CN108975412A - A method of iron compound is prepared from raw ore vermiculite - Google Patents
A method of iron compound is prepared from raw ore vermiculite Download PDFInfo
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- CN108975412A CN108975412A CN201810850474.3A CN201810850474A CN108975412A CN 108975412 A CN108975412 A CN 108975412A CN 201810850474 A CN201810850474 A CN 201810850474A CN 108975412 A CN108975412 A CN 108975412A
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- vermiculite
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- flotation
- iron
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- 235000019354 vermiculite Nutrition 0.000 title claims abstract description 67
- 229910052902 vermiculite Inorganic materials 0.000 title claims abstract description 66
- 239000010455 vermiculite Substances 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 32
- 150000002506 iron compounds Chemical class 0.000 title claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000002253 acid Substances 0.000 claims abstract description 34
- 238000005188 flotation Methods 0.000 claims abstract description 33
- 239000000047 product Substances 0.000 claims abstract description 25
- 230000005291 magnetic effect Effects 0.000 claims abstract description 24
- 238000004090 dissolution Methods 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 229910052742 iron Inorganic materials 0.000 claims abstract description 20
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 18
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 claims abstract description 16
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 229960004887 ferric hydroxide Drugs 0.000 claims abstract description 12
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000002244 precipitate Substances 0.000 claims abstract description 12
- 238000002604 ultrasonography Methods 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 11
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 8
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 8
- 230000005389 magnetism Effects 0.000 claims abstract description 7
- 238000010298 pulverizing process Methods 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 238000000108 ultra-filtration Methods 0.000 claims description 9
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 230000001476 alcoholic effect Effects 0.000 claims description 4
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000001632 sodium acetate Substances 0.000 claims description 4
- 235000017281 sodium acetate Nutrition 0.000 claims description 4
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 3
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229940056319 ferrosoferric oxide Drugs 0.000 claims 1
- 238000012545 processing Methods 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 abstract description 2
- 235000014413 iron hydroxide Nutrition 0.000 abstract 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 25
- 238000002360 preparation method Methods 0.000 description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- 238000000703 high-speed centrifugation Methods 0.000 description 2
- -1 iron ion Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- XBKMYUZPSUAVAK-KHPLUVTOSA-N 1-[(3r,5r,6s,8r,9s,10r,13s,14s,17r)-3,6,17-trihydroxy-10,13-dimethyl-1,2,3,4,5,6,7,8,9,11,12,14,15,16-tetradecahydrocyclopenta[a]phenanthren-17-yl]ethanone Chemical compound C([C@H]1[C@@H](O)C2)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@@](C(=O)C)(O)[C@@]2(C)CC1 XBKMYUZPSUAVAK-KHPLUVTOSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002892 organic cations Chemical class 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 229910052615 phyllosilicate Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a kind of method for preparing iron compound from raw ore vermiculite, this method comprises: a, raw ore vermiculite carried out microwave ultrasound expansion process；B, gained expanded vermiculite is subjected to Ultrasonic Pulverization magnetism and washes flotation；C, it is separated by solid-liquid separation after gained flotation vermiculite being carried out acid dissolution, obtains acidolysis solution；D, gained acidolysis solution is subjected to alkali precipitation reaction, obtains ferric hydroxide precipitate；E, gained ferric hydroxide precipitate is washed, dried and is roasted；F, it is separated by solid-liquid separation after gained di-iron trioxide product being carried out acid dissolution, gained liquid is dried, and obtains ferric trichloride product；G, gained ferric trichloride product is subjected to high temperature and pressure synthesis, obtains magnetic ferroferric oxide microballoon.The method of the present invention can obtain magnetic ferroferric oxide microballoon, and iron tramp in raw ore vermiculite is recycled.The present invention is through the separation and processing to vermiculite impurities, the products such as available iron hydroxide, iron chloride and magnetic ferroferric oxide.
Description
Technical field
The present invention relates to vermiculite technical fields, and in particular to a method of iron compound is prepared from raw ore vermiculite.
Background technique
Vermiculite is one of the nonmetallic minerals that there are preferable resource perspective and potential advantages in China, is a kind of important nonmetallic
The secondary metamorphic mineral of water aluminosilicate containing magnesium of mineral and a kind of layer structure belongs to phyllosilicate, cheap and easy to get.Leech
Stone energy high temperature resistant is the non-conductor of heat, has good electrical insulating property；Expanded vermiculite is easy to water imbibition and hygroscopicity；High temperature
Lower expansion, is easily peeled off.Vermiculite have preferable interlayer cation exchange capacity, swelliong power, adsorption capacity, sound-proofing, every
The features such as hot, fire resistance, freexing tolerance, and chemical property is stablized, it is not soluble in water, it is nontoxic, tasteless, it is without side-effects, industrially
Waste water, preparation mainly using its good absorption property and ion-exchange performance processing containing heavy metal and organic cation is anti-
Bacterium material and thermal insulation material, vermiculite filter aid, cleanser and Organized Vermiculite etc..
