CN114105671A - Coal gangue-quartz-based ceramic support and preparation method thereof - Google Patents
Coal gangue-quartz-based ceramic support and preparation method thereof Download PDFInfo
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0022—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof obtained by a chemical conversion or reaction other than those relating to the setting or hardening of cement-like material or to the formation of a sol or a gel, e.g. by carbonising or pyrolysing preformed cellular materials based on polymers, organo-metallic or organo-silicon precursors
- C04B38/0025—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof obtained by a chemical conversion or reaction other than those relating to the setting or hardening of cement-like material or to the formation of a sol or a gel, e.g. by carbonising or pyrolysing preformed cellular materials based on polymers, organo-metallic or organo-silicon precursors starting from inorganic materials only, e.g. metal foam; Lanxide type products
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- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
- C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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Abstract
The invention provides a coal gangue-quartz-based ceramic support and a preparation method thereof, belonging to the technical field of ceramic membranes. The invention takes quartz sand and solid waste coal gangue as main raw materials, and can prepare the high-performance ceramic support body at a lower sintering temperature. The invention not only improves the utilization rate of solid waste coal gangue, but also reduces the preparation cost of the inorganic ceramic membrane, and the prepared ceramic membrane has relevant performance capable of meeting the requirement of water treatment and has good economic, social and ecological benefits.
Description
Technical Field
The invention relates to the technical field of ceramic membranes, in particular to a coal gangue-quartz-based ceramic support body and a preparation method thereof.
Background
With the continuous deepening of the national ecological civilization construction concept and the continuous enhancement of environmental protection consciousness, in order to adapt to the more strict water quality discharge standard of the country, the membrane separation technology has become an important alternative method of the traditional water treatment process. Compared with the traditional organic membrane, the inorganic ceramic membrane has the advantages of high temperature resistance, chemical corrosion resistance, high mechanical strength, strong oxidation resistance, convenience in cleaning and regeneration, no toxicity, long service life and the like, and is widely applied to various fields of chemical industry, food, medicine, biology and the like.
The ceramic membrane consists of a support body and a membrane layer. At present, Al is mostly used for preparing commercial ceramic supports2O3、TiO2The raw materials are high in price, and the sintering temperature in the preparation process is as high as 1400 ℃, so that the production cost of the ceramic membrane is high, and the industrial application of the ceramic membrane is restricted.
Disclosure of Invention
The invention aims to provide a coal gangue-quartz-based ceramic support body and a preparation method thereof, and the preparation method does not need to adopt high-cost Al2O3、TiO2Raw materials and low sintering temperature.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a coal gangue-quartz-based ceramic support body, which comprises the following steps:
mixing quartz sand, coal gangue, potassium feldspar, sodium carbonate, sodium carboxymethylcellulose and sodium tetraborate to obtain a mixed dry material;
mixing the mixed dry material with a mixed solution containing a plasticizer, a lubricant, ethanol and water to obtain pug;
carrying out vacuum pugging on the pug, and then forming to obtain a support body blank;
drying and sintering the support body blank in sequence to obtain a coal gangue-quartz-based ceramic support body; the sintering comprises the steps of sequentially carrying out first sintering and second sintering, wherein the temperature of the first sintering is 300 ℃, and the temperature of the second sintering is 850 ℃.
Preferably, the quartz sand and the coal gangue are subjected to ball milling treatment; the particle size of the quartz sand and the coal gangue is less than 120 meshes.
Preferably, the mass of the quartz sand is 40-60% of that of the dry mixed material; the mass of the coal gangue accounts for 20-40% of the mass of the mixed dry material; the mass of the potassium feldspar is 4-8% of that of the mixed dry material; the mass of the sodium carbonate is 2-5% of that of the mixed dry material; the mass of the sodium carboxymethyl cellulose is 5-10% of that of the mixed dry material; the mass of the sodium tetraborate is 1-3% of the mass of the mixed dry material.
Preferably, the plasticizer comprises dioctyl phthalate; the lubricant comprises glycerol.
Preferably, the mass content of the plasticizer, the lubricant and the ethanol in the mixed solution is 1-3%, 1-3% and 3-5%.
Preferably, the mass ratio of the dry mixture to the mixed solution is 5: (1-2).
Preferably, the pug obtained by vacuum pugging is aged for 16-24 hours before forming.
