CN107963646B - Method for rapidly preparing aluminum potassium sulfate by using vermiculite - Google Patents
Method for rapidly preparing aluminum potassium sulfate by using vermiculite Download PDFInfo
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- CN107963646B CN107963646B CN201711283328.9A CN201711283328A CN107963646B CN 107963646 B CN107963646 B CN 107963646B CN 201711283328 A CN201711283328 A CN 201711283328A CN 107963646 B CN107963646 B CN 107963646B
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- vermiculite
- potassium sulfate
- aluminum potassium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/68—Aluminium compounds containing sulfur
- C01F7/74—Sulfates
- C01F7/76—Double salts, i.e. compounds containing, besides aluminium and sulfate ions, only other cations, e.g. alums
- C01F7/762—Ammonium or alkali metal aluminium sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention relates to a method for rapidly preparing aluminum potassium sulfate by utilizing vermiculite. According to the method, vermiculite is used as a raw material to obtain the aluminum potassium sulfate product with high added value, and the method is low in cost, simple in process, high in nucleation speed, low in energy consumption, high in production efficiency, rich in raw material source and easy to industrialize; the aluminum potassium sulfate material can be obtained under different control conditions, the speed is different, the particle size is different, and the acidified vermiculite powder can be used as a filler of modified high molecular polymers (such as polyethylene, polypropylene and polyvinyl chloride), so that the resource utilization can be finally achieved.
Description
Technical Field
The invention relates to a method for preparing aluminum potassium sulfate dodecahydrate by using vermiculite as a raw material through a series of processes of crushing, acid leaching, stirring and heating, filtering, natural cooling and the like.
Background
The world has about 6 million tons of vermiculite reserves, of which China and Russia account for about two thirds, and others are mainly distributed in the United states and south Africa. The American vermiculite is mainly distributed in Mona, the reserve is about 8000 ten thousand tons, and accounts for two thirds of the total reserve of the American vermiculite; the total reserve of south Africa is about 7300 ten thousand tons, the main producing area is Palazera area, and the reserve accounts for more than 90% of the total reserve of vermiculite in south Africa; the former soviet union has more than 20 vermiculite deposits, of which the extra large are koldoff and badanine deposits, with a total reserve of about 2 hundred million tons being expected. Vermiculite is widely distributed in China, but is mostly distributed in the northern part of China, and mainly comprises provinces such as Xinjiang, Hebei, inner Mongolia, Liaoning, Shanxi, Shaanxi and the like; it is also distributed in Sichuan, Henan and Hubei Gansu provinces, mainly in metamorphic rock areas. The largest and most representative is the Liyue county in Xinjiang and the drybulac vermiculite ore, the reserves of which account for more than 90% of the total reserves in China, the second place in the world (second to south Africa only), and the prospect reserves of which are 1 hundred million tons, wherein the 2 # ore body has been proved to have the reserves of 1400 million tons, and is a rare super-large ore deposit in the world.
At present, vermiculite in Yuli county in Xinjiang is symbiotic with phlogopite, serpentinite and diopside, mainly golden yellow, black and silver gray are taken as main materials, and the vermiculite belongs to a hydrous aluminosilicate mineral with complex chemical components and is difficult to represent by a single chemical formula due to uncertain change. Generally, the content of each component in vermiculite is SiO2(37-42％)、Al2O3(9-17％)、Fe2O3(5-18％)、MgO(11-23％)、H2O (5-11%), Ca, Na and K. Because partial Si in the vermiculite is replaced by Al, the interlayer charge density is high, the interlayer spacing is small, and the ion exchange capacity is low, so that the method is one of the main reasons why the vermiculite cannot be widely applied. If a method could be used to drive off some of the Al in the vermiculite, thereby reducing its charge density, its ion exchange capacity would be improved and the structural stability of the vermiculite would be further improved by driving off some of the aluminium.
