CN103803662B - A kind of method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate - Google Patents

A kind of method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate Download PDF

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CN103803662B
CN103803662B CN201310703446.6A CN201310703446A CN103803662B CN 103803662 B CN103803662 B CN 103803662B CN 201310703446 A CN201310703446 A CN 201310703446A CN 103803662 B CN103803662 B CN 103803662B
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bauxite
sulfuric acid
roasting
acid
add
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CN103803662A (en
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吴烈善
伍敏莉
苏翠翠
吴蒙
莫小荣
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Guangxi University
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Guangxi University
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Abstract

The invention provides a kind of method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate, it comprises after the roasting of oxidation bauxite, adding sulfuric acid carries out acid-soluble, add stablizer, small amounts agent and basifier to be hydrolyzed, post curing 36-48h after obtained faint yellow sticky solid phase prod, the temperature of wherein said roasting is gradient increased temperature; Described sulfuric acid adopts the mode of jet flow successively to add; Described acid-soluble, hydrolysis and slaking all carry out under 2-5atm pressure.The method of the invention adopts that raw material is single is easy to get, and with low cost, preparation technology is simple to operation, is convenient to carry out suitability for industrialized production, and the obtained finished product of single stage method is directly solid-state, facilitates transport and the preservation of product, is beneficial to and applies.

