CN114345137B - Ceramic microfiltration membrane with black talc as inorganic film-forming powder and preparation method thereof - Google Patents

Ceramic microfiltration membrane with black talc as inorganic film-forming powder and preparation method thereof Download PDF

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CN114345137B
CN114345137B CN202111666823.4A CN202111666823A CN114345137B CN 114345137 B CN114345137 B CN 114345137B CN 202111666823 A CN202111666823 A CN 202111666823A CN 114345137 B CN114345137 B CN 114345137B
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black talc
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CN114345137A (en
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张国亮
范子璇
孟琴
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Zhejiang University of Technology ZJUT
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Abstract

The invention belongs to the technical field of ceramic microfiltration membranes, and provides a ceramic microfiltration membrane with black talc as inorganic film-forming powder and a preparation method thereof. And (3) combining a solid particle sintering technology, introducing black talc powder into the coating solution to serve as inorganic film forming powder, and increasing sintering activation energy. Under the same sintering system, the connection depth between the film layer particles and the particles is larger, the film layer strength is increased, the abrasion resistance of the film layer is further increased, and the service life of the film layer is prolonged. According to the invention, the cheap black talc is used as a raw material for synthesis, so that the preparation cost of the ceramic membrane is reduced; the prepared ceramic ultrafiltration membrane has good acid-base resistance and a wide application prospect.

Description

Ceramic microfiltration membrane with black talc as inorganic film forming powder and preparation method thereof
Technical Field
The invention belongs to the technical field of ceramic microfiltration membrane preparation, and particularly relates to a low-cost ceramic microfiltration membrane with black talc as inorganic film-forming powder and a preparation method thereof.
Background
Membrane separation technology is a separation technology that arose in the 60's of the 20 th century and has developed rapidly over decades. The application field of the membrane separation technology is deep in various aspects of life and production of people, such as chemical industry, environmental protection, electronics, textiles, medicines, foods and the like. Since the industrialization of membrane separation technology, organic polymer membranes always dominate, but the common defects of most polymer membranes at present are that the thermal stability and chemical stability are poor, the degradation is easy, and the pH application range is narrow. Compared with an organic polymer membrane, the inorganic membrane has better thermal stability and acid and alkali resistance, wide applicability, long service life, simple and convenient operation, controllable pore diameter and little pollution, can meet the harsh conditions of high acid and alkali, high temperature and the like, is rapidly developed in recent years, and is widely applied to a plurality of fields of chemical engineering, environmental protection engineering and the like. Therefore, the development trend of the current membrane materials is mainly inorganic membrane materials.
Ceramic membranes, which are one type of inorganic membrane, are generally asymmetric structures consisting of a support layer, a transition layer, and a membrane layer. Wherein, the support layer provides necessary mechanical strength for the membrane layer, and the transition layer effectively prevents the membrane layer particles from being sucked into the support body to block the channel and increase the filtration resistance. According to the separation principle and the difference of the sizes of membrane pores, the ceramic membrane can be divided into microfiltration, ultrafiltration, nanofiltration, reverse osmosis and the like. Ceramic membranes tend to have high mechanical strength, are resistant to high pressure operation and wear, and can be backwashed with high strength. However, the high raw material cost for preparing the traditional ceramic membrane and the inevitable high-temperature sintering cost are serious defects of the development of the ceramic membrane, and moreover, the ceramic membrane of the traditional oxide materials cannot meet certain strict separation conditions in terms of performance. The black talc is a magnesium-rich silicate mineral clay, which has excellent chemical stability, large specific surface area, proper pore structure and surface structure, and the natural black talc has great reserves in China, simple development and utilization process and low production cost. Considering the bottleneck limitations of expensive raw materials for membrane preparation, few types of membrane materials, high sintering cost of membrane preparation and the like in the large-scale industrial separation application of ceramics, the cheap black talc mineral material is selected as the inorganic membrane forming powder, and the synthesized porous ceramics can have high porosity, high mechanical strength and a proper pore structure.