Based on the consideration, the vermiculite is treated by dilute sulfuric acid, and the acidified vermiculite powder can be applied to the aspects of petrochemical industry catalysis, water pollution heavy metal adsorption, building fireproof heat-insulating materials and the like, so that the application range of the vermiculite is expanded; in the process of preparing the potassium aluminum sulfate dodecahydrate by using the vermiculite, the potassium aluminum sulfate dodecahydrate with high added value can be prepared, and the acidified vermiculite powder is dried and then mixed with the nano calcium carbonate in a certain proportion to be used as the filler of the modified high molecular polymer. Therefore, the cheap Xinjiang raw ore vermiculite can be widely applied, and the cost for producing the product taking the high molecular polymer as the raw material is reduced, such as: PVC pipeline, fire prevention heated board.
For the dodecahydrate aluminum potassium sulfate, the energy consumption for producing the aluminum potassium sulfate by adopting the traditional aluminum hydroxide method is high, and the process is complex, so the cost for industrially synthesizing the aluminum potassium sulfate is increased. The invention adopts a preparation process with industrialization potential, has low raw material cost and high synthesis speed, and prepares the large-particle aluminum potassium sulfate dodecahydrate material. The material is a good raw material for preparing aluminum salt materials, water purifying agents, fire extinguishing agents, swelling agents, antibacterial drugs, paints, tanning materials and mordant materials, and has wide application prospects in the antigen repair method in bending prevention and immune organization of the primary coil copper tube of the intermediate frequency transformer in recent years.
Disclosure of Invention
The invention aims to provide a method for rapidly preparing aluminum potassium sulfate by utilizing vermiculite, which comprises the steps of cleaning raw ore vermiculite, drying, crushing, acidifying under certain conditions, filtering, taking filtrate, and placing the filtrate for crystallization; obtaining the aluminum potassium sulfate crystal. According to the method, vermiculite is used as a raw material to obtain the aluminum potassium sulfate product with high added value, and the method is low in cost, simple in process, high in nucleation speed, low in energy consumption, high in production efficiency, rich in raw material source and easy to industrialize; the aluminum potassium sulfate material can be obtained under different control conditions, the speed is different, the particle size is different, and the acidified vermiculite powder can be used as a filler of modified high molecular polymers (such as polyethylene, polypropylene and polyvinyl chloride), so that the resource utilization can be finally achieved.
The invention relates to a method for rapidly preparing aluminum potassium sulfate by utilizing vermiculite, which comprises the following steps:
a. cleaning vermiculite, drying, and crushing to 300 meshes to obtain vermiculite powder for later use;
b. slowly adding concentrated sulfuric acid with the concentration of 98% into the stirred deionized water, and continuously stirring for 10 min;
c. slowly adding the vermiculite powder obtained in the step a into the sulfuric acid aqueous solution obtained in the step b according to the proportion of adding 4mL of dilute sulfuric acid into every 1 g of vermiculite, and heating and stirring for 2-6 h at the temperature of 60-100 ℃ to obtain a mixture;
d. c, filtering the mixture in the step c, washing the mixture to be neutral by using deionized water, and taking the filtrate as an aluminum potassium sulfate crystal growth culture solution;
e. transferring the culture solution obtained in the step d into an open glass vessel, adding absolute ethyl alcohol, mixing to quickly generate small white grains, and obtaining the grains along with the standing time, wherein the volume ratio of the absolute ethyl alcohol to the culture solution is 1:1-1: 50;
f. and e, naturally airing the crystal grains obtained in the step e to obtain the aluminum potassium sulfate dodecahydrate product.
And e, the volume ratio of the absolute ethyl alcohol to the culture solution in the step e is 1: 10.
The invention relates to a method for rapidly preparing aluminum potassium sulfate by utilizing vermiculite, which is prepared by a series of processes of crushing, acid leaching, stirring, heating, filtering and natural cooling of raw material vermiculite, wherein the chemical formula is KAl (SO)4)2·12H2And O, wherein the vermiculite (g) is diluted sulfuric acid (mL) 1: 4.
