CN102260068A - Preparation method of ceramic membrane with adsorption and retention functions - Google Patents
Preparation method of ceramic membrane with adsorption and retention functions Download PDFInfo
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- CN102260068A CN102260068A CN2010101861936A CN201010186193A CN102260068A CN 102260068 A CN102260068 A CN 102260068A CN 2010101861936 A CN2010101861936 A CN 2010101861936A CN 201010186193 A CN201010186193 A CN 201010186193A CN 102260068 A CN102260068 A CN 102260068A
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Abstract
The invention provides a preparation method of a novel ceramic membrane with adsorption and retention functions. In the preparation method, modern adsorption technology and membrane technology are combined to prepare the novel ceramic membrane from attapulgite. The preparation method comprises the following steps: uniformly mixing attapulgite with deionized water to obtain a paste, pouring the paste into a mold, and pressing into a round ceramic sheet; firstly aging the ceramic sheet in an humidity-constant environment for 3-7 days, taking out, drying in the natural environment in a laboratory for 2-5 days, sending to a muffle furnace for calcination, and after cooling, polishing the surface of the ceramic sheet to be smooth with sandpaper; and preparing a sulfuric acid solution with a pH value of 2-6, immersing the ceramic sheet into the solution, taking out after 8-24 hours, washing, then soaking in deionized water for 8-24 hours, and drying in a dust-removed environment to prepare the ceramic membrane. The obtained ceramic membrane has a pore size of 10-70 nm, has both adsorption and retention functions, can adsorb and trap organic large molecules, and has a good adsorption effect on small organic molecules and metal ions, thereby having the industrial promotion value.
Description
Technical field
The invention belongs to technical field of waste water processing, be particularly related to a kind of preparation of new ceramics film, this new ceramics film has absorption property simultaneously and holds back function, is applicable to that printing and dyeing wait the processing of organic wastewater with difficult degradation thereby, also are applicable to the condensed water in high temperature of processing after electrocatalysis.
Background technology
Current water resources is exhausted just day by day and polluted, and reasonable development and protection water resources are very necessary and urgent.Industry organic waste waters such as printing and dyeing, pharmacy, agricultural chemicals are difficult to by degradation by bacteria, are the difficult problems of current wastewater treatment, and ceramic membrane has series of advantages is applied it on water technology.
Chinese invention patent " gradient ceramic-film tube and preparation method thereof " (00117221.2) is made slurry with base-material and water-soluble binder stirring, be injected in the rigidity periosteum and make green compact, obtain ceramic-film tube through the demoulding, sintering, cooling, membrane pore size is 0.05-20 μ m." ceramic film pretreatment method in the sea water desaltination " (application number 200510041360.7), the ceramic membrane that with the aperture is 10-100nm carries out pre-treatment to seawater, be forced into 0.1-0.8MPa, seawater enters the ceramic membrane filter unit, the material that is not filtered is trapped within charging one side, realizes separating and filtering." a kind of method of extracting soybean protein isolate " (application number 200510019452.5) is the ceramic membrane filter protein emulsion friendship film system of 20-40nm with the aperture, holds back products such as oligose wherein, and filtrate is the albumin milk clear water.
Above-mentioned ceramic membrane is all just used its crown_interception, lacks adsorption function, and separation performance depends primarily on the aperture of film, and the aperture is more little, and the particle diameter that film is held back particle is also more little, and corresponding membrane resistance is also big more, and membrane flux is also more little, and energy consumption is also big more.
Attapulgite has been developed the product of the above purposes of over thousands of kind abroad owing to its special construction has good adsorption performance and adhesive property.Chinese patent " Attapulgite sewage-treating agent and production method " is raw material with the Attapulgite (200410041493.X), dries after the acidification, adds alum and the common abrasive dust of treated starch and makes sewage-treating agent." a kind of technology of preparing activated bleaching clay from attapulgite clay " (94117432.8) are main raw material with the attapulgite, mix with an amount of dilute acid soln, activate under the room temperature, make activated Fuller earth after the drying and crushing.Present STUDY ON THE APPLICATION OF ATTAPULGITE CLAY also just is confined to Powdered, and the research of making ceramic membrane yet there are no report.
The present invention utilizes attapulgite to prepare a kind of ceramic membrane that has absorption and hold back dual-use function modern adsorption technology and membrane technique combination.The essential distinction of this film and existing membrane technique is, not only has the function of holding back, and has adsorption function, can handle than small-particle with larger aperture, thereby obtain to reduce membrane resistance, increase membrane flux and energy-saving effect.
