CN108579662A - One kind preparing SiO from low-grade kaolin2/Al2O3The method of composite material - Google Patents
One kind preparing SiO from low-grade kaolin2/Al2O3The method of composite material Download PDFInfo
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- CN108579662A CN108579662A CN201810359136.XA CN201810359136A CN108579662A CN 108579662 A CN108579662 A CN 108579662A CN 201810359136 A CN201810359136 A CN 201810359136A CN 108579662 A CN108579662 A CN 108579662A
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- sio
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/103—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/06—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
-
- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
Abstract
The invention discloses one kind preparing SiO from low-grade kaolin2/Al2O3The method of composite material, this method are stirred low-grade kaolin and hydrochloric acid to obtain kaolin slurry in a stirring kettle, and washings and mixture are obtained after being filtered, washed;The mixture is reacted with salpeter solution, aluminum nitrate solution and silica solid is obtained by filtration, then hydrofluoric acid is mixed with silica solid, silicon fluoride gas caused by reaction is collected with gas collection bag;Aluminum nitrate solution is mixed in a kettle with hydroxide solution, then collected hydrogen fluoride gas is passed through in the reaction kettle and is reacted, is filtered, washed to obtain the mixed solution and SiO of hydrofluoric acid and sodium nitrate2/Al(OH)3Presoma, presoma calcine to obtain SiO2/Al2O3 composite materials.This method raw material is sufficient, cheap, and wet purification process can carry out at a lower temperature, has the advantages that low energy consumption, at low cost, equipment is simple, and treating capacity is big.
Description
Technical field
The invention belongs to chemical engineering of materials fields, and in particular to one kind preparing SiO from low-grade kaolin2/Al2O3It is compound
The method of material.
Background technology
China's kaolin resource is extremely abundant, and total resources is at the forefront in the world.For a long time, most kaolin are only used
Make the raw material of ceramics or as volume type non-functional packing material.Simultaneously as utilizing improper, utilization rate ten to kaolinic
Point low, tailings output capacity is very high, and kaoline tailing processing constructs Tailings Dam using landform mostly, stacks or backfilled again on the spot
It cultivates, seriously pollutes environment, break the ring ecological balance, while causing being largely lost for resource.
Kaolin is divided into high low-grade because the ingredient type difference contained and each content of material accounting are different.
Quality is purer, the higher kaolin of grade have washed kaolin processing after physicochemical characteristic, for example whiteness, can
The features such as plasticity, dispersibility, fire resistance, associativity, ion exchangeable, chemical stability and electrical insulating property, thus answered extensively
For the five big category of industry such as papermaking, coating, ceramics, rubber, additive.With industry products matter such as ceramics, glass and chemical industry
The promotion of amount, high-grade kaolin starting material demand is increasing, and China's high grade kaolinite resource is increasingly reduced.
In the abundant kaolin resource in China, the lower kaolin inferior of grade occupies sizable ratio, because its
Utilization rate is very low, and wherein most, which is stacked, discards, this not only occupies a large amount of soils, but also seriously pollutes environment.It is existing
Low-grade kaolin, wherein about containing O:58.1%, Si:25.2%, Al:13.0% equal elements.
Uniqueness possessed by earth silicon material makes it in catalysis, adsorbing separation, macromolecular carrier, sensor and drug
It is used widely in the fields such as controlled release;And aluminium oxide is a kind of important industrial chemicals, is widely used in ceramics, medicine, absorption
The fields such as material, catalyst and catalyst carrier.Both products have a good application prospect.
The lower kaolin inferior of resourceful grade, a kind of easy harmless treatment of exploration is made full use of to discard
Oil-base mud new process, new method, purification prepare SiO2/Al2O3Composite material, by the composite material prepared for adsorbing
Pollutant has a very important significance the dirty unit pollution innoxious governance of improvement, the production of local environment.But this respect
Research be but rarely reported.
Invention content
For the application present situation of low-grade kaolin, the present invention provides a kind of wet purification process, using low-grade height
Ridge soil mineral are raw material, and purification prepares SiO2/Al2O3Composite material, and the composite material prepared is polluted for adsorbing
Object.
