CN112221462A - Preparation method and application of porous spherical particles - Google Patents
Preparation method and application of porous spherical particles Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/165—Natural alumino-silicates, e.g. zeolites
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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Abstract
The invention discloses a preparation method and application of porous spherical particles, belonging to the technical field of inorganic materials, and the specific preparation method comprises the following steps: (1) preparing a base material: preparing powder from various raw materials of cristobalite, phosphorosilicate, melilite, spinel, magrose pyroxene, anorthite, pyroxene and mullite to obtain a base material with the particle size of 300-800 meshes; (2) preparing porous spherical particles: and uniformly mixing the base materials, adding an adhesive into the base materials at normal temperature, kneading for 20-30 min at 30-50 ℃, drying, roasting and screening to obtain the porous spherical particles. The porous spherical particles are applied to wastewater treatment, and can filter macromolecular organic matters and fine impurities in wastewater so as to purify the wastewater. In addition, the product provided by the invention has lower manufacturing cost and use cost, and is suitable for industrial popularization and use.
Description
Technical Field
The invention relates to the technical field of inorganic materials, in particular to a preparation method and application of porous spherical particles.
Background
In the 60's of the 20 th century, it was discovered that environmental water bodies were polluted by discharged wastewater, which not only caused changes in aquatic organism population and community structure, but also, in severe cases, resulted in destruction and collapse of aquatic ecosystems. At present, the influence of industrial wastewater in China on an aquatic ecosystem is increasingly serious, and meanwhile, the pollution of environmental water also threatens the health of human bodies. Conclusions about the toxic effects of water pollution on aquatic organisms can be applied to other higher animals, from which consequences and threats of pollution on human health can be predicted and presumed.
For example, wastewater from the coking industry contains a lot of phenolic substances, and wastewater from pharmaceutical factories contains not only phenolic-containing organic substances but also more complex other organic substances, including substances that are difficult to degrade by microorganisms and even have inhibitory effects on microorganisms; organic or inorganic substance residues which need to be added in the fermentation or extraction process due to production, residual solvent, residual antibiotics and degradation products thereof and the like discharged in the production process. The pharmaceutical wastewater is characterized by high content of organic pollutants, large pH change, high content of suspended matters, large alkalinity, large chromaticity and large water quality change. In addition, the industrial wastewater in the carbon industry mainly comes from equipment circulating cooling water pollution discharge, flue gas purification wastewater, product cooling water, flushing water in operation places and the like in the carbon production process. The industrial wastewater pollutants are influenced by industrial production raw materials, mainly fluoride, petroleum, chromaticity and suspended matters, and secondly COD and dissolved solids. Wherein the suspended matters contain part of fine dust besides conventional silt and colloidal substances; the oil stain mainly contains heavy tar, light floating oil and a small amount of emulsified oil
In the prior art, phenolic substances in wastewater are mostly removed by a resin adsorption method; for more antibiotics and other substances in pharmaceutical factories, an anaerobic-aerobic intermittent activated sludge process is mostly adopted to treat penicillin wastewater; in addition, for the waste water with more suspended matters, a flocculating agent is added to precipitate the suspended matters, and then the waste water is purified after filtration and separation. However, the above treatment methods are all high in cost, and the wastewater treatment material cannot be recycled, which is not beneficial to industrial popularization.
In addition, the materials for filtering the waste water containing fine impurities in the prior art can be classified into plastic products, iron products and ceramic products. The plastic product for filtering has small mechanical strength in the using process, particularly the film to the product is easy to damage and not easy to clean so as to recycle the product, and the plastic product is not easy to decompose and easily causes white pollution. Secondly, the iron products for filtering are easy to rust and form secondary pollution after being placed in the wastewater for a long time, and the manufacturing cost of the iron products is higher. And thirdly, the ceramic product for filtering has complex manufacturing steps and higher cost.
Therefore, how to provide a waste water filtering material which is low in cost and can be reused after simple treatment is a problem to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a preparation method and application of porous spherical particles, which are low in cost, simple in preparation method and capable of being recycled.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of porous spherical particles specifically comprises the following steps:
(1) preparing a base material: one or more raw materials of cristobalite, phosphorosilicate, melilite, spinel, magrose pyroxene, anorthite, pyroxene and mullite are pulverized to obtain a base material with the particle size of 300-800 meshes;
(2) preparing porous spherical particles for filtering wastewater: uniformly mixing the base materials, adding an adhesive into the base materials at normal temperature, kneading in a kneading pot, adding a proper amount of water into the kneading pot to ensure the kneading effect, kneading at 30-50 ℃ for 20-30 min to form spherical particles, and drying, roasting and screening the obtained spherical particles to obtain the porous spherical particles.