Preferably, the drying comprises: standing at room temperature for 10-16 h, then raising the temperature from room temperature to 70 ℃ and preserving heat for 4-6 h, and then raising the temperature from 70 ℃ to 120 ℃ and preserving heat for 4-6 h.
Preferably, the heat preservation time of the first sintering is 30 min; and the heat preservation time of the second sintering is 30 min.
The invention provides the coal gangue-quartz-based ceramic support prepared by the preparation method in the scheme.
The invention provides a preparation method of a coal gangue-quartz-based ceramic support body, which comprises the following steps: mixing quartz sand, coal gangue, potassium feldspar, sodium carbonate, sodium carboxymethylcellulose and sodium tetraborate to obtain a mixed dry material; mixing the mixed dry material with a mixed solution containing a plasticizer, a lubricant, ethanol and water to obtain pug; carrying out vacuum pugging on the pug, and then forming to obtain a support body blank; drying and sintering the support body blank in sequence to obtain a coal gangue-quartz-based ceramic support body; the sintering comprises the steps of sequentially carrying out first sintering and second sintering, wherein the temperature of the first sintering is 300 ℃, and the temperature of the second sintering is 850 ℃.
The coal gangue is one of the industrial solid wastes with the largest annual discharge amount and accumulated stacking amount in China at present, the mineral components of the coal gangue are mainly clay minerals and quartz, and the coal gangue is rich in SiO2And Al2O3Can be used as a raw material for preparing the ceramic support body. The invention takes quartz sand and solid waste coal gangue as main raw materials, and can prepare the high-performance ceramic support body at a lower sintering temperature. The invention not only improves the utilization rate of solid waste coal gangue, but also reduces the preparation cost of the inorganic ceramic membrane, and the prepared ceramic membrane has relevant performance capable of meeting the requirement of water treatment and has good economic, social and ecological benefits.
Detailed Description
The invention provides a preparation method of a coal gangue-quartz-based ceramic support body, which comprises the following steps:
mixing quartz sand, coal gangue, potassium feldspar, sodium carbonate, sodium carboxymethylcellulose and sodium tetraborate to obtain a mixed dry material;
mixing the mixed dry material with a mixed solution containing a plasticizer, a lubricant, ethanol and water to obtain pug;
carrying out vacuum pugging on the pug, and then forming to obtain a support body blank;
drying and sintering the support body blank in sequence to obtain a coal gangue-quartz-based ceramic support body; the sintering comprises the steps of sequentially carrying out first sintering and second sintering, wherein the temperature of the first sintering is 300 ℃, and the temperature of the second sintering is 850 ℃.
In the present invention, the starting materials used are all commercially available products well known in the art, unless otherwise specified.
The invention mixes quartz sand, coal gangue, potassium feldspar, sodium carbonate, sodium carboxymethylcellulose and sodium tetraborate to obtain a dry mixed material.
In the invention, the quartz sand and the coal gangue are preferably subjected to ball milling treatment. In the invention, the time for ball milling treatment of the quartz sand and the coal gangue is preferably 24-36 h independently. The invention utilizes ball milling treatment to grind off sharp edges and corners of the quartz sand and the coal gangue, spheroidizes the quartz sand and the coal gangue, and prevents the molding of materials and the pore size distribution after sintering from being influenced by anisotropy in the subsequent molding and sintering processes. In the present invention, the particle size of the quartz sand and the coal gangue is preferably less than 120 mesh. According to the invention, the quartz sand and the coal gangue are preferably respectively subjected to ball milling treatment and then sieved by a 120-mesh sieve.
In the invention, the mass of the quartz sand is preferably 40-60% of that of the dry mixed material, and more preferably 45-55%; the mass of the coal gangue is preferably 20-40% of that of the mixed dry material, and more preferably 25-35%; the mass of the potassium feldspar is preferably 4-8% of that of the mixed dry material, and more preferably 5-7%; the mass of the sodium carbonate is preferably 2-5% of that of the dry mixed material, and more preferably 3-4%; the mass of the sodium carboxymethyl cellulose is preferably 5-10% of that of the dry mixed material, and more preferably 6-8%; the mass of the sodium tetraborate is preferably 1-3% of the mass of the dry mixed material, and more preferably 1.5-2.5%.