Description

A kind of method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate
Technical field
The present invention relates to the preparation method of PAFS, relate more specifically to a kind of method utilizing oxidation bauxite directly to prepare solid polymeric aluminum ferric sulfate.
Background technology
PAFS conventional preparation techniques many employings technical grade green vitriol or iron content, aluminium various materials are combined as raw material, high to ingredient requirement, and processing condition require comparatively strict, next is that finished product great majority are for liquid, the shortcoming of not easily preserving transport is very outstanding, minority solid-state polymerization aluminium iron sulfate is also dry rear obtained under given conditions by liquid polymerization aluminium iron sulfate, this considerably increases the complexity of solid-state polymerization aluminium iron sulfate preparation technology.As aluminum ore, the content of the low aluminum oxidation bauxite aluminium of high ferro is lower than 40%, and grade is lower, does not reach the requirement of aluminum current industrial processes, therefore, and at present also cannot extensive industrial utilization.
Summary of the invention
For the problems referred to above, the object of the invention is to utilize the feature being simultaneously rich in iron and aluminium component in ore, adopt the Technology of innovation and formula to achieve and directly prepare solid polymeric aluminum ferric sulfate production technique with solid material single stage method, this not only enormously simplify preparation process, decrease production cost, be convenient to transport and the preservation of product simultaneously.
The method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate of the present invention, it comprises after the roasting of oxidation bauxite, adding sulfuric acid carries out acid-soluble, add stablizer, small amounts agent and basifier to be hydrolyzed, post curing 36-48h after obtained faint yellow sticky solid phase prod, the temperature of wherein said roasting is gradient increased temperature; Described sulfuric acid adopts the mode of jet flow successively to add; Described acid-soluble, hydrolysis and slaking all carry out under 2-5atm pressure.React under certain pressure scope, be more conducive to accelerating reaction process.
Wherein, described roasting comprises: roasting 0.5-1h at 400 DEG C-500 DEG C; Roasting 1-2h at 700-800 DEG C afterwards.When 400 DEG C of < T≤500 DEG C, this one-phase is de-surface adsorption water, exsiccation, structure dehydration and internal mineral dehydration mainly, this process increases the porosity on bauxite ore particles surface, add the contact area of bauxite and sulfuric acid, there is a small amount of pyrrhosiderite (α-FeO (OH)) in raw ore simultaneously and be transformed into rhombohedral iron ore (α-Fe 2o 3), this is conducive to the stripping of iron in bauxite; When 700 DEG C of < T≤800 DEG C, AlO (OH) dehydration in diaspore is transformed into α-Al 2o 3, compare in diaspore, the form of the latter is more conducive to the stripping of aluminium in bauxite.
Wherein saidly acid-solublely to comprise: in liquid-solid ratio be 0.8: 1-1.6: 1 ratio the sulfuric acid of baked oxidation bauxite and 7-11mol/L is placed in temperature range is 80-120 DEG C, pressure range is 2-5atm reactor and fully stirs, wherein said sulfuric acid adopts jet flow gradation to add: the sulfuric acid first adding 10-11mol/L, and its atomizing particle size is 3000-5000 μm; Add the sulfuric acid of 8-9mol/L after stirring, its atomizing particle size is 2000-3000 μm; Add the sulfuric acid of 7-8mol/L after stirring again, its atomizing particle size is 1500-2000 μm.Described sulfuric acid adopts jet flow to add, and can accelerate reaction process, the atomizing particle size gradually reducing described sulfuric acid can increase level of response, makes it react more abundant.
The method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate of the present invention carries out pulverizing and crosses 100-200 mesh sieve before being also included in the roasting of described oxidation bauxite.
Preferably, described stablizer P/ [Fe+Al] is 0.08-0.1, is selected from the one in phosphoric acid, Sodium phosphate dibasic, dipotassium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC or potassium primary phosphate.
Preferably, described oxygenant is selected from the one in concentrated nitric acid, hydrogen peroxide, sodium chlorate or Potcrate.Find under study for action, carry out also having a small amount of ferrous iron in described acid-soluble described oxidation alum clay mineral solution afterwards, therefore add appropriate oxygenant and described second order iron can be converted into ferric iron, be conducive to the purity of the solid polymeric aluminum ferric sulfate improving described preparation.
Preferably, described basifier [OH]/[Fe+Al] is 0.8-1.6, is selected from the one in sodium hydroxide, calcium hydroxide, sodium bicarbonate or saleratus.
Preferably, the described acid-soluble time is 40-60min.
Preferably, described hydrolysis time is 30-40min.
In one of them embodiment of the present invention, the described method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate comprises the following steps:
Step one, will be oxidized after bauxite fragmentation crosses 100-200 mesh sieve;
In step 2, retort furnace at 400 DEG C of-500 DEG C of temperature, roasting is about 30-60min, then at 700 DEG C-800 DEG C roasting 1-2h;
Step 3, roasting is complete after oxidation bauxite put into that temperature is 80 DEG C-120 DEG C, pressure-controlling at the reactor of 2-5atm, jet flow adds the sulfuric acid of 10-11mol/L, and its atomizing particle size is 3000-5000 μm; Add the sulfuric acid of 8-9mol/L after stirring, its atomizing particle size is 2000-3000 μm; Add the sulfuric acid of 7-8mol/L after stirring again, its atomizing particle size is 1500-2000 μm; The acid-soluble 40-60min of abundant stirring post-heating;
Step 4, add the basifier that stablizer that P/ [Fe+Al] is 0.08-0.1, small amounts agent and [OH]/[Fe+Al] are 0.8-1.6 successively and stir hydrolytic polymerization 30-40min, stop heating taking out;
Step 5, slaking are about 36-48h and obtain faint yellow sticky solid product.
The method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate of the present invention, uses single raw material, does not need plurality of raw materials to participate in reaction, reduce the requirement to raw material and process complexity; Gradient increased temperature roasting is more conducive to the stripping of aluminium in bauxite.In acid dissolution, adopt jet flow to add sulfuric acid, control sulfuric acid and add fashionable atomizing particle size, accelerate reaction process, make acid dissolution level of response within the effective time more abundant.The method of the invention simplifies solid product preparation process condition, and the solid phase prod that single stage method obtains is convenient to preserve transport.Raw material is single to be easy to get, and with low cost, preparation technology is simple to operation, is convenient to carry out suitability for industrialized production, and the finished product that single stage method obtains is directly solid-state, facilitates transport and the preservation of product, is beneficial to and applies.