The invention relates to a method for rapidly preparing aluminum potassium sulfate by utilizing vermiculite, which is prepared by a series of processes of raw material vermiculite through crushing, acid invasion, stirring, heating, filtering and natural cooling, wherein the aluminum potassium sulfate dodecahydrate crystal obtained by the method can be used for preparing raw materials in the aspects of aluminum salt materials, water purifying agents, fire extinguishing agents, swelling agents, antibacterial drugs, paints, tanning materials and mordant, and specifically 1, aluminum potassium sulfate (alum) is used as the water purifying agent; ionization of alum after dissolving in water produces A13+，A13+0H produced by ionization with water―The combination produces aluminum hydroxide, and the colloidal particles of aluminum hydroxide, which have positive charges, encounter the negatively charged silt particles and are neutralized. The colloidal particles, which lose their charge, quickly agglomerate together, and the larger the particle is, the more it ends up sinking into the water. Thus, the water becomes clear. 2. Potassium aluminum sulfate (alum) as a fire extinguishing agent; the foam fire extinguisher contains alum solution and NaHC03(baking soda) solution (with foaming agent) in a volume ratio of about 11: 2. the excess alum is used for fully reacting the baking soda in the fire extinguisher to release sufficient carbon dioxide so as to achieve the purpose of fire extinguishing. 3. Potassium aluminum sulfate (alum) is used as a swelling agent; when the baking soda is added into the flour and then the alum is added during frying the fried bread sticks (cakes), the same amount of baking soda releases twice more carbon dioxide than the baking soda alone, so that the fried bread sticks (cakes) can be swelled in a hot oil pot at a time, and the crispy and delicious fried bread sticks (cakes) are obtained. However, since alum contains aluminum ions and is potassium aluminum sulfate as a chemical component, excessive intake of alum can affect the absorption of iron, calcium and other components by human body, resulting in osteoporosis and anemiaAnd even to the development of nerve cells. 4. Potassium aluminum sulfate (alum) as a drug; alum is cold in nature, sour and astringent in taste, and has strong astringent effect. The traditional Chinese medicine considers that the alum has the effects of detoxifying, killing parasites, eliminating dampness, relieving itching, stopping bleeding, relieving diarrhea, clearing heat and eliminating phlegm. Recent studies have confirmed that alum also has the effect of repairing pathogens by antigen repair in immune organization. 5. Other effects of potassium aluminum sulfate (alum); the alum can also be used for preparing aluminum salt, paint, tanning material, mordant and the like, and can be applied to the bending prevention of the copper pipe of the primary coil of the intermediate frequency transformer.
Compared with the prior art, the method for rapidly preparing the aluminum potassium sulfate by using the vermiculite has the following substantial characteristics:
1) the method for rapidly preparing the aluminum potassium sulfate by using the vermiculite in Yue county in Xinjiang as the raw material is realized for the first time;
2) compared with the traditional aluminum hydroxide method, bauxite ore method and recrystallization purification method, the method has the advantages of simple process, low energy consumption and high speed.
Drawings
FIG. 1 is an X-ray diffraction pattern of the present invention;
FIG. 2 is an X-ray energy spectrum of the present invention;
FIG. 3 is a scanning electron micrograph of the inventive material.
The specific implementation mode is as follows:
example 1
a. Cleaning vermiculite, drying, crushing to 300 meshes, and weighing 500g of vermiculite powder for later use;
b. measuring 430mL of 98% concentrated sulfuric acid, slowly adding the concentrated sulfuric acid into 1570mL of stirred deionized water, and continuously stirring for 10 min;
c. slowly adding 500g of the vermiculite powder obtained in the step a into 2000mL of sulfuric acid aqueous solution obtained in the step b, transferring into a 5000mL three-neck flask, and heating and stirring at the temperature of 60 ℃ for 6h to obtain a mixture;
d. c, filtering the mixture obtained in the step c, washing the mixture with deionized water to be neutral, and taking the filtrate as an aluminum potassium sulfate crystal growth culture solution;
e. transferring the culture solution obtained in the step d into an open glass vessel, adding 200mL of absolute ethyl alcohol, mixing, wherein the volume ratio of the absolute ethyl alcohol to the culture solution is 1:10, quickly generating small white grains, and obtaining the required grains along with the standing time;
f. and e, naturally airing the crystal grains obtained in the step e to obtain the aluminum potassium sulfate dodecahydrate product.