In the invention, the quartz sand and the coal gangue are used as main raw materials of the ceramic support body; the potash feldspar has the functions of a sintering aid and a binder, and can improve the shaping of a green body; the sodium carbonate is a pore-forming agent, and the silicon dioxide and the sodium carbonate contained in the coal gangue react at high temperature to generate silicate and carbon dioxide, so that a uniform and compact pore structure is easy to form by a blank; sodium carboxymethylcellulose is used as a binder; the sodium tetraborate is vitrified at high temperature and can be melted with metal ions, so that the compressive strength of the ceramic membrane can be improved.
In the invention, the quartz sand, the coal gangue, the potassium feldspar, the sodium carbonate, the sodium carboxymethyl cellulose and the sodium tetraborate are preferably mixed under the condition of stirring, and the stirring time is preferably 15-30 min. The present invention does not require any particular speed of agitation, and can employ agitation speeds well known in the art.
After the mixed dry material is obtained, the mixed dry material is mixed with mixed liquid containing plasticizer, lubricant, ethanol and water to obtain pug.
In the present invention, the plasticizer preferably includes dioctyl phthalate; the lubricant preferably comprises glycerol; the water is preferably deionized water; the ethanol is preferably anhydrous ethanol. In the present invention, the mass content of the plasticizer, the lubricant and the ethanol in the mixed solution is preferably 1 to 3%, 1 to 3% and 3 to 5%, respectively. In the present invention, the plasticizer functions to reduce the effect of van der waals force between support molecules, increase the mobility of molecular chains, and expand the processing temperature range of the support, so that the support has higher strength; the lubricant glycerol is very easy to dissolve in water, has a small molecular structure and low surface tension, and can be quickly mixed with a ceramic membrane raw material to play a role in wetting; the ethanol has the functions of preventing excessive condensation of the raw materials in the process of stirring the materials, promoting sintering and improving density. The preparation method of the mixed solution has no special requirements, and all the substances are directly and uniformly mixed.
In the present invention, the mass ratio of the dry mixture to the mixed solution is preferably 5: (1-2), more preferably 5: 1.5. In the invention, the mixing of the dry mixed material and the mixed liquid is preferably carried out in a mixer, and the mixing time of the dry mixed material and the mixed liquid is preferably 20-40 min.
According to the invention, the use amount of the binder, the plasticizer and the lubricant is controlled, so that the plasticity and the viscosity of the pug are proper, the subsequent shaping and blank making can be better ensured, and the support body blank is prevented from chapping or collapsing.
After pug is obtained, the pug is subjected to vacuum pugging and then is molded to obtain a support body blank.
In the invention, the frequency of the vacuum pugging is preferably 4-7 times. The invention has no special requirements on the vacuum pugging process, and the vacuum pugging process well known in the field can be adopted. The invention utilizes the vacuum pugging to more thoroughly discharge the air in the pug, so that the pug is more uniform, the density and the plasticity are better, the forming is convenient, and the drying strength and the mechanical strength of the blank body are also improved.
After the vacuum pugging is completed, the invention preferably also comprises aging the obtained pug. In the invention, the aging time is preferably 16-24 h. In the invention, the aging has the function of enabling the moisture in the pug to tend to be homogenized and driving substances such as a binder, a pore-forming agent and the like in the pug to be homogenized.
The present invention does not require any particular shaping means, and any shaping means known in the art may be used. In the present invention, the shape of the support body blank is preferably a tubular shape, more preferably a single-hole tube or a multi-hole tube.
After the support body green body is obtained, the support body green body is sequentially dried and sintered to obtain the coal gangue-quartz-based ceramic support body.
In the present invention, the drying preferably includes: standing at room temperature for 10-16 h, then raising the temperature from room temperature to 70 ℃ and preserving heat for 4-6 h, and then raising the temperature from 70 ℃ to 120 ℃ and preserving heat for 4-6 h. The invention is placed at room temperature for 10-16 h for shaping, so that a wet blank has a free shrinkage process, the adaptability of the blank in atmospheric moisture is observed, and if no cracking phenomenon occurs, the blank can be directly placed into an oven for drying; the sectional drying mode is adopted to prevent the deformation or cracking of the green body caused by the uneven distribution of water in the green body due to the overhigh initial temperature setting or the overhigh speed.