Has the advantages that: the product can form a spherical structure, and is mainly prepared by kneading three raw materials, namely a base material, an adhesive and water in a kneading pot by a kneading technology to form spherical particles. And the spherical particles form a porous structure after being roasted, so that the product has good adsorbability due to the porous structure, and impurities such as fine impurities and organic matters in the wastewater can be adsorbed, and clean wastewater is obtained.
In addition, the cristobalite and the phosphorosilicate are main sources of silicon dioxide in the spherical particles, so that the strength and the hardness of the spherical particles are ensured, and the stability of the spherical particles is ensured by spinel, anorthite, pyroxene and melilite.
Preferably, in the step (1), the mass fraction of the cristobalite in the raw materials is 20-40%, the mass fraction content of the phosphorosilicate is 10-20%, and the total mass fraction of other raw materials is 30-40%;
the powder preparation method comprises one or two of crushing, dry grinding and wet grinding.
Preferably, the matrix material comprises calcium oxide, aluminum oxide, titanium dioxide, vanadium pentoxide, silicon oxide, iron oxide, magnesium oxide and zinc oxide;
wherein the mass fraction of the silicon oxide is 20-40%, the content of the calcium oxide is 10-20%, and the content of other substances is 40-70%.
Has the advantages that: the basic materials of the product are common inorganic materials, are easy to obtain and low in price, so that the manufacturing cost of the product is reduced, and the process difficulty of the product is reduced. According to the invention, the addition amounts of cristobalite, phosphorosilicate, melilite, spinel, magrose pyroxene, anorthite, pyroxene and mullite are optimized for multiple times, so that the base material meets the proportion that the mass fraction of silicon oxide is 20-40%, the content of calcium oxide is 10-20%, and the content of other substances is 40-70%, and further, the product has good hardness, stability and high temperature resistance. Wherein, the silicon oxide increases the hardness and the strength of the product of the invention, and the calcium oxide increases the particle stability and the high temperature resistance of the product of the invention after the high temperature participates in the reaction.
Preferably, in the step (2), the amount of the binder is 0.5-2% of the total mass of the base material; the adhesive is a mixture of silicate adhesive, aluminate adhesive and phosphate adhesive;
wherein, the silicate binder comprises one or more of calcium silicate cement, sodium silicate, potassium silicate and bonding clay;
the aluminate cement binder comprises one or more of calcium aluminate cement, barium aluminate cement and spinel-containing calcium aluminate cement;
the phosphate type adhesive comprises one or more of aluminum dihydrogen phosphate, magnesium phosphate, ammonium phosphate, aluminum chromium phosphate, sodium tripolyphosphate and sodium hexametaphosphate.
Has the advantages that: the adhesive of the product of the invention can chemically react with the basic material under the addition of water, and lays a foundation for preparing and forming products with good hardness, stability and high temperature resistance. The chemical reaction equation of part of the adhesive, the matrix material and the water is as follows.
Na2SiO3+CaO+H2O＝CaSiO3+2NaOH；
CaO·Al2O3+10H2O＝CaO·Al2O3·10H2O；
2(CaO·Al2O3)+11H2O＝2CaO·Al2O3·8H2O+Al2O3·3H2O；
3(CaO·Al2O3)+12H2O＝3CaO·Al2O3·6H2O+2(Al2O3·3H2O)；
2AlO2 -+CO2+3H2O＝2Al(OH)3+CO3 2-；
2H3PO4+3CaO＝Ca3(PO4)2+3H2O；
Al2O3+6H3PO4＝2Al(H2PO4)3+6H2O；
Al2O3+3H3PO4＝Al2(HPO4)3+3H2O；
Al2O3+2H3PO4＝2AlPO4+3H2O；
The action mechanism of the silicate inorganic binder is as follows: in the heating curing process, the silicate and the aluminum are bonded and cured to form a strong structure mainly containing silicon, oxygen and aluminum in a three-dimensional space, so that the adhesive has high bonding force.