Example 2
a. Cleaning vermiculite, drying, crushing to 300 meshes, and weighing 500g of vermiculite powder for later use;
b. measuring 430mL of 98% concentrated sulfuric acid, slowly adding the concentrated sulfuric acid into 1570mL of stirred deionized water, and continuously stirring for 10 min; completely transferring the prepared 2000mL of sulfuric acid aqueous solution into a 5000mL three-neck flask;
c. slowly adding 500g of the vermiculite powder obtained in the step a into 2000mL of sulfuric acid aqueous solution obtained in the step b, transferring into a 5000mL three-neck flask, and heating and stirring at the temperature of 80 ℃ for 3h to obtain a mixture;
d. c, filtering the mixture obtained in the step c, washing the mixture with deionized water to be neutral, and taking the filtrate as an aluminum potassium sulfate crystal growth culture solution;
e. transferring the culture solution obtained in the step d into an open glass vessel, adding 200mL of absolute ethyl alcohol, mixing, wherein the volume ratio of the absolute ethyl alcohol to the culture solution is 1:10, quickly generating small white grains, and obtaining the required grains along with the standing time;
f. and e, naturally airing the crystal grains obtained in the step e to obtain the aluminum potassium sulfate dodecahydrate product.
Example 3
a. Cleaning vermiculite, drying, crushing to 300 meshes, and weighing 500g of vermiculite powder for later use;
b. measuring 430mL of 98% concentrated sulfuric acid, slowly adding the concentrated sulfuric acid into 1570mL of stirred deionized water, and continuously stirring for 10 min;
c. slowly adding 500g of the vermiculite powder obtained in the step a into 2000mL of sulfuric acid aqueous solution obtained in the step b, transferring the mixture into a 5000mL three-neck flask, and heating and stirring the mixture for 2 hours at the temperature of 100 ℃ to obtain a mixture;
d. c, filtering the mixture obtained in the step c, washing the mixture with deionized water to be neutral, and taking the filtrate as an aluminum potassium sulfate crystal growth culture solution;
e. transferring the culture solution obtained in the step d into an open glass vessel, adding 200mL of absolute ethyl alcohol, mixing, wherein the volume ratio of the absolute ethyl alcohol to the culture solution is 1:10, quickly generating small white grains, and obtaining the required grains along with the standing time;
f. and e, naturally airing the crystal grains obtained in the step e to obtain the aluminum potassium sulfate dodecahydrate product.
Example 4
a. Cleaning vermiculite, drying, crushing to 300 meshes, and weighing 500g of vermiculite powder for later use;
b. measuring 430mL of 98% concentrated sulfuric acid, slowly adding the concentrated sulfuric acid into 1570mL of stirred deionized water, and continuously stirring for 10 min;
c. slowly adding 500g of the vermiculite powder obtained in the step a into 2000mL of sulfuric acid aqueous solution obtained in the step b, transferring into a 5000mL three-neck flask, and heating and stirring at the temperature of 80 ℃ for 3h to obtain a mixture;
d. c, filtering the mixture obtained in the step c, washing the mixture with deionized water to be neutral, and taking the filtrate as an aluminum potassium sulfate crystal growth culture solution;
e. transferring the culture solution obtained in the step d into an open glass vessel, adding 400mL of absolute ethyl alcohol, mixing, wherein the volume ratio of the absolute ethyl alcohol to the culture solution is 1:5, quickly generating small white grains, and obtaining the required grains along with the standing time;
f. and e, naturally airing the crystal grains obtained in the step e to obtain the aluminum potassium sulfate dodecahydrate product.