Disclosure of Invention
Aiming at the defect of high film-making sintering cost in the prior art, the invention provides an acid and alkali resistant black talc ceramic microfiltration membrane using inorganic film-forming powder and a preparation method thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
in a first aspect, the present invention provides a ceramic microfiltration membrane using black talc as an inorganic film-forming powder, wherein the ceramic microfiltration membrane using black talc as an inorganic film-forming powder is prepared by the following method:
(1) Uniformly dispersing 0.1-5 parts by mass (preferably 0.2 part by mass) of nano inorganic oxide particles and 0.01-0.1 part by mass (preferably 0.01 part by mass) of a dispersing agent in water A to obtain a nano inorganic oxide particle dispersion liquid; adding the nano inorganic oxide particle dispersion and 10-60 parts by mass (preferably 15 parts by mass) of black talc nano particles with the particle size of 100-400nm into water B, adjusting the pH to 3-6 (adding 1M nitric acid solution or 1M hydrochloric acid), stirring at 7000-8000rpm for 10-30min, adding 0.1-5 parts by mass (preferably 0.6 part by mass) of film forming agent and 0.05-0.2 part by mass of defoaming agent (preferably 0.1 part by mass), and stirring for 1-3h to obtain a coating liquid;
the nano inorganic oxide particles are one or a mixture of more than two of nano aluminum oxide, nano titanium oxide, nano zirconium oxide and nano silicon oxide (preferably nano aluminum oxide, nano titanium oxide or nano zirconium oxide, particularly preferably nano zirconium oxide); the dispersant is one or a mixture of more than two of polyacrylamide, sodium carboxymethylcellulose and sodium dodecyl benzene sulfonate (preferably polyacrylamide or sodium carboxymethylcellulose, and particularly preferably polyacrylamide); the film forming agent is polyvinyl alcohol, hydroxypropyl methylcellulose or ethyl cellulose (preferably polyvinyl alcohol or hydroxypropyl methylcellulose, and particularly preferably hydroxypropyl methylcellulose); the defoaming agent is one or a mixture of two of polydimethylsiloxane and polyether modified organic silicon defoaming agent (preferably polyether modified organic silicon defoaming agent);
(2) Coating the film coating liquid in the step (1) on a macroporous ceramic film support, drying for 5-24h (preferably 10-20 h) at room temperature, aging for 24-48h (preferably 28-45 h) at 60-90 ℃ for 24-48h (preferably 28-45 h) to ensure that the coating is stably adhered to the surface, heating to 700-1200 ℃ at the rate of 1-4 ℃/min (preferably 4 ℃/min) (nonuniform film sintering can be caused by excessively high heating speed), sintering for 2-5h (preferably 1000 ℃ for 3 h), and naturally cooling to obtain the ceramic microfiltration film with the black talc as the inorganic film forming powder.
Further, the volume of the water A in the step (1) is 3-10mL/g (preferably 5 mL/g) based on the mass of the nano inorganic oxide particles.
Further, the volume of the water B in the step (1) is 1.5-9.9mL/g (preferably 5.5 mL/g) based on the mass of the black talc nano particles.