The action mechanism of the aluminate cement binder is as follows: (CaO. Al)2O3)·CaSO4And gypsum to form ettringite and Al (OH)3And (4) gelling. The dicalcium silicate formed at lower temperatures hydrates more rapidly to form hydrated calcium silicate gels, whereas Al (OH)3And calcium silicate hydrate gel is filled among calcium sulfate hydrate to reinforce and compact the structure of the set cement.
The action mechanism of the phosphate adhesive is as follows: phosphate binders are generally prepared by reacting an acid salt or derivative of phosphoric acid with a weak base or amphoteric oxide at ambient temperature. The metal ions having a smaller cation radius contribute to the formation of a disordered or glassy structure, improving the adhesion. The phosphate adhesive not only has certain bonding strength at normal temperature, but also improves the bonding strength along with the improvement of temperature, and in addition, the phosphate adhesive has inherent high temperature resistance and corrosion resistance, thereby being beneficial to improving the stability of bonding products.
Preferably, the drying temperature in the step (2) is 100-120 ℃, and the time is 10-12 h;
the roasting temperature is 1100-1500 ℃, and the roasting time is 2-4 h.
Has the advantages that: the roasting temperature of the product is 1100-1500 ℃, the high temperature resistance of the product is ensured, the formation of a porous structure of the product is promoted, and the thermal stability of the product is ensured.
Preferably, the porous spherical particles in the step (2) are of a porous structure, and the pore size is 0.3-10 μm.
Has the advantages that: the product is of a spherical porous structure, the pore size is 0.3-10 mu m, and the product not only can filter dust substances and organic matters in wastewater, but also ensures the structural stability of the product.
Use of porous spherical particles for filtering waste water.
Preferably, the wastewater contains fine impurities, specifically fine particles such as dust, and the treatment method comprises the following steps:
and putting the porous spherical particles into wastewater containing fine impurities for adsorption, taking out the spherical particles saturated in adsorption, drying, and performing vibration screening on the dried spherical particles to recycle.
Has the advantages that: the fine impurities adsorbed by the porous spherical particles can escape from the pores of the spherical particles under the vibration screening of the vibrating screen. The spherical particles after vibration screening can be put into the wastewater again for recycling.
Preferably, the wastewater contains organic matter, and the treatment method comprises the following steps:
and putting the porous spherical particles into the organic matter-containing wastewater for adsorption, taking out the spherical particles after adsorption is finished, drying, and then roasting at high temperature, cooling, vibrating and screening to obtain the porous spherical particles which can be recycled.
The spherical particles with saturated adsorption are taken out and dried at the temperature of 100-160 ℃, the vibration screening of the spherical particles with saturated adsorption and drying is vibration screening on a top impact type vibration screen, and the vibration screening time is 4-8 hours.
Has the advantages that: the organic matters in the spherical particles are roasted at high temperature to become inorganic matters, and the inorganic matters run out of the pores of the spherical particles under the vibration screening of a vibration screen after being cooled to room temperature; the spherical particles after vibration screening can be put into the wastewater again for recycling.
The remarkable progress is that: the invention has simple manufacturing process and convenient operation.
According to the technical scheme, compared with the prior art, the porous spherical particles are prepared at 1100-1500 ℃, can be used at high temperature, have higher hardness and thermal stability, and do not have flammability. The usable temperature range of the product is room temperature to 800 ℃, the Mohs hardness at room temperature is 6-6.5, and the stability of the particles at room temperature is 93-96%. In addition, the spherical particles have small pore diameter, and can filter macromolecular organic matters and fine impurities in the wastewater so as to purify the wastewater. The impurities in the spherical particles can be cleaned only by vibration, the bearable amplitude is 10mm, and the vibration strength of the product can not be born by other materials in the prior art. Finally, the product provided by the invention is low in manufacturing cost, can be repeatedly recycled, and is suitable for industrial popularization.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a photograph showing a physical example of porous spherical particles obtained in example 1 of the present invention;
FIG. 2 is a photograph showing a physical example of porous spherical particles obtained in example 2 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention discloses a preparation method of porous spherical particles, which comprises the following specific steps:
(1) preparing a base material: pulverizing and uniformly mixing various raw materials of cristobalite, phosphorosilicate, melilite, spinel, magrose pyroxene, anorthite, pyroxene and mullite to obtain a base material with the particle size of 300-800 meshes;
(2) preparing porous spherical particles for filtering wastewater: uniformly mixing the base materials, adding an adhesive into the base materials at normal temperature, kneading for 20-30 min at 30-50 ℃, drying, roasting and screening to obtain the porous spherical particles.