Example 5
a. Cleaning vermiculite, drying, crushing to 300 meshes, and weighing 500g of vermiculite powder for later use;
b. measuring 430mL of 98% concentrated sulfuric acid, slowly adding the concentrated sulfuric acid into 1570mL of stirred deionized water, and continuously stirring for 10 min;
c. slowly adding 500g of the vermiculite powder obtained in the step a into 2000mL of sulfuric acid aqueous solution obtained in the step b, transferring into a 5000mL three-neck flask, and heating and stirring at the temperature of 80 ℃ for 3h to obtain a mixture;
d. c, filtering the mixture obtained in the step c, washing the mixture with deionized water to be neutral, and taking the filtrate as an aluminum potassium sulfate crystal growth culture solution;
e. transferring the culture solution obtained in the step d into an open glass vessel, adding 1000mL of absolute ethyl alcohol, mixing, wherein the volume ratio of the absolute ethyl alcohol to the culture solution is 1:2, quickly generating a plurality of small white grains, and obtaining the required grains along with the standing time;
f. and e, naturally airing the crystal grains obtained in the step e to obtain the aluminum potassium sulfate dodecahydrate product.
Example 6
a. Cleaning vermiculite, drying, crushing to 300 meshes, and weighing 500g of vermiculite powder for later use;
b. measuring 430mL of 98% concentrated sulfuric acid, slowly adding the concentrated sulfuric acid into 1570mL of stirred deionized water, and continuously stirring for 10 min;
c. slowly adding 500g of the vermiculite powder obtained in the step a into 2000mL of sulfuric acid aqueous solution obtained in the step b, transferring the mixture into a 5000mL three-neck flask, and heating and stirring the mixture for 4 hours at the temperature of 70 ℃ to obtain a mixture;
d. c, filtering the mixture obtained in the step c, washing the mixture with deionized water to be neutral, and taking the filtrate as an aluminum potassium sulfate crystal growth culture solution;
e. transferring the culture solution obtained in the step d into an open glass vessel, adding 2000mL of absolute ethyl alcohol, mixing, wherein the volume ratio of the absolute ethyl alcohol to the culture solution is 1:1, quickly generating a white crystal, and obtaining the required crystal grains along with the standing time;
f. and e, naturally airing the crystal grains obtained in the step e to obtain the aluminum potassium sulfate dodecahydrate product.
Example 7
Any one of the potassium aluminum sulfate dodecahydrate obtained in the embodiments 1 to 6 is selected and tested by an X-ray diffractometer (XRD) and an X-ray energy spectrometer (EDS), so that the potassium aluminum sulfate material is shown in figure 3.
Claims (2)
1. A method for rapidly preparing aluminum potassium sulfate by utilizing vermiculite is characterized by comprising the following steps:
a. cleaning vermiculite, drying, and crushing to 300 meshes to obtain vermiculite powder for later use;
b. slowly adding concentrated sulfuric acid with the concentration of 98% into the stirred deionized water, and continuously stirring for 10 min;
c. slowly adding the vermiculite powder obtained in the step a into the sulfuric acid aqueous solution obtained in the step b according to the proportion that 4mL of sulfuric acid aqueous solution is added into every 1 g of vermiculite, and heating and stirring for 2-6 h at the temperature of 60-100 ℃ to obtain a mixture;
d. c, filtering the mixture in the step c, washing the mixture to be neutral by using deionized water, and taking the filtrate as an aluminum potassium sulfate crystal growth culture solution;
e. transferring the culture solution obtained in the step d into an open glass vessel, adding absolute ethyl alcohol, mixing to quickly generate small white grains, and obtaining the grains along with the standing time, wherein the volume ratio of the absolute ethyl alcohol to the culture solution is 1:1-1: 50;
f. and e, naturally airing the crystal grains obtained in the step e to obtain the aluminum potassium sulfate dodecahydrate product.
2. The method for rapidly preparing the potassium aluminum sulfate by using the vermiculite according to claim 1, wherein the volume ratio of the absolute ethyl alcohol to the culture solution in the step e is 1: 10.
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| CN102180502B (en) * | 2011-03-27 | 2012-07-25 | 江西本源新材料科技有限公司 | Method for extracting alum from lepidolite raw material |
| CN104386720B (en) * | 2014-10-30 | 2016-03-30 | 北京矿冶研究总院 | Method for acid-alkali combined extraction of alumina from high-silicon aluminum-containing mineral raw material |
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