CN102258974A - Preparation method and use of porous titanate integrated composite column - Google Patents
Preparation method and use of porous titanate integrated composite column Download PDFInfo
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Abstract
The invention discloses a preparation method and use of a porous titanate integrated composite column. The porous titanate integrated composite column is prepared by using ceramic fibers as a supporting skeleton and cotton as template agent and by suing a sol-gel process. The preparation method comprises the following steps: cutting ceramic fiber paper into rectangles of a proper area, and spreading cotton into a thin sheet of the same area as the ceramic fiber paper; preparing solution of titanate by using nitrates of one or two of tetrabutyl titanate and alkaline earth as raw material; soaking the ceramic fiber paper and the cotton sheet into sol respectively, taking the ceramic fiber paper and the cotton sheet out, overlapping the ceramic fiber paper and the cotton sheet with the ceramic fiber paper on the outer side, and coiling to make compact multi-layer composite small column; drying the composite column at 105 DEG C, calcining at 600 to 900 DEG C, removing a cotton template, converting titanate gel into porous tubular titanate, and thus obtaining the integrated composite column in which the ceramic fiber and the porous titanate are alternatively arranged. The column has intercommunicated pores. The ceramic fiber-titanate composite porous integrated column disclosed by the invention can be used for enriching and separating trace amount of heavy metals in field of analysis and deeply purifying heavy metals in water in field of water treatment.
Description
Technical field
The present invention relates to analytical chemistry and water treatment field, relate to the preparation of porous integral post, specifically, relate to whole combined column of POROUS TITANIUM hydrochlorate that heavy metal purifies in separation and concentration in the analytical chemistry and the drinking water and preparation method thereof.
Background technology
Because the toxicity of heavy metal and the property accumulated in vivo, strict regulation has all been done to the content of beary metal in water and the food etc. in countries in the world.At present, mainly adopt atomic absorption method and ICP method for Determination of Heavy Metal.Though the sensitivity of these two kinds of methods is very high,, for low content or the sample of serious interference still needs Preconcentration and Separation.Enrichment and separation method commonly used has liquid-liquid extraction method, chelate extraction method, ionic liquid preenrichment method, chemical coprecipitation, ion-exchange and cloud point extraction method etc.In these methods, what have uses poisonous and hazardous reagent, the cost height that has, and the poor stability that has, the complex operation that has, the enrichment factor that has is lower.And the method that adopts usually for the heavy metal deep purifying in the water is counter-infiltration (RO) method, but the RO film cost height that this method is used, and in the purge process of water, need consumed power, can produce a large amount of concentrated water discharges simultaneously, waste water resource.In recent years, in water in the concentration and separation field of heavy metal, adsorption and enrichment partition method (SPE) with its have simple to operate, pollution-free, enrichment factor is high, speed is fast and be convenient to and advantages such as other technology coupling, extensive use in practice.And in water aspect the heavy metal processing, absorption method is because of its non-secondary pollution, and regeneration is convenient, is easy to reclaim advantages such as utility, also is subjected to extensive concern.