The invention particularly recommends that the black talc is prepared as a ceramic microfiltration membrane of inorganic film-forming powder according to the following method:
(1) Uniformly dispersing 0.2 part by mass of nano inorganic oxide particles and 0.01 part by mass of a dispersing agent in water A to obtain nano inorganic oxide particle dispersion liquid; adding the nano inorganic oxide particle dispersion and 15 parts by mass of black talc nanoparticles with the particle size of 100-400nm into water B, adjusting the pH to 3-6 (adding 1M nitric acid solution or 1M hydrochloric acid), stirring at 7000-8000rpm for 10-30min, adding 0.6 part by mass of film-forming agent and 0.1 part by mass of defoaming agent, and stirring for 2h to obtain a coating solution;
the nano inorganic oxide particles are nano zirconia; the dispersing agent is hydroxypropyl methyl cellulose; the defoaming agent is a polyether modified organic silicon defoaming agent;
(2) Coating the film coating liquid in the step (1) on a macroporous ceramic film support, drying at room temperature for 12h, aging at 80 ℃ for 36h, heating to 1000 ℃ at the rate of 4 ℃/min, and sintering at the constant temperature for 3h to obtain the ceramic microfiltration membrane with the black talc as inorganic film forming powder.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, nanoparticles are introduced into the coating liquid as sintering active aids, so that the sintering activation energy is increased. The cheap black talc is used as inorganic film forming powder, so that the preparation cost of the ceramic film is greatly reduced; compared with the high-temperature sintering technology of solid particles in the existing ceramic membrane industrial production, the invention adopts the clay-based mineral material as the film-forming powder to effectively reduce the sintering temperature and the energy consumption, so that the produced product has higher cost performance. And (3) combining a solid particle sintering technology, introducing black talc powder into the coating solution to serve as inorganic film forming powder, and increasing sintering activation energy. Under the same sintering system, the connection depth between the film layer particles and the particles is larger, the film layer strength is increased, the abrasion resistance of the film layer is further increased, and the service life of the film layer is prolonged. According to the invention, the black talc with lower price is used as a raw material for synthesis, so that the preparation cost of the ceramic membrane is reduced; the prepared ceramic ultrafiltration membrane has good acid and alkali resistance and a wide application prospect.
Detailed Description
The invention is further described below by means of specific examples, without the scope of protection of the invention being limited thereto.
The black talc nanoparticles having a particle size of 300nm in the examples of the present invention were prepared as follows:
adding 15mL of absolute ethyl alcohol into 8g of black talc (the black talc is from Guangfeng region in Shanghai province in Jiangxi province), wet-grinding for 2h by using a ball mill 600r/min, washing and centrifuging, drying at 60 ℃, vigorously stirring the obtained black talc particles in 4L of deionized water at normal temperature for one week, fully stripping, centrifuging, and drying at 80 ℃ to obtain the black talc nano material (the average particle size is 300 nm).
Example 1
(1) Adding 20g of nano zirconia with the particle size of 50nm into 100mL of deionized water, adding 1g of polyacrylamide, and stirring at the rotating speed of 8000rpm for 30min to obtain nano zirconia dispersion liquid;
(2) Respectively weighing 15g of black talc nanoparticles with the particle size of 300nm and 1.2g of the nano zirconia dispersion, simultaneously adding 83.1mL of deionized water, adding 1mol/L of nitric acid to adjust the pH value to 4, stirring at a rotating speed of 8000rpm for 10min, then adding 0.6g of hydroxypropyl methyl cellulose and 0.1g of polyether modified organic silicon defoamer, and stirring for 2h to obtain a coating liquid;
(3) And (3) coating the film coating liquid on a macroporous ceramic film support (permanent-light chemical engineering, the diameter of the pore is 1 mu m and is 5 cm), drying at room temperature for 12h, drying at 80 ℃ for 36h, finally heating to 1000 ℃ at the speed of 4 ℃/min, preserving heat, sintering for 3h, and naturally cooling to obtain the low-cost black talc composite ceramic microfiltration membrane.
The pure water flux of the membrane tested by the cross-flow filtration device at a pressure of 0.5bar was 4500L m -2 ·h -1 Bar, measured by a three-point bending resistance test methodThe bending strength of the prepared film was 37.56MPa.