Summary of the invention
The object of the present invention is to provide a kind of preparation method who has absorption property and hold back the new ceramics film of function, this new ceramics film is specially adapted to handle high chroma, high COD used water difficult to degradate, also be applicable to iron ion and oil in the condensed water in high temperature of processing after electrocatalysis, make the waste water after the processing reach discharging standards.With modern adsorption technology and membrane technique combination, reach energy saving purposes.
A kind of preparation method who has absorption property and hold back the new ceramics film of function provided by the invention is a raw material with the attapulgite, makes through slurrying moulding, high-temperature calcination, polishing, aftertreatment and drying, and concrete steps and method are as follows:
A: 100～300 purpose attapulgites are mixed with deionized water, under mechanical stirring, mix, slowly pour forming mould compression moulding into, make the round sheet pottery of 1～2cm thickness after the demoulding to pasty state.
B: the ceramic plate that is prefabricated into ageing 3～7 days in the constant humidity environment earlier, taking-up under physical environment dry 2～5 days, drying temperature is 10～40 ℃, the interior free surface moisture of ceramic plate evenly is dried to fully, deliver to the retort furnace calcining, calcining temperature is 200～600 ℃, and soaking time is 0.5～6h, heat-up rate is 0.5～6 ℃/min, and cooling rate is 1～3 ℃/min.The cooling back is smooth with surface finish with sand paper.Remove ceramic plate surface dirt and residual powder with soft writing brush.
C: the sulphuric acid soln of configuration pH value 2～6.Ceramic membrane is immersed taking-up after 8～24 hours in this solution, wash repeatedly through deionized water, soaked 8～24 hours with deionized water, dedusting environment dry 6～9 days is down made ceramic membrane.
The new ceramics film of the present invention's preparation has the advantage of following uniqueness:
(1) ratio and the drying system etc. of the present invention by control attapulgite and deionized water prepared the new ceramics film that has absorption property and hold back function.And by control calcining temperature, temperature rise rate and soaking time, pyroprocessing new ceramics film, optimize the internal structure of ceramic membrane, adjust its pore size distribution, strengthen absorption property and hold back function, the new ceramics membrane pore size of preparing distributes narrow, between 10～70nm, voidage is 35%～65%, and water flux is 150～300L/m
2* h, this new ceramics film is a ceramic super-filtering film.
(2) the present invention preparation has absorption and holds back the new ceramics film treatment of dyeing and printing of function, adopts membrane filtering method, and water outlet COD value drops to below the 100mg/L, reaches national grade one discharge standard.This invention material can repeat repeatedly to use simultaneously, the non-secondary pollution problem.
(3) iron ion and the oil in the condensed water in high temperature of processing after electrocatalysis, iron ion content is 1～2mg/L in the preceding water of processing, and oleaginousness is 4～6mg/L, and experimental temperature is between 50～90 ℃, and after the new ceramics film was handled, the content of iron was below 0.3mg/L; Oleaginousness all reaches the oiler feed water quality requirement less than 2mg/L.The iron ion particle diameter is 0.134～0.164nm, less than the aperture of film, illustrates that removing the middle iron ion that anhydrates is because the adsorption of film.This new ceramics film decapacitation absorption is held back outside the organic macromolecule, and small organic molecule and metal ion are also had the good adsorption effect.
(4) the method efficient height that has absorption and hold back the new ceramics film processing waste water of function of the present invention, working conditions is loose, and adaptability is strong, applied range, floor space is little, can reuse.Be applicable to the processing of high chromas such as dyeing waste water, high-COD waste water, also be applicable to iron ion and oil handling in the condensed water in high temperature after electrocatalysis.
(5) the present invention prepares a kind of ceramic membrane that has absorption and hold back dual-use function with modern adsorption technology and membrane technique combination, reaches energy saving purposes.The preparation method who is adopted is simple, and controllability is strong, can be used for suitability for industrialized production.
Description of drawings
Fig. 1 is the embodiment 1 described graph of pore diameter distribution that has absorption and hold back the new ceramics film of function;
Embodiment
Embodiment 1
(1) attapulgite with 8.345g mixes with the 10ml deionized water, and at room temperature mechanical stirring mixes to pasty state, slowly pours mould compression moulding into, is prefabricated into diameter 2.9cm after the demoulding, and thickness is the round sheet pottery of 1.3cm.
(2) prefabricated ceramic plate ageing 5 days in the constant humidity environment was taken out under physical environment dry 3 days, and the interior free surface moisture of ceramic plate evenly is dried to fully.
