption catalyst |
| CN106040164A (en) * | 2016-06-27 | 2016-10-26 | 安徽金联地矿科技有限公司 | Water body eutrophication ion attapulgite adsorbent |
| CN109022097A (en) * | 2018-07-09 | 2018-12-18 | 安徽冠建新能源科技有限公司 | A kind of additive improving biology burning matter particle burning degree |
| CN112111977A (en) * | 2020-07-28 | 2020-12-22 | 浙江锶通净新材料有限公司 | Flame-retardant transition metal oxide sepiolite composite material, and preparation method and application thereof |
| CN112111977B (en) * | 2020-07-28 | 2022-08-05 | 浙江锶通净新材料有限公司 | Flame-retardant transition metal oxide sepiolite composite material, and preparation method and application thereof |
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