Technical scheme is as follows:
One kind preparing SiO from low-grade kaolin2/Al2O3The method of composite material, including:By low-grade kaolin and
Hydrochloric acid is stirred to obtain kaolin slurry in a stirring kettle, and washings and mixture are obtained after being filtered, washed;By the mixing
Object is reacted with salpeter solution, aluminum nitrate solution and silica solid is obtained by filtration, then hydrofluoric acid and silica solid are mixed
It closes, silicon fluoride gas caused by reaction is collected with gas collection bag;By aluminum nitrate solution and hydroxide solution in reaction kettle
Middle mixing, then collected hydrogen fluoride gas is passed through in the reaction kettle, after reacting a period of time, filtration washing obtains hydrogen
The mixed solution and SiO of fluoric acid and sodium nitrate2/Al(OH)3Presoma, Muffle furnace calcine SiO2/Al(OH)3Presoma obtains
SiO2/Al2O3Composite material.
Further, above-mentioned that SiO is prepared from low-grade kaolin2/Al2O3The method of composite material, by the washings
It is passed through in settling tank, adsorbent is added and is stirred continuously, is discharged after solution is up to standard.
Further, above-mentioned that SiO is prepared from low-grade kaolin2/Al2O3The method of composite material, by hydrofluoric acid and nitre
The mixed solution of sour sodium is mixed with milk of lime, isolated CaF after reaction2And sodium nitrate solution, sodium nitrate solution re-evaporation are dense
Contracting obtains sodium nitrate solid.
Further, above-mentioned that SiO is prepared from low-grade kaolin2/Al2O3The method of composite material, the hydroxide
For sodium hydroxide.
Further, above-mentioned that SiO is prepared from low-grade kaolin2/Al2O3The method of composite material, the matter of the hydrochloric acid
It is 5%~20% to measure score, and the mass fraction of the salpeter solution is 30%~45%, and the mass fraction of the hydrofluoric acid is
30%~40%.
Further, above-mentioned that SiO is prepared from low-grade kaolin2/Al2O3The method of composite material, with low-grade kaolinite
Native inventory is counted for 100g, and each material amounts are:200~300ml of hydrochloric acid, 150~200ml of salpeter solution, hydrofluoric acid 150~
250ml, 40~60g of hydroxide, 100~150g of milk of lime.
Further, above-mentioned that SiO is prepared from low-grade kaolin2/Al2O3The method of composite material, the mixture with
The reaction temperature of salpeter solution is 130~180 DEG C, and the time is 2~5.0h, and Muffle furnace calcination temperature is 300~700 DEG C, calcining
Time is 1~3.0h.
The present invention still further provides the SiO of above method preparation2/Al2O3Composite material is in adsorbing Wastewater Pollutant
Application.Some specific embodiments according to the present invention, SiO prepared by the above method2/Al2O3Composite material is to Congo red, first
Base indigo plant and quadracycline have stronger adsorption capacity.
The preparation method of the present invention uses low-grade kaolinite ore object for raw material, and source is sufficient, cheap, reduces into
This, and wet purification process can carry out at a lower temperature, have that low energy consumption, and at low cost, equipment is simple, and it is excellent that treating capacity is big etc.
Product is applied to pollution control by point, and low-grade kaolinite ore object has been opened up again while reducing kaolin pollution inferior
Environmentally friendly application approach.Rationally to utilize low-grade kaolin, avoids the wasting of resources, environmental protection from reducing pollutant emission, promote
Ecological Civilization Construction forms good economic benefit, social benefit, environmental benefit, provides a kind of easy harmless treatment
Method.
Description of the drawings
Fig. 1 is that 1 sample of embodiment changes collection of illustrative plates to the absorption of Congo red, methyl blue and quadracycline;
Fig. 2 is that the embodiment of the present invention prepares SiO2/Al2O3The synthetic schemes of composite material.