(3) deliver to the retort furnace high-temperature calcination, initial temperature is 50 ℃, and the calcining outlet temperature is 350 ℃, and heat-up rate is 1.5 ℃/min, and soaking time is 2h, and cooling rate is 1 ℃/min.
(4) the cooling back is smooth with surface finish with 120#～360# sand paper.Remove ceramic plate surface dirt and residual powder with soft writing brush.
(5) configuration pH value is 4 sulphuric acid soln, ceramic membrane is immersed this solution take out after 12 hours, washes repeatedly through deionized water, soaks 12 hours with deionized water again, and dedusting environment dry 7 days is down made ceramic membrane.
The new ceramics membrane pore size that makes is distributed in 10～70nm, and voidage is 35%～65%, and water flux is 150～300L/m
2* h is ceramic super-filtering film.
Adopting membrane filtering method to handle COD is 250～450mol/L, and colourity is the dyeing waste water of 80～120PCU, and experimental temperature is a room temperature, water outlet COD＜90mol/L, colourity＜36PCU.
Adopting membrane filtering method to handle iron ion content is 1.1mg/L, and oleaginousness is the condensed water in high temperature of 4.5mg/L, and experimental temperature is between 50～90 ℃, and the content of water outlet iron is 0.2mg/L, and oleaginousness is 1.4mg/L, reaches the oiler feed water quality requirement.
Embodiment 2
(1) attapulgite with 8.297g mixes with the 10ml deionized water, and at room temperature mechanical stirring mixes to pasty state, slowly pours mould compression moulding into, is prefabricated into diameter 2.9cm after the demoulding, and thickness is the round sheet pottery of 1.3cm.
(2) ageing 7 days in the constant humidity environment earlier of the ceramic plate that is prefabricated into was taken out under physical environment dry 5 days, and the interior free surface moisture of ceramic plate evenly is dried to fully.
(3) deliver to the retort furnace high-temperature calcination, initial temperature is 50 ℃, and the calcining outlet temperature is 450 ℃, and heat-up rate is 1 ℃/min, and soaking time is 2h, and cooling rate is 1 ℃/min.Do not need inert protective gas in the calcination process.
(4) the cooling back is smooth with surface finish with 120#～360# sand paper.Remove ceramic plate surface dirt and residual powder with soft writing brush.
(5) configuration pH value is 4 sulphuric acid soln, ceramic membrane is immersed this solution take out after 12 hours, washes repeatedly through deionized water, soaks 12 hours with deionized water again, and dedusting environment dry 9 days is down made ceramic membrane.
Adopting membrane filtering method to handle COD is 250～450mol/L, and colourity is the dyeing waste water of 80～120PCU, and experimental temperature is a room temperature, water outlet COD＜150mol/L, colourity＜50PCU.
Embodiment 3
(1) attapulgite with 8.009g mixes with the 9ml deionized water, and at room temperature mechanical stirring mixes to pasty state, slowly pours mould compression moulding into, is prefabricated into diameter 2.9cm after the demoulding, and thickness is the round sheet pottery of 1.2cm.
(2) prefabricated ceramic plate ageing 5 days in the constant humidity environment was taken out under physical environment dry 3 days, and the interior free surface moisture of ceramic plate evenly is dried to fully.
(3) deliver to the retort furnace high-temperature calcination, initial temperature is 50 ℃, and the calcining outlet temperature is 250 ℃, and heat-up rate is 2.5 ℃/min, and soaking time is 2h, and cooling rate is 1 ℃/min.
(4) the cooling back is smooth with surface finish with 120#～360# sand paper.Remove ceramic plate surface dirt and residual powder with soft writing brush.
(5) configuration pH value is 4 sulphuric acid soln, ceramic membrane is immersed this solution take out after 12 hours, washes repeatedly through deionized water, soaks 12 hours with deionized water again, and dedusting environment dry 7 days is down made ceramic membrane.
Adopting membrane filtering method to handle COD is 250～450mol/L, and colourity is the dyeing waste water of 80～120PCU, and experimental temperature is a room temperature, water outlet COD＜120mol/L, colourity＜42PCU.
Embodiment 4
(1) attapulgite with 8.104g mixes with the 9ml deionized water, and at room temperature mechanical stirring mixes to pasty state, slowly pours mould compression moulding into, is prefabricated into diameter 2.9cm after the demoulding, and thickness is the round sheet pottery of 1.2cm.