Example 2
(1) Adding 20g of nano-alumina with the particle size of 80nm into 100mL of deionized water, adding 1g of sodium dodecyl benzene sulfonate, and stirring at 8000rpm for 30min to obtain a nano-alumina dispersion liquid;
(2) Respectively weighing 15g of black talc nanoparticles with the particle size of 300nm and 3.6g of the nano alumina dispersion, simultaneously adding 80.7mL of deionized water, adding 1mol/L of nitric acid to adjust the pH value to 3.5, stirring at the rotating speed of 8000rpm for 10min, then adding 0.6g of polyvinyl alcohol and 0.1g of polyether modified organic silicon defoamer, and stirring for 2h to obtain a coating liquid;
(3) And (3) coating the coating liquid on a macroporous ceramic membrane support, drying at room temperature for 12 hours, then drying at 80 ℃ for 36 hours, finally heating to 900 ℃ at the speed of 4 ℃/min, preserving heat, sintering for 3 hours, and then naturally cooling to obtain the low-cost black talc composite ceramic microfiltration membrane.
The pure water flux of the membrane tested by the cross-flow filtration device under the pressure of 0.5bar is 5100L m -2 ·h -1 Bar, the bending strength of the prepared film is 35.52MPa by adopting a three-point bending resistance test method.
Example 3
(1) Adding 20g of nano titanium oxide with the particle size of 50nm into 100mL of deionized water, adding 1g of polyacrylamide, and stirring at 8000rpm for 45min to obtain nano titanium oxide dispersion;
(2) Respectively weighing 15g of black talc nanoparticles with the particle size of 300nm and 6g of the nano titanium oxide dispersion liquid, simultaneously adding 78.3mL of deionized water, adding 1mol/L hydrochloric acid to adjust the pH value to 3.5, stirring at the rotating speed of 8000rpm for 10min, then adding 0.6g of hydroxypropyl methyl cellulose and 0.1g of polyether modified organic silicon defoamer, and stirring for 2h to obtain a coating liquid;
(3) And (3) coating the coating liquid on a macroporous ceramic membrane support, drying at room temperature for 12 hours, then drying at 80 ℃ for 36 hours, finally heating to 900 ℃ at the speed of 4 ℃/min, preserving heat, sintering for 3 hours, and then naturally cooling to obtain the low-cost black talc composite ceramic microfiltration membrane.
Testing of the purity of the membranes at a pressure of 0.5bar using a crossflow filtration deviceThe water flux is 4820L m -2 ·h -1 Bar, the bending strength of the prepared film tested by the three-point bending resistance test method was 38.12MPa.
Comparative example 1
(1) Adding 20g of nano zirconia with the particle size of 50nm into 100mL of deionized water, adding 1g of polyacrylamide, and stirring at the rotating speed of 8000rpm for 30min to obtain nano zirconia dispersion liquid;
(2) Respectively weighing 15g of alumina nanoparticles (alatin, alumina 99.99%) with the particle size of 300nm and 1.2g of the nano zirconia dispersion, simultaneously adding 83.1mL of deionized water, adding 1mol/L of nitric acid to adjust the pH to 4, stirring at the rotating speed of 8000rpm for 10min, then adding 0.6g of hydroxypropyl methyl cellulose and 0.1g of polyether modified organic silicon defoamer, and stirring for 2h to obtain a coating liquid;
(3) And (3) coating the coating liquid on a macroporous ceramic membrane support, drying at room temperature for 12h, drying at 80 ℃ for 36h, heating to 1300 ℃ at the speed of 4 ℃/min, preserving heat, sintering for 3h, and naturally cooling to obtain the alumina composite ceramic microfiltration membrane.
The pure water flux of the membrane tested with a cross-flow filtration unit at a pressure of 0.5bar was 4100L m -2 ·h -1 Bar, bending strength of 34.10MPa for the membrane prepared by the three-point bending resistance test method, in particular, 1300 ℃ sintering is required for the alumina composite ceramic microfiltration membrane to be higher than 1000 ℃ in example 1, and sintering energy consumption is reduced.