In order to further optimize the technical scheme, in the step (1), the mass fraction of the cristobalite in the raw materials is 20-40%, the mass fraction content of the phosphorosilicate is 10-20%, and the total mass fraction of other raw materials is 30-40%;
the powder preparation method comprises one or two of crushing, dry grinding and wet grinding.
Further, in the step (2), the dosage of the adhesive accounts for 0.5 to 2 percent of the total mass of the base material; the adhesive is a mixture of silicate adhesive, aluminate adhesive and phosphate adhesive;
wherein the silicate binder comprises one or more of calcium silicate cement, sodium silicate, potassium silicate and bonding clay;
the aluminate binder comprises one or more of calcium aluminate cement, barium aluminate cement and calcium aluminate cement containing spinel;
the phosphate adhesive comprises one or more of aluminum dihydrogen phosphate, magnesium phosphate, ammonium phosphate, aluminum chromium phosphate, sodium tripolyphosphate and sodium hexametaphosphate.
Further, in the step (2), the drying temperature is 100-120 ℃, and the time is 10-12 hours;
the roasting temperature is 1100-1500 ℃, and the time is 2-4 h.
Further, the porous spherical particles in the step (2) are of a porous structure, and the pore size is 0.3-10 μm.
Use of porous spherical particles for filtering waste water.
Furthermore, the waste water contains fine impurities, and the treatment method comprises the following steps:
and putting the porous spherical particles into wastewater containing fine impurities for adsorption, taking out the spherical particles saturated in adsorption, drying, and performing vibration screening on the dried spherical particles to recycle.
Furthermore, the waste water contains organic matters, and the treatment method comprises the following steps:
and putting the porous spherical particles into the organic matter-containing wastewater for adsorption, taking out the spherical particles after adsorption is finished, drying, and then roasting at high temperature, cooling, vibrating and screening to obtain the porous spherical particles which can be recycled.
The above technical solution is further illustrated by the following specific examples.
Example 1
(1) Preparing a base material: the method comprises the following steps of taking 20% of cristobalite, 15% of phosphorus quartz, 15% of melilite, 10% of spinel, 10% of magnesian rosepside, 10% of anorthite, 10% of pyroxene and 10% of mullite in percentage by mass as raw materials, and crushing, dry grinding and wet grinding the raw materials to prepare powder with the particle size of 300-800 meshes as a base material, wherein the total amount of the powder is 5 kg.
(2) Preparing spherical particles with high thermal stability for filtering wastewater: and (2) mixing the matrix material obtained in the step (1) with 0.05kg of 35% of sodium silicate, 25% of spinel calcium aluminate and 15% of aluminum dihydrogen phosphate (all powders), uniformly mixing, adding 600g of water, uniformly mixing and kneading in a kneading pot at 30 ℃ for 25min to obtain spherical particles, drying at 120 ℃ for 12h, roasting at 1100 ℃ and keeping the temperature for 4h, wherein the heating rate is 10 ℃/min. And finally, screening the wastewater by using a standard screen with square holes of 5-10 mm on a top-impact type sieving machine to obtain spherical particles (shown in figure 1) with high thermal stability, wherein the size of the particles is 5-10 mm, and the size of the particles is 0.3-10 microns.
Example 2
(1) Preparing a base material: the method comprises the following steps of taking 25% of cristobalite, 20% of phosphorus quartz, 15% of melilite, 10% of spinel, 10% of magnesian rosepside, 10% of anorthite and 10% of pyroxene as raw materials by mass fraction, taking 5kg in total, and crushing, dry-grinding and wet-grinding the raw materials to prepare powder with the particle size of 300-800 meshes as a base material.