At present, in absorption method, from sorbing material, sorbing material commonly used has resin, active carbon, ion marking chelate, natural minerals, microbial material etc., but in these materials, is used on the concentration and separation, the enrichment factor that has is lower, synthesis technique that has and condition harshness, complicated operation, agents useful for same costliness; Be used in the water treatment, the disposal ability that has is limited, the cost height that has, the reclaiming poor performance that has.Along with the development of nanosecond science and technology, nano material has caused people's great attention.The inventor, preamble (Zhang Dong etc., " spectroscopy and spectrum analysis ",, 28 volumes, 1 phase, 218-221 page or leaf in 2008; Zhang Dong etc., " chemical journal ", 2009,67 volumes, 12 phases, the 1336-1342 page or leaf) research confirms: compare with adsorbent commonly used, Nano titanate powders such as nano barium-strontium titanate and nano barium titanate calcium because it has special surface nature and high specific area, have stronger absorption and accumulation ability to heavy metal ion in the water, has faster adsorption rate, the wider scope of application, and the titanate adsorption capacity is big, and chemical stability is good, renovation process is simple, is a kind of very desirable heavy metal absorption and enrichment material.On absorption and enrichment mode: preface commonly used is criticized method and enrichment (absorption) post method.Because preface is criticized the method complicated operation, is unfavorable for automatic control, seldom use in the reality.The post method is easy and simple to handle with it, rate of recovery height, and good reproducibility is easy to regeneration, can realize advantages such as online concentration and separation and purification, has been used for the concentration and separation and the water treatment field of heavy metal.But adopt packed column at present mostly, but, packed column generally just is used for oarse-grained sorbing materials such as resin, and for the tiny nano-powder materials such as Nano titanate of particle, shortcoming such as existing powder easily runs off, and the pillar resistance is big, can't satisfy fast, efficiently, high flux, the requirement of high enrichment factor or high detergent power.The porous integral post itself has the micropore of mutual perforation, has good permeability, can avoid the shortcoming of nano-powder packed column.But at present, what can access integral post has only seldom number several such as monolithic silica column, and these integral post generally itself do not possess adsorption function, can only be as the carrier post, and synthetic cost height, chemical stability and mechanical strength are all lower, and the Nano titanate that will possess splendid absorption and enrichment performance is made the porous integral post, does not appear in the newspapers.But the bad mechanical strength of titanate own can not self form the porous post.
The present invention utilizes ceramic fibre as support frame, in order to improve the mechanical strength of integral post; With the cotton fiber is the template agent, preparation permeability duct, and increase surface area.Adopt Prepared by Sol Gel Method to duplicate the composite monolithic post of the void channels of cotton fiber pattern.Be used for the removal of heavy metal in the water of the concentration and separation of analysis field trace heavy metal and water treatment field.
Summary of the invention
In order to remedy the shortcoming of common adsorbent and nano-powder packed column, preparation POROUS TITANIUM hydrochlorate integral post, it is strong to obtain the adsorption and enrichment ability, the enrichment that mechanical strength is high (absorption) post, satisfy quick that modern separation and concentration and water purify, efficient, high flux, the requirement of high enrichment factor or high detergent power, the invention provides a kind of POROUS TITANIUM hydrochlorate composite monolithic post and be used for the preenrichment of water heavy metal and water in the deep purifying of heavy metal.
The technical scheme that adopts:
The whole combined column of a kind of POROUS TITANIUM hydrochlorate is characterized in that: this integral post is to be made of with the perforation titanate pipeline that has duplicated the cotton fiber structure the ceramic fibre as support frame.Be cross-linked with each other by micropore between its penetrability duct wall, form permeable structures, the pore aperture is at 5 μ m ~ 20 μ m.Ceramic fibre skeleton surface coverage one deck Nano titanate, duct wall also is made up of Nano titanate crystal grain, and the titanate crystals particle diameter is all at 20nm ~ 100nm.Described titanate is a kind of in calcium titanate, strontium titanates, barium strontium titanate, the barium titanate.It is 5mm-20mm that the porous post is of a size of diameter of phi, and length is generally at 2cm-30cm.
Whole combined column preparation method of POROUS TITANIUM hydrochlorate and application thereof may further comprise the steps:
(1) ceramic fiber paper (thickness 0.5mm) is cut into the square of suitable area, in 900 ℃ of calcination 2h, cool to room temperature soaks activation 30 min in 6mol/L hydrochloric acid, be washed to nearly neutrality, 105 ℃ of oven dry;
(2) cotton fiber is paved into and the thin slice of (1) described ceramic fiber paper equal area and shape (thickness 0.5mm ~ 1.0mm);
(3) preparation of titanate colloidal sol: take by weighing a certain amount of calcium nitrate (strontium nitrate, barium nitrate) and citric acid and dissolve in the absolute ethyl alcohol, magnetic agitation 30 min obtain the precursor solution of metal ion.Under vigorous stirring, a certain amount of butyl titanate is dissolved in the absolute ethyl alcohol, continue to stir, behind 30 min, drip a certain amount of glacial acetic acid, form Ti (IV) precursor solution.The precursor solution that mixes Ti (IV) and metal ion, make that citric acid and total alkaline-earth metal ion mol ratio are 2: 1, titanium is 1:1 with total alkaline-earth metal ion mol ratio, if strontium titanates/barium, then the mol ratio of barium, strontium and titanium is 0.5:0.5:1, the polyethylene glycol 1500 aqueous solution that adds a certain amount of 30g/L, the pH value of transferring solution with ammoniacal liquor or glacial acetic acid continues to stir 1 h and promptly gets titanate colloidal sol to 3-4.