Specific implementation mode
SiO is prepared in the slave low-grade kaolin of the present invention2/Al2O3The method of composite material, including:By low-grade kaolinite
Soil and hydrochloric acid are stirred to obtain kaolin slurry in a stirring kettle, and washings and mixture are obtained after being filtered, washed;It will be described
Mixture is reacted with salpeter solution, aluminum nitrate solution and silica solid is obtained by filtration, then hydrofluoric acid and silica are consolidated
Body mixes, and silicon fluoride gas caused by reaction is collected with gas collection bag;By aluminum nitrate solution with hydroxide solution anti-
It answers in kettle and is mixed, then collected hydrogen fluoride gas is passed through in the reaction kettle, after reacting a period of time, filtration washing obtains
To the mixed solution and SiO of hydrofluoric acid and sodium nitrate2/Al(OH)3Presoma, Muffle furnace calcine SiO2/Al(OH)3Presoma
Obtain SiO2/Al2O3Composite material.
For the consideration of environmental protection, some embodiments of the present invention further provide the processing side of above method by-product
Method.For example, in some embodiments of the invention, the washings are passed through in settling tank, adsorbent is added and is stirred continuously, waits for
Discharge after solution is up to standard.And the mixed solution of hydrofluoric acid and sodium nitrate is mixed with milk of lime, isolated CaF after reaction2
And sodium nitrate solution, sodium nitrate solution re-evaporation are concentrated to give sodium nitrate solid.The CaF of gained2With sodium nitrate but also as pair
Product is used.
In the present invention, term hydroxide is the compound that can provide hydroxide ion, typically alkali metal hydroxide
Object, for example, lithium hydroxide, sodium hydroxide, potassium hydroxide, the embodiment of the present invention mainly uses sodium hydroxide, but art technology
Personnel are appreciated that it is not limited to this.
In the present invention, term hydrochloric acid, hydrofluoric acid, salpeter solution are HCl, HF, HNO respectively3Aqueous solution, in the present invention
Some embodiments in, the mass fraction of hydrochloric acid is 5%~20%, and the mass fraction of salpeter solution is 30%~45%, hydrogen fluorine
The mass fraction of acid is 30%~40%.
In some embodiments of the invention, the rate of charge of the preparation method reactant is with low-grade kaolin inventory
It is counted for 100g, each material amounts are:200~300ml of hydrochloric acid, 150~200ml of salpeter solution, 150~250ml of hydrofluoric acid, hydrogen-oxygen
40~60g of compound, 100~150g of milk of lime.
One embodiment of the present of invention also further illustrates the SiO of above method preparation2/Al2O3Composite material is adsorbing
Application in Wastewater Pollutant.The embodiment with the adsorption capacity of Congo red, methyl blue and quadracycline test compound material,
By testing result as can be seen that the method for the present invention will be resourceful, and the low-grade kaolinite that can cause environmental pollution
Soil obtains the SiO with higher utility value using succinct effective Methods For Purification2/Al2O3Composite material is applied to environment
Pollution is handled, with obvious effects.
It is illustrated below by way of specific embodiment is further to the invention content of the present invention, but should not be construed as the present invention
Range be only limitted to example below, invention thinking according to the present invention and entire contents, can will be each in following instance
Technical characteristic makes combination/replacement/adjustment/modification appropriate etc., this is will be obvious to those skilled in the art that still
Belong to the scope that the present invention protects.