Vermiculite is a kind of stratified material, and the key of industrial application is first expanded before, obtains stratified material.It is real
On border, since vermiculite contains ferro element, make the vermiculite Composite of preparation that all there is the color of compound of iron, it is rubescent, seriously
Hinder the practical application of vermiculite material.Therefore, how effectively to deviate from ferro element in vermiculite is the key that expand vermiculite application to ask
Topic.Therefore, the research for carrying out vermiculite separation ferro element has important practical significance.
Summary of the invention
The purpose of the present invention is to provide a kind of methods that iron compound is prepared from raw ore vermiculite, and the method for the present invention can
Magnetic ferroferric oxide microballoon is obtained, iron tramp in raw ore vermiculite is recycled.
To achieve the above object, the present invention provides a kind of method that iron compound is prepared from raw ore vermiculite, this method packet
It includes:
A, raw ore vermiculite is subjected to microwave ultrasound expansion process, obtains expanded vermiculite；
B, gained expanded vermiculite is subjected to Ultrasonic Pulverization, magnetic washing flotation, obtains iron particle and flotation vermiculite；
C, it is separated by solid-liquid separation after gained flotation vermiculite being carried out the first acid dissolution, obtains acidolysis solution；
D, gained acidolysis solution is subjected to alkali precipitation reaction, obtains ferric hydroxide precipitate；
E, gained ferric hydroxide precipitate is washed, dried and is roasted, obtain di-iron trioxide product；
F, it is separated by solid-liquid separation after gained di-iron trioxide product being carried out the second acid dissolution with hydrochloric acid solution, gained liquid
It is dried, obtains ferric trichloride product；
G, gained ferric trichloride product is dispersed in progress high temperature and pressure synthesis in organic alcoholic solution of anhydrous sodium acetate, obtained
To magnetic ferroferric oxide microballoon.
Optionally, the condition of microwave ultrasound expansion process described in step a is 10-20000 hertz, microwave power 100-
5000W, time are 0.01-10 hours.
Optionally, the washing of magnetism described in step b flotation carries out under stiring, and speed of agitator 600-5500Rpm is magnetic
Washing flotation power is 0.5-1 tesla.
Optionally, in step c, the flotation vermiculite is crushed to after 90-350 mesh and carries out first acid dissolution again, the
Acid used by one acid dissolution is at least one of nitric acid, phosphoric acid, acetic acid and hydrogen peroxide, and the mass concentration of acid solution is
0.01-35%, reaction temperature are 80-98 DEG C, and the reaction time is 0.1-20 hours, and the mass ratio of acid solution and flotation vermiculite is 1:
(0.1-100), the method for separation of solid and liquid are centrifugation, revolving speed 15000-100000Rpm.
Optionally, the condition of the reaction of alkali precipitation described in step d are as follows: lye is ammonium hydroxide and/or potassium hydroxide solution, alkali soluble
Liquid concentration is 0.01-5mol/L, and reaction temperature is 50-99 DEG C, and the time is 0.1-32 hours, pH value 2.5-3.5.
Optionally, washing times are 5-10 times in step e, and drying temperature is 30-120 DEG C, and the time is 1-50 hours, roasting
Temperature is 300-850 DEG C, and the time is 1-50 hours.
Optionally, in step f, hydrochloric acid solution mass concentration is 0.1-36%, hydrochloric acid solution and di-iron trioxide product
Weight ratio is (0.1-100): 1, described be separated by solid-liquid separation is ultra-filtration filters, and ultrafiltration membrane aperture is 0.01-100 microns, and vacuum degree is
0.01-0.20MPa。
Optionally, in step g, the Organic Alcohol is in ethylene glycol, vinyl alcohol, glycerine, polyethylene glycol and poly- triol
One or more, the mass ratio of sodium acetate, ferric trichloride and Organic Alcohol is 1:(5-20): (1-1000), high temperature and pressure synthesis temperature
Degree is 100-280 DEG C, and generated time is 0.5-30 hours.