Comparative example 2
(1) Adding 20g of nano zirconia with the particle size of 50nm into 79mL of deionized water, adding 1g of polyacrylamide, and stirring at 8000rpm for 30min to obtain nano zirconia dispersion;
(2) Respectively weighing 15g of silicon oxide (alatin, silicon dioxide) nanoparticles with the particle size of 300nm and 1.2g of the nano-zirconia dispersion liquid, simultaneously adding 83.1mL of deionized water, adding 1mol/L of nitric acid to adjust the pH to 4, stirring at the rotating speed of 8000rpm for 10min, then adding 0.6g of hydroxypropyl methyl cellulose and 0.1g of polyether modified organic silicon defoamer, and stirring for 2h to obtain a coating liquid;
(3) And (3) coating the coating liquid on a macroporous ceramic membrane support, drying at room temperature for 12 hours, then drying at 80 ℃ for 36 hours, finally heating to 1200 ℃ at a speed of 4 ℃/min, preserving heat, sintering for 3 hours, and then naturally cooling to obtain the silicon oxide composite ceramic microfiltration membrane.
The pure water flux of the membrane tested with a cross-flow filtration unit at a pressure of 0.5bar was 4200L m -2 ·h -1 Bar, the bending strength of the membrane prepared by the three-point bending resistance test method is 33.16MPa, and particularly, the sintering temperature of the alumina composite ceramic microfiltration membrane is 1200 ℃ higher than 1000 ℃ in the embodiment 1, so that the sintering energy consumption is reduced.
Comparative example 3
(1) Adding 20g of nano zirconia with the particle size of 50nm into 79mL of deionized water, adding 1g of polyacrylamide, and stirring at the rotating speed of 8000rpm for 30min to obtain nano zirconia dispersion liquid;
(2) Respectively weighing 15g of talc nanoparticles (K-brand talcum powder) with the particle size of 300nm and 1.2g of the nano zirconia dispersion, simultaneously adding 83.1mL of deionized water, adding 1mol/L of nitric acid to adjust the pH value to 4, stirring at the rotating speed of 8000rpm for 10min, then adding 0.6g of hydroxypropyl methyl cellulose and 0.1g of polyether modified organic silicon defoamer, and stirring for 2h to obtain a coating liquid;
(3) And (3) coating the coating liquid on a macroporous ceramic membrane support, drying at room temperature for 12h, drying at 80 ℃ for 36h, heating to 1000 ℃ at the speed of 4 ℃/min, preserving heat, sintering for 3h, and naturally cooling to obtain the talc composite ceramic microfiltration membrane.
The pure water flux of the membrane tested by adopting a cross-flow filtering device under the pressure of 0.5bar is 3900L m -2 ·h -1 Bar, flexural strength of 35.12MPa of the membrane prepared as tested by the three-point bending resistance test method, in particular talc composite ceramic microfiltration membranes having a lower pure water flux due to the absence of the graphitic carbon-like layer between the layers.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the scope of the invention, i.e. the equivalent variations and modifications made by the patent scope and the specification of the present invention should be covered by the present invention.