Low-grade kaolin each element content such as following table used in following embodiment:
Embodiment 1
It weighs 100g kaolin to be added in the stirred tank for the dilute hydrochloric acid solution for being 5% equipped with 300ml mass fractions, stirring
Mixed liquor in stirred tank is poured into the filter residue being obtained by filtration in seperator and about 400ml washings by 30min.It is washed above-mentioned
It washs water to be passed through in settling tank, 4g adsorbents are added and stop stirring after being stirred continuously 60min, discharged after solution is up to standard.Filter residue
It then reacts in 150 DEG C of reaction kettle with the salpeter solution for being 30% equipped with 200ml mass fractions, after reacting 2h, is obtained by filtration
Aluminum salt solution and solid SiO2, solid is mixed with 200ml hydrofluoric acid and gas collection bag is used to collect silicon fluoride gas;Aluminium salt is molten
20min is then mixed in liquid in a kettle with the sodium hydroxide of 40g, then the silicon fluoride gas of above-mentioned collection is passed through reaction kettle
In.After reacting 10min, mixed solution is poured into, SiO is obtained by filtration in seperator2/Al(OH)3Presoma and hydrofluoric acid and
The mixed solution of sodium nitrate mixes mixed solution with the milk of lime that mass fraction is 100g, isolated CaF2And sodium nitrate
Solution, sodium nitrate solution re-evaporation are concentrated to give sodium nitrate solid;Above-mentioned SiO2/Al(OH)3Presoma is placed in temperature 60 in baking oven
DEG C dry 6h, then be placed in 500 DEG C of Muffle kiln roasting 3h and obtain SiO2/Al2O3Composite material.Flow chart is referring to Fig. 2.
Embodiment 2
It weighs 100g kaolin to be added in the stirred tank for the dilute hydrochloric acid solution for being 10% equipped with 200ml mass fractions, stirring
Mixed liquor in stirred tank is poured into the filter residue being obtained by filtration in seperator and about 400ml washings by 30min.It is washed above-mentioned
It washs water to be passed through in settling tank, 4g adsorbents are added and stop stirring after being stirred continuously 60min, discharged after solution is up to standard.Filter residue
It then reacts in 150 DEG C of reaction kettle with the salpeter solution for being 40% equipped with 150ml mass fractions, after reacting 2h, is obtained by filtration
Aluminum salt solution and solid SiO2, solid is mixed with 200ml hydrofluoric acid and gas collection bag is used to collect silicon fluoride gas;Aluminium salt is molten
20min is then mixed in liquid in a kettle with the sodium hydroxide of 40g, then the silicon fluoride gas of above-mentioned collection is passed through reaction kettle
In.After reacting 10min, mixed solution is poured into, SiO is obtained by filtration in seperator2/Al(OH)3Presoma and hydrofluoric acid and
The mixed solution of sodium nitrate mixes mixed solution with the milk of lime of 100g, isolated CaF2And sodium nitrate solution, sodium nitrate
Solution re-evaporation is concentrated to give sodium nitrate solid;Above-mentioned SiO2/Al(OH)3Presoma is placed in temperature 60 C in baking oven and dries 6h, then
It is placed in 500 DEG C of Muffle kiln roasting 3h and obtains SiO2/Al2O3Composite material.
Embodiment 3
It weighs 100g kaolin to be added in the stirred tank for the dilute hydrochloric acid solution for being 20% equipped with 200ml mass fractions, stirring
Mixed liquor in stirred tank is poured into the filter residue being obtained by filtration in seperator and about 400ml washings by 30min.It is washed above-mentioned
It washs water to be passed through in settling tank, 4g adsorbents are added and stop stirring after being stirred continuously 60min, discharged after solution is up to standard.Filter residue
It then reacts in 150 DEG C of reaction kettle with the salpeter solution for being 40% equipped with 150ml mass fractions, after reacting 2h, is obtained by filtration
Aluminum salt solution and solid SiO2, solid is mixed with 200ml hydrofluoric acid and gas collection bag is used to collect silicon fluoride gas;Aluminium salt is molten
20min is then mixed in liquid in a kettle with the sodium hydroxide of 40g, then the silicon fluoride gas of above-mentioned collection is passed through reaction kettle
In.After reacting 10min, mixed solution is poured into, SiO is obtained by filtration in seperator2/Al(OH)3Presoma and hydrofluoric acid and
The mixed solution of sodium nitrate mixes mixed solution with the milk of lime that mass fraction is 100g, isolated CaF2And sodium nitrate
Solution, sodium nitrate solution re-evaporation are concentrated to give sodium nitrate solid;Above-mentioned SiO2/Al(OH)3Presoma is placed in temperature 60 in baking oven
DEG C dry 6h, then be placed in 500 DEG C of Muffle kiln roasting 3h and obtain SiO2/Al2O3Composite material.