In the present invention, the sintering includes sequentially performing a first sintering and a second sintering; the temperature of the first sintering is 300 ℃, and the heat preservation time is preferably 30 min; the temperature of the second sintering is preferably 850 ℃, and the holding time is preferably 30 min. In the invention, the physical bound water in the blank body is removed in the first sintering process, and in the second sintering process, the silicon dioxide in the coal gangue reacts with sodium carbonate to generate carbon dioxide gas; the organic additive is volatilized. The invention adopts the sectional sintering to prevent the molecules in the support body from linear shrinkage too fast and cracking, which is beneficial to the complete crystal form of the support body; by controlling the sintering temperature within the range, the invention can prevent the collapse and secondary crystallization of the ceramic support body caused by overhigh sintering temperature from influencing the performance, and can also prevent the ceramic support body from having no densification reaction caused by overlow sintering temperature, changing the shape and size of the air hole and influencing the performance of the sample.
In the invention, the heating rate of heating from room temperature to the first sintering temperature is preferably 1-3 ℃/min; the heating rate from the first sintering temperature to the second sintering temperature is preferably 2-5 ℃/min. By controlling the heating rate, the invention can prevent the incomplete volatilization of the additive caused by the over-high heating rate and the influence on the mechanical strength of the sample, and can also prevent the influence on the densification reaction of the blank body caused by the over-low heating rate.
The invention obtains the ceramic support body with enough strength and higher porosity by sintering.
After the sintering is completed, the ceramic support body is preferably obtained by naturally cooling to room temperature.
The invention provides the coal gangue-quartz-based ceramic support prepared by the preparation method in the scheme. The coal gangue-quartz-based ceramic support prepared by the method has good mechanical property, the breaking strength is 8.0-9.01 MPa, the porosity is 39-42.1%, and the pure water flux is 80-100.7 m3·m-2·h-1·bar-1。
The coal gangue-quartz-based ceramic support and the preparation method thereof provided by the present invention will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) Putting the raw materials of quartz sand and coal gangue into a ball mill respectively, ball-milling for 36h, and then sieving with a 120-mesh sieve to ensure that the particles are uniform;
(2) adding potassium feldspar, sodium carbonate, sodium carboxymethylcellulose and sodium tetraborate powder into the quartz sand and coal gangue obtained in the step (1), mixing and stirring for 20min, and uniformly mixing the whole material powder to obtain a mixed dry material; the mixed dry material comprises the following components in percentage by mass: 53.5% of quartz sand, 30% of coal gangue, 5% of potassium feldspar, 5% of sodium carboxymethylcellulose, 4% of sodium carbonate and 2.5% of sodium tetraborate;
(3) adding a mixed solution of dioctyl phthalate (plasticizer), glycerol (lubricant), absolute ethyl alcohol and deionized water into the mixed dry material obtained in the step (2), and fully stirring in a mixer for 30min to obtain pug; the mixed solution comprises 2% of dioctyl phthalate, 2% of glycerol, 4% of absolute ethyl alcohol and the balance of deionized water in percentage by mass; the mass ratio of the mixed dry materials to the mixed liquid is 5: 1.5;
(4) putting the pug obtained in the step (3) into a vacuum pug mill, repeatedly vacuumizing and pugging for 5 times, and then aging the obtained pug for 24 hours;
(5) pouring the pug obtained in the step (4) into a forming machine, and forming to obtain a porous ceramic membrane tube support body blank;
(6) placing the porous ceramic membrane tube support body blank obtained in the step (5) at room temperature for 12-16 h, firstly drying at 70 ℃ for 5h, then drying at 120 ℃ for 5h, and finally placing in a muffle furnace for sintering, wherein the sintering process is segmented sintering, and the first stage is as follows: the temperature is between room temperature and 300 ℃, the heating rate is 2.5 ℃/min, the heating time is 200min, and then the temperature is kept at 300 ℃ for 30 min; and in the second stage, heating to 850 ℃ at 300 ℃, wherein the heating rate is 5 ℃/min, the heating time is 70min, keeping the temperature at 850 ℃ for 30min, and finally naturally cooling to room temperature to obtain the quartz porous ceramic membrane support.