(4) (1) described ceramic fiber paper of handling well and (2) described cotton fiber be impregnated in 30min in (3) described colloidal sol respectively, take out back two superimposed, the ceramic fibre ply of paper outside, be rolled into the MULTILAYER COMPOSITE pillar of consolidation, in 105 ℃ of oven dry, 600 ℃ ~ 900 ℃ calcining 6h, remove the cotton fiber template, the titanate gel changes into the perforated tubular titanate, naturally cools to room temperature, has obtained the ceramic fibre whole combined column alternate with the POROUS TITANIUM hydrochlorate.
(5) absorption that can be used for heavy metal in the Preconcentration and Separation of trace heavy metal in the analysis field and the water treatment field of the whole combined column of POROUS TITANIUM hydrochlorate is removed.
The invention has the advantages that:
The enriching column advantage of this method preparation is that it has possessed the mechanical strength of ceramic fibre simultaneously, the high stability of the through tube of cotton fiber template and bigger serface and titanate and high absorption property, preparation technology is simple, adsorption capacity to heavy metal ion is big, the enrichment factor height, detergent power is strong, and reproducibility is good, stable performance, it is many to be suitable for the heavy metal ion kind.
The specific embodiment
By example method of the present invention and technology are illustrated:
Embodiment one
Preparation process with nano barium titanate calcium porous integral combined column is an example, is described in detail as follows:
(1) ceramic fiber paper (thickness 0.5mm) is cut into the rectangle of a * b=60mm * 50mm, in 900 ℃ of calcination 2h, cool to room temperature soaks activation 30min in 6mol/L hydrochloric acid, be washed to nearly neutrality, 105 ℃ of oven dry;
(2) take by weighing 0.2 g cotton fiber and be paved into thin slice with (1) described ceramic fiber paper equal area and shape.
(3) preparation of titanate colloidal sol: the four water-calcium nitrate and the 52.5g citric acid that take by weighing 59 g are dissolved in the 200mL absolute ethyl alcohol, and magnetic agitation 30 min obtain Ca
2+Solution.Under vigorous stirring, the 85g butyl titanate is dissolved in the 90mL absolute ethyl alcohol, continue to stir, behind 30 min, drip the 330mL glacial acetic acid, form Ti (IV) precursor solution.Under the stirring condition, with Ca
2+Solution slowly is added dropwise in the presoma of Ti (IV), drips the polyethylene glycol 1500 aqueous solution 200mL of 30g/L again, transfers pH 3-4 with ammoniacal liquor or nitric acid, continues to stir 1 h and promptly gets titanate colloidal sol.
(4) (1) described ceramic fiber paper of handling well and (2) described cotton fiber be impregnated in 30min in (3) described colloidal sol respectively, take out back two superimposed, the ceramic fibre ply of paper outside, be rolled into the MULTILAYER COMPOSITE pillar (is column length with the b limit) of consolidation, in 105 ℃ of oven dry, 900 ℃ of calcining 6h, remove the cotton fiber template, the calcium titanate gel changes into the perforated tubular calcium titanate, naturally cools to room temperature, has obtained the ceramic fibre whole composite enrichment post alternate with the porous calcium titanate.
(5) (4) described porous integral post is packed into the length that internal diameter is fit to is in the glass tube of 60mm, clog with glass fibre cotton at two ends, one end is connected with separatory funnel (volume is 1L) end opening with adapter of plastic, be fixed on the iron stand with extension clamp, nitric acid 50mL with 2mol/L, the washing pillar is washed till neutrality with distilled water again, and is stand-by.