Embodiment 4
Weigh the 100mg SiO of the preparation of embodiment 12/Al2O3Composite sample is added to a concentration of 50mg/L's of 100mL
In dyestuff or antibiotic (Congo red, methyl blue or quadracycline) solution, it is placed on magnetic stirring apparatus and at the uniform velocity stirs, exist respectively
1,2,3,4,6,8,10,12,15,18,21,24min sampling 5mL and with the processing of 0.22 μm of membrane filtration, using UV, visible light
Spectrophotometric determination solution concentration, processing data are as shown in Figure 1.
It can be seen that SiO2/Al2O3Three kinds of compounds of composite material pair have preferable adsorption capacity.It is prepared by low-grade kaolin
At SiO2/Al2O3Composite material is a kind of feasible method simply turned waste into wealth for environmental protection.
Claims (8)
1. one kind preparing SiO from low-grade kaolin2/Al2O3The method of composite material, which is characterized in that including:By low product
Position kaolin and hydrochloric acid are stirred to obtain kaolin slurry in a stirring kettle, and washings and mixture are obtained after being filtered, washed;
The mixture is reacted with salpeter solution, is obtained by filtration aluminum nitrate solution and silica solid, then by hydrofluoric acid solution with
Silica solid mixes, and silicon fluoride gas caused by reaction is collected with gas collection bag;By aluminum nitrate solution and hydroxide
Object solution is mixed in a kettle, then collected hydrogen fluoride gas is passed through in the reaction kettle, after reacting a period of time,
Filtration washing obtains the mixed solution and SiO of hydrogen fluoride and sodium nitrate2/Al(OH)3Presoma, Muffle furnace calcine SiO2/Al
(OH)3Presoma obtains SiO2/Al2O3Composite material.
2. according to claim 1 prepare SiO from low-grade kaolin2/Al2O3The method of composite material, feature exist
In, the washings are passed through in settling tank, be added adsorbent be stirred continuously, discharged after solution is up to standard.
3. according to claim 1 prepare SiO from low-grade kaolin2/Al2O3The method of composite material, feature exist
In the mixed solution of hydrofluoric acid and sodium nitrate being mixed with milk of lime, isolated CaF after reaction2And sodium nitrate solution, nitric acid
Sodium solution re-evaporation is concentrated to give sodium nitrate solid.
4. according to claim 1 prepare SiO from low-grade kaolin2/Al2O3The method of composite material, feature exist
In the hydroxide is sodium hydroxide.
5. according to claim 1 prepare SiO from low-grade kaolin2/Al2O3The method of composite material, feature exist
In the mass fraction of the hydrochloric acid is 5%~20%, and the mass fraction of the salpeter solution is 30%~45%, the hydrogen fluorine
The mass fraction of acid solution is 30%~40%.
6. according to claim 2 prepare SiO from low-grade kaolin2/Al2O3The method of composite material, feature exist
In, by low-grade kaolin inventory for 100g in terms of, each material amounts are:200~300ml of hydrochloric acid, salpeter solution 150~
200ml, 150~250ml of hydrofluoric acid solution, 40~60g of hydroxide, 100~150g of milk of lime.
7. according to claim 1 prepare SiO from low-grade kaolin2/Al2O3The method of composite material, feature exist
In the reaction temperature of the mixture and salpeter solution is 130~180 DEG C, and the time is 2~5.0h, and Muffle furnace calcination temperature is
300~700 DEG C, calcination time is 1~3.0h.
8. the SiO prepared such as claim 1~7 the method2/Al2O3Application of the composite material in adsorbing Wastewater Pollutant.
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Cited By (1)
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CN113751031A (en) * | 2021-08-20 | 2021-12-07 | 中国科学院上海有机化学研究所 | Composite solid acid, preparation method and application thereof |
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CN113751031B (en) * | 2021-08-20 | 2022-12-27 | 中国科学院上海有机化学研究所 | Composite solid acid, preparation method and application thereof |
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