(2) Preparing spherical particles with high thermal stability for filtering wastewater: and (2) mixing the matrix material obtained in the step (1), 35% of calcium silicate, 25% of calcium aluminate cement and 15% of aluminum dihydrogen phosphate (all powders) to total 0.05kg, uniformly mixing, adding 600g of water, uniformly mixing and kneading in a kneading pot at 30 ℃ for 25min to obtain spherical particles, drying at 120 ℃ for 12h, roasting at 1100 ℃ and keeping the temperature for 4h, wherein the heating rate is 10 ℃/min. And finally, screening the wastewater by using a standard screen with square holes of 5-10 mm on a top-impact type sieving machine to obtain spherical particles (shown in figure 2) with high thermal stability, wherein the size of the particles is 5-10 mm, and the size of the particles is 0.3-10 microns.
Example 3
(1) Preparing a base material: the method comprises the following steps of taking 25% of cristobalite, 20% of phosphorus quartz, 15% of melilite, 10% of spinel, 10% of magnesian rosepside, 10% of anorthite and 10% of pyroxene as raw materials by mass fraction, taking 5kg in total, and crushing, dry-grinding and wet-grinding the raw materials to prepare powder with the particle size of 300-800 meshes as a base material.
(2) Preparing spherical particles with high thermal stability for filtering wastewater: and (2) uniformly mixing the matrix material obtained in the step (1), 50% of sodium silicate and 50% of spinel calcium aluminate (all powders) to total 0.05kg, adding 600g of water, uniformly kneading in a kneading pot at 30 ℃ for 25min to obtain spherical particles, drying at 120 ℃ for 12h, roasting at 1100 ℃ and keeping the temperature for 4h, wherein the heating rate is 10 ℃/min. And finally, screening the wastewater by using a standard screen with square holes of 5-10 mm on a top impact type sieving machine to obtain spherical particles with high thermal stability, wherein the size of the particles is 5-10 mm, and the size of the particles is 0.3-10 microns.
Example 4
(1) Preparing a base material: the method comprises the following steps of taking 25% of cristobalite, 20% of phosphorus quartz, 15% of melilite, 10% of spinel, 10% of magnesian rosepside, 10% of anorthite and 10% of pyroxene as raw materials by mass fraction, taking 5kg in total, and crushing, dry-grinding and wet-grinding the raw materials to prepare powder with the particle size of 300-800 meshes as a base material.
(2) Preparing spherical particles with high thermal stability for filtering wastewater: and (2) uniformly mixing the base material obtained in the step (1), 50% of sodium silicate and 50% of aluminum dihydrogen phosphate (all powders) to total 0.05kg, adding 600g of water, uniformly kneading in a kneading pot at 30 ℃ for 25min to obtain spherical particles, drying at 120 ℃ for 12h, roasting at 1100 ℃ and keeping the temperature for 4h, wherein the heating rate is 10 ℃/min. And finally, screening the wastewater by using a standard screen with square holes of 5-10 mm on a top impact type sieving machine to obtain spherical particles with high thermal stability, wherein the size of the particles is 5-10 mm, and the size of the particles is 0.3-10 microns.
Example 5
(1) Preparing a base material: the method comprises the following steps of taking 25% of cristobalite, 20% of phosphorus quartz, 15% of melilite, 10% of spinel, 10% of magnesian rosepside, 10% of anorthite and 10% of pyroxene as raw materials by mass fraction, taking 5kg in total, and crushing, dry-grinding and wet-grinding the raw materials to prepare powder with the particle size of 300-800 meshes as a base material.
(2) Preparing spherical particles with high thermal stability for filtering wastewater: and (2) uniformly mixing the matrix material obtained in the step (1), 50% of spinel calcium aluminate and 50% of aluminum dihydrogen phosphate (both powders) to total 0.05kg, adding 600g of water, uniformly kneading in a kneading pot at 30 ℃ for 25min to obtain spherical particles, drying at 120 ℃, roasting at 1100 ℃ and keeping the temperature for 4h, wherein the heating rate is 10 ℃/min. And finally, screening the wastewater by using a standard screen with square holes of 5-10 mm on a top impact type sieving machine to obtain spherical particles with high thermal stability, wherein the size of the particles is 5-10 mm, and the size of the particles is 0.3-10 microns.
Example 6
(1) Preparing a base material: the method comprises the following steps of taking 20% of cristobalite, 15% of phosphorus quartz, 15% of melilite, 10% of spinel, 10% of magnesian rosepside, 10% of anorthite, 10% of pyroxene and 10% of mullite in percentage by mass as raw materials, and crushing, dry grinding and wet grinding the raw materials to prepare powder with the particle size of 300-800 meshes as a base material, wherein the total amount of the powder is 5 kg.