Embodiment two
With the heavy metal lead is the application of example explanation nano barium titanate calcium porous integral combined column in concentration and separation:
The lead mark liquid 1L of preparation 50ug/L, adjust pH adds embodiment 1(5 greater than 4) in the separatory funnel of device, make solution with the flow velocity of 10mL/min by enriching column, with 100mL distilled water washing enriching column, remove the lead that is not adsorbed.Outflow liquid with 1mL/min flow velocity wash-out lead, is accepted with test tube with 5mL2mol/L nitric acid in the absorption back, and with the content of NITRATE BY FLAME ATOMIC absorption measurement lead, calculate recovery rate is 97.2%.
Embodiment three
It is as follows that nano barium titanate calcium porous integral combined column is removed applying step to the absorption of heavy metal lead in the water:
The lead mark liquid 2L of preparation 10mg/L, adjust pH adds in the separatory funnel of embodiment 1 device greater than 4, makes solution pass through enriching column with the flow velocity of 20mL/min, flows out content plumbous in the liquid with the NITRATE BY FLAME ATOMIC absorption measurement, and the result is not for detecting.
Embodiment four
Use the regeneration step of back pillar as follows:
With the pillar after using in embodiment 2 and 3, the nitric acid 50mL with 2mol/L crosses post with the 5mL/min flow velocity, is washed till nearly neutrality with distilled water again, promptly finishes regeneration.
Claims (4)
1. the preparation method and the application of the whole combined column of POROUS TITANIUM hydrochlorate is characterized in that: this integral post is to be made of with the titanate pipeline that runs through that has duplicated the cotton fiber structure the ceramic fibre as support frame.
2. the preparation method and the application of the whole combined column of a kind of POROUS TITANIUM hydrochlorate according to claim 1, it is characterized in that: be to support raw material with the ceramic fiber paper, with the cotton fiber is the template agent, adopt the porous integral combined column of Prepared by Sol Gel Method, be cross-linked with each other by micropore between its penetrability duct wall, form permeable structures, the pore aperture is at 5 μ m-20 μ m.
3. the preparation method and the application of the whole combined column of a kind of POROUS TITANIUM hydrochlorate according to claim 1 and 2, it is characterized in that: ceramic fibre skeleton surface is covered by Nano titanate, duct wall also is made up of Nano titanate crystal grain, the titanate crystals particle diameter is at 20nm-100nm, and described titanate is a kind of in calcium titanate, strontium titanates, barium strontium titanate, the barium titanate.
4. the preparation method and the application of the whole combined column of a kind of POROUS TITANIUM hydrochlorate according to claim 1 may further comprise the steps:
(1) ceramic fiber paper (thickness 0.5mm) is cut into the square of suitable area, in 900 ℃ of calcination 2h, cool to room temperature soaks activation 30min in 6mol/L hydrochloric acid, be washed to nearly neutrality, 105 ℃ of oven dry;
(2) cotton fiber is paved into the thin slice with (1) described ceramic fiber paper equal area and shape;
(3) preparation of titanate colloidal sol: under vigorous stirring, butyl titanate is introduced in the hydrogen peroxide solution of citric acid, pH3-4 with the ammoniacal liquor regulator solution, stir certain hour under the uniform temperature and form Ti (IV) precursor solution, respectively with calcium (or strontium/barium, or strontium, or barium) nitrate is dissolved in the lemon acid solution, form the precursor solution of stable metal ion, the precursor solution that mixes Ti (IV) and alkaline-earth metal ions, make that citric acid and total alkaline-earth metal ion mol ratio are 2: 1, if strontium titanates/barium, barium then, the mol ratio of strontium and titanium is 0.5:0.5:1, continues to stir 1 h and promptly gets titanate colloidal sol;
(4) (1) described ceramic fiber paper of handling well and (2) described cotton fiber be impregnated in 30min in (3) described colloidal sol respectively, take out back two superimposed, the ceramic fibre ply of paper outside, be rolled into the MULTILAYER COMPOSITE pillar of consolidation, in 105 ℃ of oven dry, 600 ℃ of-900 ℃ of calcination 6h remove the cotton fiber template, the titanate gel changes into the perforated tubular titanate, has obtained the ceramic fibre whole combined column alternate with the POROUS TITANIUM hydrochlorate;
(5) the whole combined column of POROUS TITANIUM hydrochlorate can be used for the adsorption cleaning of heavy metal in the Preconcentration and Separation of trace heavy metal in the analysis field and the water treatment field.