The present invention has the advantage that
The present invention by raw ore vermiculite by microwave ultrasound expansion, magnetic washing flotation, acid dissolution, alkali precipitation, acid dissolution and
High-temperature laminating is at obtaining magnetic ferroferric oxide microballoon and iron particle, iron tramp in raw ore vermiculite is recycled.
In addition, the present invention has, separation method is simple and effective, separation is quick, and energy loss is low, is easily isolated, equipment letter
Single, production efficiency improves, pollutant is few, has apparent economic value.
Detailed description of the invention
Fig. 1 is the electron microscope of the magnetic ferroferric oxide microballoon of preparation of the embodiment of the present invention.
Fig. 2 is the photo for the raw ore vermiculite that the embodiment of the present invention uses.
Fig. 3 is the photo of the expanded vermiculite of preparation of the embodiment of the present invention.
Fig. 4 is the photo of the flotation vermiculite of preparation of the embodiment of the present invention.
Fig. 5 is the photo of the acidolysis solution of preparation of the embodiment of the present invention.
Fig. 6 is the photo of the ferric hydroxide precipitate of preparation of the embodiment of the present invention.
Fig. 7 is the photo of the ferric trichloride product of preparation of the embodiment of the present invention.
Fig. 8 is the photo of the magnetic ferroferric oxide microballoon of preparation of the embodiment of the present invention.
Fig. 9 is the first acid dissolution temperature and iron ion extracted amount in step of embodiment of the present invention c (in terms of di-iron trioxide)
Relational graph.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
The present invention provides a kind of method that iron compound is prepared from raw ore vermiculite, this method comprises: a, by raw ore vermiculite
Microwave ultrasound expansion process is carried out, expanded vermiculite is obtained；B, gained expanded vermiculite is subjected to Ultrasonic Pulverization, magnetic washing flotation,
Obtain iron particle and flotation vermiculite；C, it is separated by solid-liquid separation after gained flotation vermiculite being carried out the first acid dissolution, it is molten to obtain acidolysis
Liquid；D, gained acidolysis solution is subjected to alkali precipitation reaction, obtains ferric hydroxide precipitate；E, gained ferric hydroxide precipitate is subjected to water
It washes, dry and roasts, obtain di-iron trioxide product；F, gained di-iron trioxide product and the second acid of hydrochloric acid solution progress is molten
It is separated by solid-liquid separation after solution, gained liquid is dried, and obtains ferric trichloride product；G, gained ferric trichloride product is dispersed in
High temperature and pressure synthesis is carried out in organic alcoholic solution of anhydrous sodium acetate, obtains magnetic ferroferric oxide microballoon.The present invention is by raw ore
Vermiculite is expanded by microwave ultrasound, magnetic flotation, acid dissolution, alkali precipitation, acid dissolution and the high temperature and pressure of washing synthesizes, and obtains iron
Grain and magnetic ferroferric oxide microballoon, iron tramp in raw ore vermiculite is recycled.
In the present invention, microwave ultrasound expansion process facilitates iron particle therein de- for expanding raw ore vermiculite
It falls, for example, the condition of microwave ultrasound expansion process described in step a is 10-20000 hertz, microwave power 100-5000W, when
Between be 0.01-10 hours.Those skilled in the art can also be carried out at the microwave ultrasound expansion using other suitable conditions
Reason.
In the present invention, magnetism washing flotation is reduced using density after expanding vermiculite, can be bubbled through the water column, and iron particle can
The characteristics of being adsorbed by magnet, quick separating iron particle and vermiculite, it is preferable that magnetism described in step b washes flotation under stiring
It carries out, speed of agitator can be 600-5500Rpm, and magnetism washing flotation power can be 0.5-1 tesla.
In the present invention, the iron particle not removed in granular form for convenience is separated from flotation vermiculite, by flotation vermiculite
The first acid dissolution is carried out, in order to improve the efficiency of acid dissolution, in step c, the flotation vermiculite can be crushed to 90-350 mesh
Carry out first acid dissolution again afterwards, acid used by the first acid dissolution can be in nitric acid, phosphoric acid, acetic acid and hydrogen peroxide
At least one, the mass concentration of acid solution can be 0.01-35%, and reaction temperature can be 80-98 DEG C, and the reaction time can be
0.1-20 hours, acid solution and the mass ratio of flotation vermiculite can be 1:(0.1-100), the method for separation of solid and liquid can be centrifugation,
Revolving speed can be 15000-100000Rpm.