(2) prefabricated ceramic plate ageing 6 days in the constant humidity environment was taken out under physical environment dry 4 days, and the interior free surface moisture of ceramic plate evenly is dried to fully.
(3) deliver to the retort furnace high-temperature calcination, initial temperature is 50 ℃, and the calcining outlet temperature is 550 ℃, and heat-up rate is 5 ℃/min, and soaking time is 2h, and cooling rate is 1 ℃/min.
(4) the cooling back is smooth with surface finish with 120#～360# sand paper.Remove ceramic plate surface dirt and residual powder with soft writing brush.
(5) configuration pH value is 4 sulphuric acid soln, ceramic membrane is immersed this solution take out after 12 hours, washes repeatedly through deionized water, soaks 12 hours with deionized water again, and dedusting environment dry 8 days is down made ceramic membrane.
Adopting membrane filtering method to handle COD is 250～450mol/L, and colourity is the dyeing waste water of 80～120PCU, and experimental temperature is a room temperature, water outlet COD＜125mol/L, colourity＜43PCU.
Claims (3)
1. a preparation method who has absorption and hold back the new ceramics film of dual-use function is characterized in that, may further comprise the steps:
A: 100～300 purpose attapulgites are mixed with deionized water, under mechanical stirring, mix, slowly pour forming mould compression moulding into, be prefabricated into the round sheet pottery of 1～2cm thickness after the demoulding to pasty state.
B: the ceramic plate that is prefabricated into ageing 3～7 days in the constant humidity environment earlier, taking-up under physical environment dry 2～5 days, drying temperature is 10～40 ℃, the interior free surface moisture of ceramic plate evenly is dried to fully, deliver to the retort furnace calcining, calcining temperature is 200～600 ℃, and heat-up rate is 0.5～6 ℃/min, soaking time is 0.5～6h, and cooling rate is 1～3 ℃/min.The cooling back is smooth with surface finish with sand paper, removes ceramic plate surface dirt and residual powder with soft writing brush.
C: the sulphuric acid soln of configuration pH value 2～6.Ceramic membrane is immersed taking-up after 8～24 hours in this solution, wash repeatedly through deionized water, soaked 8～24 hours with deionized water, dedusting environment dry 6～9 days is down made ceramic membrane.
2. according to the preparation method of claim 1, it is characterized in that: use attapulgite to be the feedstock production ceramic membrane with good adsorption properties.
3. according to the preparation method of claim 1, it is characterized in that: first ageing is dry again, and calcining is after the simple process of aftertreatment prepares ceramic membrane.
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| CN2010101861936A CN102260068A (en) | 2010-05-31 | 2010-05-31 | Preparation method of ceramic membrane with adsorption and retention functions |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614782A (en) * | 2012-04-12 | 2012-08-01 | 上海海事大学 | Ceramic filter film of rare-earth modified attapulgite with nano coating and preparation method thereof |
| CN104128100A (en) * | 2014-06-30 | 2014-11-05 | 淮阴师范学院 | Nano attapulgite based hollow fiber microfiltration membrane and preparation method thereof |
| CN104275096A (en) * | 2014-10-23 | 2015-01-14 | 兰州理工大学 | Preparation method of attapulgite porous membrane |
| CN108840703A (en) * | 2018-08-16 | 2018-11-20 | 北京工业大学 | A method of desalination hydrophobic porous cordierite ceramic film is prepared by raw material low cost of high silicon industrial solid castoff |
-
2010
- 2010-05-31 CN CN2010101861936A patent/CN102260068A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614782A (en) * | 2012-04-12 | 2012-08-01 | 上海海事大学 | Ceramic filter film of rare-earth modified attapulgite with nano coating and preparation method thereof |
| CN104128100A (en) * | 2014-06-30 | 2014-11-05 | 淮阴师范学院 | Nano attapulgite based hollow fiber microfiltration membrane and preparation method thereof |
| CN104128100B (en) * | 2014-06-30 | 2016-03-23 | 淮阴师范学院 | Nano-attapulgite ground mass hollow fiber microfiltration membrane and preparation method thereof |
| CN104275096A (en) * | 2014-10-23 | 2015-01-14 | 兰州理工大学 | Preparation method of attapulgite porous membrane |
| CN108840703A (en) * | 2018-08-16 | 2018-11-20 | 北京工业大学 | A method of desalination hydrophobic porous cordierite ceramic film is prepared by raw material low cost of high silicon industrial solid castoff |
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Application publication date: 20111130 |