Claims (10)

1. The ceramic microfiltration membrane using the black talc as the inorganic film-forming powder is characterized in that the ceramic microfiltration membrane using the black talc as the inorganic film-forming powder is prepared by the following method:
(1) Uniformly dispersing 0.1-5 parts by mass of nano inorganic oxide particles and 0.01-0.1 part by mass of a dispersing agent in water A to obtain nano inorganic oxide particle dispersion liquid; adding the nano inorganic oxide particle dispersion and 10-60 parts by mass of black talc nanoparticles with the particle size of 100-400nm into water B, adjusting the pH to 3-6, stirring at 7000-8000rpm for 10-30min, adding 0.1-5 parts by mass of a film-forming agent and 0.05-0.2 part by mass of an antifoaming agent, and stirring for 1-3h to obtain a coating liquid;
the nano inorganic oxide particles are one or a mixture of more than two of nano aluminum oxide, nano titanium oxide, nano zirconium oxide and nano silicon oxide; the dispersing agent is one or a mixture of more than two of polyacrylamide, sodium carboxymethylcellulose and sodium dodecyl benzene sulfonate; the film forming agent is polyvinyl alcohol, hydroxypropyl methyl cellulose or ethyl cellulose; the defoaming agent is one or a mixture of two of polydimethylsiloxane and polyether modified organic silicon defoaming agent; the volume of the water A is 3-10mL/g based on the mass of the nano inorganic oxide particles; the volume of the water B is 1.5-9.9mL/g based on the mass of the black talc nano particles;
(2) Coating the film coating liquid in the step (1) on a macroporous ceramic film support, drying at room temperature for 5-24h, aging at 60-90 ℃ for 24-48h, heating to 700-1200 ℃ at the speed of 1-4 ℃/min, and sintering at the temperature for 2-5h to obtain the ceramic microfiltration membrane with the black talc as inorganic film forming powder.
2. The ceramic microfiltration membrane containing black talc as an inorganic film-forming powder according to claim 1 wherein: the volume of the water A in the step (1) is 5mL/g based on the mass of the nano inorganic oxide particles.
3. The ceramic microfiltration membrane containing black talc as an inorganic film-forming powder according to claim 1 wherein: the volume of the water B in the step (1) is 5.5mL/g based on the mass of the black talc nano particles.
4. The ceramic microfiltration membrane using black talc as an inorganic film-forming powder according to claim 1, wherein: in the step (1), the nano inorganic oxide particles are nano aluminum oxide, nano titanium oxide or nano zirconium oxide.
5. The ceramic microfiltration membrane containing black talc as an inorganic film-forming powder according to claim 4 wherein: in the step (1), the nano inorganic oxide particles are nano zirconia.
6. The ceramic microfiltration membrane containing black talc as an inorganic film-forming powder according to claim 1 wherein: in the step (1), the dispersant is polyacrylamide or sodium carboxymethylcellulose.
7. The ceramic microfiltration membrane containing black talc as an inorganic film-forming powder according to claim 1 wherein: in the step (1), the film forming agent is polyvinyl alcohol or hydroxypropyl methyl cellulose.
8. The ceramic microfiltration membrane containing black talc as an inorganic film-forming powder according to claim 1 wherein: the defoaming agent in the step (1) is a polyether modified organic silicon defoaming agent.
9. The ceramic microfiltration membrane containing black talc as an inorganic film-forming powder according to claim 1 wherein: the temperature of the aging in the step (2) was 80 ℃.
10. The ceramic microfiltration membrane using black talc as an inorganic membrane-forming powder according to claim 1, wherein the ceramic microfiltration membrane using black talc as an inorganic membrane-forming powder is prepared by the following method:
(1) Uniformly dispersing 0.2 part by mass of nano inorganic oxide particles and 0.01 part by mass of a dispersing agent in water A to obtain nano inorganic oxide particle dispersion liquid; adding the nano inorganic oxide particle dispersion and 15 parts by mass of black talc nanoparticles with the particle size of 100-400nm into water B, adjusting the pH to 3-6, stirring at 7000-8000rpm for 10-30min, adding 0.6 part by mass of a film-forming agent and 0.1 part by mass of an antifoaming agent, and stirring for 2h to obtain a coating liquid;
the nano inorganic oxide particles are nano zirconia; the dispersing agent is hydroxypropyl methyl cellulose; the defoaming agent is a polyether modified organic silicon defoaming agent;
(2) Coating the film coating liquid in the step (1) on a macroporous ceramic film support, drying at room temperature for 12h, aging at 80 ℃ for 36h, heating to 1000 ℃ at the speed of 4 ℃/min, and sintering at the constant temperature for 3h to obtain the ceramic microfiltration membrane with the black talc as inorganic film forming powder.
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