In the present invention, in order to be precipitated out the ferro element for being dissolved in acid solution, it is added lye in acidolysis solution, in step d
The condition of alkali precipitation reaction can be with are as follows: lye is ammonium hydroxide and/or potassium hydroxide solution, alkaline concentration 0.01-5mol/
L, reaction temperature are 50-99 DEG C, and the time is 0.1-32 hours, pH value 2.5-3.5.
In the present invention, washed in order to remove the alkali composition in ferric hydroxide precipitate and obtain di-iron trioxide, in step e secondary
Number can be 5-10 times, and drying temperature can be 30-120 DEG C, and dry mode can be vacuum drying, and the time can be 1-50
Hour, maturing temperature can be 300-850 DEG C, and the time can be 1-50 hours.
In the present invention, in order to obtain ferric trichloride further to purify iron compound, in step f, hydrochloric acid solution quality is dense
Degree can be 0.1-36%, and the weight ratio of hydrochloric acid solution and di-iron trioxide product can be (0.1-100): 1, the solid-liquid point
From that can be ultra-filtration filters, ultrafiltration membrane aperture can be 0.01-100 microns, and vacuum degree can be 0.01-0.20MPa, in ultrafiltration
It can carry out high speed centrifugation in advance before.
In the present invention, in order to obtain the magnetic ferroferric oxide microballoon of high-purity, in step g, the Organic Alcohol is can be with
One of ethylene glycol, vinyl alcohol, glycerine, polyethylene glycol and poly- triol are a variety of, sodium acetate, ferric trichloride and Organic Alcohol
Mass ratio can be 1:(5-20): (1-1000), high temperature and pressure synthesis temperature are 100-280 DEG C, and generated time is that 0.5-30 is small
When, the product of high temperature and pressure synthesis can be washed and be dried, and magnetic ferroferric oxide microballoon is obtained.
The present invention is further illustrated below by embodiment, but the present invention is not therefore subject to any restriction.
Embodiment
A, by raw ore vermiculite (iron containing di-iron trioxide is 5.8 mass %, and photo is as shown in Figure 2), in microwave power
900W carries out expansion 5 minutes, obtains expanded vermiculite under 500 hertz ultrasonic (photo is as shown in Figure 3).
B, gained expanded vermiculite is placed under stiring in container and the magnetic washing flotation of ultrasound, control is carried out using electromagnet
Mixing speed processed is 300Rpm, and flotation power is 0.5 tesla, iron particle and flotation vermiculite (photo such as Fig. 4 after being separated
It is shown).
C, gained flotation vermiculite is filtered out, the hydrogen peroxide that 30 mass % then are added according to mass ratio 1:10 is molten
Liquid controls pH value 3, carries out the first acid dissolution, and the reaction time is 1.5 hours, and reaction temperature is 85 DEG C (as shown in figure 9, if temperature
Lower than 85 DEG C, then extraction efficiency reduces, and ordinate is the extracted iron ion quality (in terms of di-iron trioxide) of 13 grams of vermiculites, warp
It is centrifuged 5 minutes under 15000Rpm, obtains acidolysis solution (photo is as shown in Figure 5).The step is molten according to the first acid of phosphoric acid progress
Solution extracts iron, then extraction rate is accelerated, and the phosphoric acid solution of 5 mass % reaches identical extracted amount and only needs 0.4 hour.
D, the potassium hydroxide lye of 0.1mol/L will be added in gained acidolysis solution, reaction 2.5 is then carried out at 90 DEG C
Hour, obtain ferric hydroxide precipitate (photo is as shown in Figure 6).
E, vacuum drying 8 hours is carried out at 75 DEG C after gained ferric hydroxide precipitate being carried out washing 5 times, then 450
It carries out roasting 2 hours at DEG C, obtains di-iron trioxide product (photo is as shown in Figure 7).
F, the second acid is carried out after mixing gained di-iron trioxide according to weight ratio 1:10 with the acid salt solution of 36 mass %
Then dissolution carries out high speed centrifugation and ultra-filtration filters, ultrafiltration membrane aperture is 0.02 micron, then vacuum degree 0.25MPa will surpass
Filter acquired solution is concentrated and dried, and ferric trichloride product is obtained.
G, gained ferric trichloride product is dispersed according to the mass ratio of sodium acetate, ferric trichloride and Organic Alcohol for 1:9:30
High temperature and pressure is carried out in the ethylene glycol alcoholic solution of anhydrous sodium acetate at 200 DEG C to synthesize 8 hours, it is micro- to obtain magnetic ferroferric oxide
Ball (photo is as shown in Figure 8).