The porous ceramic membrane support prepared in example 1 is a single-hole tube (the diameter of a tube opening is 3cm, the wall thickness is 0.5cm), the breaking strength of the prepared single-tube coal gangue-quartz-based ceramic support reaches 9.01MPa, the porosity is 40%, and the pure water flux is 100.7m3·m-2·h-1·bar-1。
Example 2
The difference from example 1 is that the mixed dry material comprises: 63.5% of quartz sand, 20% of coal gangue, 5% of potassium feldspar, 5% of sodium carboxymethyl cellulose, 4% of sodium carbonate and 2.5% of sodium tetraborate.
The breaking strength of the prepared single-tube coal gangue-quartz-based ceramic support body is 8.27MPa, the porosity is 39.2 percent, and the pure water flux is 97.5m3·m-2·h-1·bar-1。
Example 3
The difference from example 1 is that the mixed dry material comprises: 43.5% of quartz sand, 40% of coal gangue, 5% of potassium feldspar, 5% of sodium carboxymethyl cellulose, 4% of sodium carbonate and 2.5% of sodium tetraborate.
The breaking strength of the prepared single-tube coal gangue-quartz-based ceramic support body is 8.33MPa, the porosity is 42.1 percent, and the pure water flux is 80m3·m-2·h-1·bar-1。
Comparative example 1
The difference from example 1 is that the mixed dry material comprises: 33.5% of quartz sand, 50% of coal gangue, 5% of potassium feldspar, 5% of sodium carboxymethyl cellulose, 4% of sodium carbonate and 2.5% of sodium tetraborate.
The breaking strength of the prepared single-tube coal gangue-quartz-based ceramic support body is 7.94MPa, the porosity is 42.4 percent, and the pure water flux is 74.4m3·m-2·h-1·bar-1。
From the results of example 1 and comparative example 1, it is understood that the support strength is reduced and the pure water flux is reduced when the content of gangue in the mixed dry material is increased to a certain extent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a coal gangue-quartz-based ceramic support body comprises the following steps:
mixing quartz sand, coal gangue, potassium feldspar, sodium carbonate, sodium carboxymethylcellulose and sodium tetraborate to obtain a mixed dry material;
mixing the mixed dry material with a mixed solution containing a plasticizer, a lubricant, ethanol and water to obtain pug;
carrying out vacuum pugging on the pug, and then forming to obtain a support body blank;
drying and sintering the support body blank in sequence to obtain a coal gangue-quartz-based ceramic support body; the sintering comprises the steps of sequentially carrying out first sintering and second sintering, wherein the temperature of the first sintering is 300 ℃, and the temperature of the second sintering is 850 ℃.
2. The preparation method according to claim 1, wherein the quartz sand and the coal gangue are ball-milled quartz sand and coal gangue; the particle size of the quartz sand and the coal gangue is less than 120 meshes.
3. The preparation method according to claim 1, wherein the mass of the quartz sand is 40-60% of the mass of the dry mixed material; the mass of the coal gangue accounts for 20-40% of the mass of the mixed dry material; the mass of the potassium feldspar is 4-8% of that of the mixed dry material; the mass of the sodium carbonate is 2-5% of that of the mixed dry material; the mass of the sodium carboxymethyl cellulose is 5-10% of that of the mixed dry material; the mass of the sodium tetraborate is 1-3% of the mass of the mixed dry material.
4. The method of claim 1, wherein the plasticizer comprises dioctyl phthalate; the lubricant comprises glycerol.
5. The method according to claim 1, wherein the mixed solution contains 1 to 3% by mass of the plasticizer, 1 to 3% by mass of the lubricant, and 3 to 5% by mass of the ethanol.
6. The preparation method according to claim 1, wherein the mass ratio of the dry mixed material to the mixed liquid is 5: (1-2).
7. The preparation method according to claim 1, characterized by aging the pug obtained by vacuum pugging for 16-24 hours before forming.
8. The method of manufacturing according to claim 1, wherein the drying includes: standing at room temperature for 10-16 h, then raising the temperature from room temperature to 70 ℃ and preserving heat for 4-6 h, and then raising the temperature from 70 ℃ to 120 ℃ and preserving heat for 4-6 h.
9. The production method according to claim 1, wherein the holding time for the first sintering is 30 min; and the heat preservation time of the second sintering is 30 min.
10. The coal gangue-quartz-based ceramic support prepared by the preparation method of any one of claims 1 to 9.
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