(2) Preparing spherical particles with high thermal stability for filtering wastewater: and (2) mixing the matrix material obtained in the step (1), 35% of sodium silicate, 25% of spinel calcium aluminate and 15% of aluminum dihydrogen phosphate (all powders) to total 0.05kg, uniformly mixing, adding 600g of water, uniformly mixing and kneading in a mixing and kneading pot at 50 ℃ for 40min to obtain spherical particles, drying at 120 ℃ for 12h, roasting at 1200 ℃ and keeping the temperature for 4h, wherein the heating rate is 10 ℃/min. And finally, screening the wastewater by using a standard screen with square holes of 5-10 mm on a top impact type sieving machine to obtain spherical particles with high thermal stability, wherein the size of the particles is 5-10 mm, and the size of the particles is 0.3-10 microns.
Example 7
The porous spherical particles prepared in example 1 were used to filter wastewater containing fine impurities, and the specific steps were as follows:
and putting the porous spherical particles into wastewater containing fine impurities for adsorption, taking out the spherical particles saturated in adsorption, drying, and performing vibration screening on the dried spherical particles to recycle.
Example 8
The application of porous spherical particles in filtering wastewater, which contains organic matters, comprises the following specific steps:
and putting the porous spherical particles into the organic matter-containing wastewater for adsorption, taking out the spherical particles after adsorption is finished, drying, roasting at high temperature of 600-800 ℃, cooling, vibrating and screening, and recycling. The product of the invention is roasted. The organic matter attached to the product of the present invention is converted into inorganic matter which is easy to handle, and further removed from the spherical particles of the present invention by vibratory screening.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. The preparation method of the porous spherical particles is characterized by comprising the following steps:
(1) preparing a base material: preparing powder from various raw materials of cristobalite, phosphorosilicate, melilite, spinel, magrose pyroxene, anorthite, pyroxene and mullite to obtain a base material with the particle size of 300-800 meshes;
(2) preparing porous spherical particles: uniformly mixing the base materials, adding an adhesive into the base materials at normal temperature, kneading the mixture for 20-30 min at 30-50 ℃ to form a spherical shape, and then drying, roasting and screening the spherical shape to obtain the porous spherical particles.
2. The preparation method of the porous spherical particles as claimed in claim 1, wherein in the step (1), the mass fraction of the cristobalite in the raw materials is 20-40%, the mass fraction of the phosphorosilicate is 10-20%, the mass fraction of the melilite is 5-15%, the mass fraction of the mullite is 0-10%, the rest raw materials are one or more of spinel, magrose pyroxene, anorthite and pyroxene, and the mass fractions of any two raw materials of the spinel, the magrose pyroxene, the anorthite and the pyroxene are the same.
3. The method for preparing porous spherical particles according to claim 2, wherein the matrix material contains 20-40% by mass of silicon oxide, 10-20% by mass of calcium oxide and 40-70% by mass of other substances.
4. The method of claim 1, wherein the milling in step (1) comprises one or two of crushing, dry milling and wet milling.
5. The method for preparing porous spherical particles according to claim 1, wherein the amount of the binder used in the step (2) is 0.5-2% of the total mass of the matrix material; the adhesive is a mixture of silicate adhesive, aluminate adhesive and phosphate adhesive;
wherein, the silicate binder comprises one or more of calcium silicate cement, sodium silicate, potassium silicate and bonding clay;
the aluminate binder comprises one or more of calcium aluminate cement, barium aluminate cement and spinel-containing calcium aluminate cement;
the phosphate type adhesive comprises one or more of aluminum dihydrogen phosphate, magnesium phosphate, ammonium phosphate, aluminum chromium phosphate, sodium tripolyphosphate and sodium hexametaphosphate.
6. The method for preparing porous spherical particles according to claim 1, wherein the drying temperature in step (2) is 100-120 ℃ and the drying time is 10-12 h;
the roasting temperature is 1100-1500 ℃, and the roasting time is 2-4 h.
7. The method for preparing porous spherical particles according to claim 1, wherein the porous spherical particles in step (2) have a porous structure and a pore size of 0.3-10 μm.
8. Use of a porous spherical particle according to any one of claims 1 to 7 for filtering waste water containing fine impurities or organic matter.
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