Through detecting, iron content is 99.2 mass % in magnetic ferroferric oxide microballoon, and magnetic ferroferric oxide microballoon has
Paramagnetic properties, electron microscope are shown in Fig. 1.From this experiment as can be seen that through the separation and processing to vermiculite impurities, available hydrogen
The products such as iron oxide, iron chloride and magnetic ferroferric oxide.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.
Claims (8)
1. a kind of method for preparing iron compound from raw ore vermiculite, which is characterized in that this method comprises:
A, raw ore vermiculite is subjected to microwave ultrasound expansion process, obtains expanded vermiculite；
B, gained expanded vermiculite is subjected to Ultrasonic Pulverization, magnetic washing flotation, obtains iron particle and flotation vermiculite；
C, it is separated by solid-liquid separation after gained flotation vermiculite being carried out the first acid dissolution, obtains acidolysis solution；
D, gained acidolysis solution is subjected to alkali precipitation reaction, obtains ferric hydroxide precipitate；
E, gained ferric hydroxide precipitate is washed, dried and is roasted, obtain di-iron trioxide product；
F, it is separated by solid-liquid separation after gained di-iron trioxide product being carried out the second acid dissolution with hydrochloric acid solution, gained liquid carries out
It is dry, obtain ferric trichloride product；
G, gained ferric trichloride product is dispersed in progress high temperature and pressure synthesis in organic alcoholic solution of anhydrous sodium acetate, obtains magnetic
Property ferroso-ferric oxide microballoon.
2. the method according to claim 1, wherein the condition of microwave ultrasound expansion process described in step a is
10-20000 hertz, microwave power 100-5000W, the time is 0.01-10 hours.
3. it is carried out under stiring the method according to claim 1, wherein magnetism described in step b washes flotation,
Speed of agitator is 600-5500Rpm, and magnetism washing flotation power is 0.5-1 tesla.
4. the method according to claim 1, wherein the flotation vermiculite is crushed to 90-350 mesh in step c
Carry out first acid dissolution, the used phosphoric acid of the first acid dissolution again afterwards, the mass concentration of acid solution is 0.01-35%, reaction temperature
Degree is 80-98 DEG C, and the reaction time is 0.1-20 hours, and the mass ratio of acid solution and flotation vermiculite is 1:(0.1-100), it is separated by solid-liquid separation
Method be centrifugation, revolving speed 15000-100000Rpm.
5. the method according to claim 1, wherein the condition of the reaction of alkali precipitation described in step d are as follows: lye is
Ammonium hydroxide and/or potassium hydroxide solution, alkaline concentration 0.01-5mol/L, reaction temperature are 50-99 DEG C, time 0.1-32
Hour, pH value 2.5-3.5.
6. drying temperature is the method according to claim 1, wherein washing times are 5-10 times in step e
30-120 DEG C, the time is 1-50 hours, and maturing temperature is 300-850 DEG C, and the time is 1-50 hours.
7. hydrochloric acid solution mass concentration is 0.1-36% the method according to claim 1, wherein in step f,
The weight ratio of hydrochloric acid solution and di-iron trioxide product is (0.1-100): 1, described be separated by solid-liquid separation is ultra-filtration filters, ultrafiltration fenestra
Diameter is 0.01-100 microns, vacuum degree 0.01-0.20MPa.
8. the method according to claim 1, wherein the Organic Alcohol is ethylene glycol, vinyl alcohol, third in step g
One of triol, polyethylene glycol and poly- triol are a variety of, and the mass ratio of sodium acetate, ferric trichloride and Organic Alcohol is 1:(5-
20): (1-1000), high temperature and pressure synthesis temperature are 100-280 DEG C, and generated time is 0.5-30 hours.
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| CN111573686A (en) * | 2020-05-19 | 2020-08-25 | 陕西科技大学 | Preparation method of vermiculite ultrafine powder |
| CN113603150A (en) * | 2021-09-23 | 2021-11-05 | 广州大学 | Iron oxide red and preparation method thereof |
| CN115487816A (en) * | 2022-08-16 | 2022-12-20 | 中国地质大学（武汉） | Vermiculite-based iron molybdate nano enzyme and preparation method and application thereof |
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| CN115487816A (en) * | 2022-08-16 | 2022-12-20 | 中国地质大学（武汉） | Vermiculite-based iron molybdate nano enzyme and preparation method and application thereof |
| CN115487816B (en) * | 2022-08-16 | 2023-08-04 | 中国地质大学（武汉） | Vermiculite-based ferric molybdate nano enzyme and preparation method and application thereof |
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