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| CN102921236A (en) * | 2011-12-23 | 2013-02-13 | 成都杰丽净水设备有限公司 | Lightweight type filtration material for water treatment |
| CN105000626A (en) * | 2015-06-26 | 2015-10-28 | 中山大学 | Method for reinforcing piezoelectric effect to improve organic pollutant degradation efficiency and application thereof |
| CN110208258A (en) * | 2019-06-19 | 2019-09-06 | 沈阳理工大学 | Catalytic digestion column and its preparation method, CODCrRapid determination device and its make method |
| CN110280045A (en) * | 2019-06-19 | 2019-09-27 | 沈阳理工大学 | Catalytic digestion concentration and separation column and Catalytic digestion concentration and separation cup and preparation method thereof |
| CN111018564A (en) * | 2019-12-27 | 2020-04-17 | 苏州尼普环境科技有限公司 | Piezoelectric catalytic porous ceramic material, preparation method and application thereof |
| CN112958127A (en) * | 2021-02-26 | 2021-06-15 | 上海大学材料基因组工程(萍乡)研究院 | Method for loading catalyst on ceramic fiber |
| CN115155535A (en) * | 2022-07-11 | 2022-10-11 | 辽宁华泰环保科技集团有限公司 | Resin nano titanate composite microsphere and preparation method thereof for adsorption steam thermal hydrolysis |
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| CN102921236A (en) * | 2011-12-23 | 2013-02-13 | 成都杰丽净水设备有限公司 | Lightweight type filtration material for water treatment |
| CN105000626A (en) * | 2015-06-26 | 2015-10-28 | 中山大学 | Method for reinforcing piezoelectric effect to improve organic pollutant degradation efficiency and application thereof |
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| CN110280045A (en) * | 2019-06-19 | 2019-09-27 | 沈阳理工大学 | Catalytic digestion concentration and separation column and Catalytic digestion concentration and separation cup and preparation method thereof |
| CN110208258B (en) * | 2019-06-19 | 2021-09-24 | 沈阳理工大学 | Catalytic digestion column, preparation method thereof and CODCrRapid measuring apparatus and method of using the same |
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| CN111018564A (en) * | 2019-12-27 | 2020-04-17 | 苏州尼普环境科技有限公司 | Piezoelectric catalytic porous ceramic material, preparation method and application thereof |
| CN112958127A (en) * | 2021-02-26 | 2021-06-15 | 上海大学材料基因组工程(萍乡)研究院 | Method for loading catalyst on ceramic fiber |
| CN112958127B (en) * | 2021-02-26 | 2023-03-31 | 上海大学材料基因组工程(萍乡)研究院 | Method for loading catalyst on ceramic fiber |
| CN115155535A (en) * | 2022-07-11 | 2022-10-11 | 辽宁华泰环保科技集团有限公司 | Resin nano titanate composite microsphere and preparation method thereof for adsorption steam thermal hydrolysis |
| CN115155535B (en) * | 2022-07-11 | 2023-07-25 | 辽宁华泰环保科技集团有限公司 | Resin nano titanate composite microsphere and preparation method for adsorption steam thermal hydrolysis thereof |
| CN115282772A (en) * | 2022-08-04 | 2022-11-04 | 安徽元琛环保科技股份有限公司 | Preparation method of dust removal and denitration integrated ceramic filter cylinder and prepared ceramic filter cylinder |
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