Embodiment
The present invention is described in further detail below, can implement according to this with reference to specification sheets word to make those skilled in the art.
The method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate of the present invention comprises the following steps:
Step one, bauxite fragmentation will be oxidized cross 100-200 mesh sieve;
In step 2, retort furnace at 400 DEG C of-500 DEG C of temperature, roasting is about 30-60min, then at 700 DEG C-800 DEG C roasting 1-2h;
Step 3, roasting is complete after oxidation bauxite put into that temperature is 80 DEG C-120 DEG C, pressure-controlling at the reactor of 2-5atm, jet flow adds the sulfuric acid of 10-11mol/L, and its atomizing particle size is 3000-5000 μm; Add the sulfuric acid of 8-9mol/L after stirring, its atomizing particle size is 2000-3000 μm; Add the sulfuric acid of 7-8mol/L after stirring again, its atomizing particle size is 1500-2000 μm; The acid-soluble 40-60min of abundant stirring post-heating;
Step 4, successively add P/ [Fe+Al] be 0.1 stablizer, small amounts agent and [OH]/[Fe+Al] be 1.6 basifier stir hydrolytic polymerization 30-40min, stop heating taking out;
Step 5, slaking are about 36-48h and obtain faint yellow sticky solid product.
Embodiment 1
The method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate of the present invention comprises the following steps:
Step one, bauxite fragmentation will be oxidized cross after 200 mesh sieves;
In step 2, retort furnace at 500 DEG C of temperature, roasting is about 60min, then at 800 DEG C roasting ih;
Step 3, the oxidation bauxite after complete for 20g roasting put into temperature is 80 DEG C, pressure-controlling at the reactor of 5atm, according to the ratio of solid-to-liquid ratio 1.6: 1, jet flow adds the sulfuric acid of 11mol/L, and its atomizing particle size is 5000 μm; Add the sulfuric acid of 9mol/L after stirring, its atomizing particle size is 3000 μm; Add the sulfuric acid of 8mol/L after stirring again, its atomizing particle size is 2000 μm; The acid-soluble 60min of abundant stirring post-heating;
Step 4, successively add P/ [Fe+Al] be 0.08 stablizer such as phosphoric acid, small amounts agent such as hydrogen peroxide and [OH]/[Fe+Al] be 0.8 basifier such as sodium hydroxide stir hydrolytic polymerization 40min, stop heating taking out;
Step 5, slaking are about 36h and obtain faint yellow sticky solid product.
Embodiment 2
Step one, will be oxidized bauxite fragmentation cross 120 mesh sieves;
In step 2, retort furnace at 400 DEG C of temperature, roasting is about 30min, then roasting is about 1h at 800 DEG C,
Step 3, the oxidation bauxite after complete for 20g roasting put into temperature is 80 DEG C, pressure-controlling at the reactor of 3atm, the proportioning jet flow being 1.4: 1 by liquid-solid ratio adds the sulfuric acid of 10mol/L, and its atomizing particle size is 3000 μm; Add the sulfuric acid of 8mol/L after stirring, its atomizing particle size is 2000 μm; Add the sulfuric acid of 7mol/L after stirring again, its atomizing particle size is 1500 μm; The acid-soluble 60min of abundant stirring heating,
Step 4, successively add P/ [Fe+Al] be 0.1 stablizer such as phosphoric acid, small amounts agent such as hydrogen peroxide and [OH]/[Fe+Al] be 1.0 basifier such as sodium hydroxide stir hydrolytic polymerization 40min, stop heating taking out;
Step 5, slaking 36h obtain faint yellow sticky solid product.
Embodiment 3
The method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate of the present invention comprises the following steps:
Step one, bauxite fragmentation will be oxidized cross after 100 mesh sieves;
In step 2, retort furnace at 800 DEG C of temperature, roasting is about 60min;
Step 3, the oxidation bauxite after complete for 20g roasting put into temperature is 120 DEG C, pressure-controlling at the reactor of 2atm, add the sulfuric acid of 10mol/L according to the ratio jet flow of solid-to-liquid ratio 1.4: 1; The acid-soluble 40min of abundant stirring post-heating;
Step 4, successively add P/ [Fe+Al] be 0.09 stablizer, small amounts agent and [OH]/[Fe+Al] be 1.6 basifier stir hydrolytic polymerization 30min, stop heating taking out;
Step 5, slaking are about 40h and obtain faint yellow sticky solid product.
The product performance table of described solid polymeric aluminum ferric sulfate prepared by the method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate of the present invention is as follows:
As can be seen from table, described PAFS prepared by described embodiment 1-3 all meets the technical requirement scope of PAFS.But Fe described in the described solid polymeric aluminum ferric sulfate utilizing oxidation bauxite to prepare embodiment 1 and embodiment 2 preparation in the method for solid polymeric aluminum ferric sulfate of the present invention 2o 3content, Al 2o 3content, basicity and turbidity removal rate far away higher than the indices of the described solid polymeric aluminum ferric sulfate prepared by embodiment 3, will this shows, adopt gradient increased temperature effectively to improve Al described in described solid polymeric aluminum ferric sulfate during described roasting 2o 3content and basicity, in hydrolysis reaction, add small amounts agent can effectively improve described Fe 2o 3content, in described acid dissolution, successively jet flow adds sulfuric acid and makes it react more abundant, improves Al described in described solid polymeric aluminum ferric sulfate 2o 3and Fe 2o 3content and basicity, by table in can find out that described embodiment 1 and embodiment 2 prepare the turbidity removal rate of described PAFS all higher than PAFS prepared by described embodiment 3.
Although embodiment of the present invention are open as above, but it is not restricted to listed in specification sheets and embodiment utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the embodiment described.

Claims (3)

1. the method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate, it comprises after the roasting of oxidation bauxite, adding sulfuric acid carries out acid-soluble, add stablizer, small amounts agent and basifier to be hydrolyzed, post curing 36-48h after obtained faint yellow sticky solid phase prod, the temperature of wherein said roasting is gradient increased temperature; Described sulfuric acid adopts the mode of jet flow successively to add; Described acid-soluble, hydrolysis and slaking all carry out under 2-5atm pressure; Described roasting comprises: roasting 0.5-1h at 400 DEG C-500 DEG C; Roasting 1-2h at 700-800 DEG C afterwards; Describedly acid-solublely to comprise: be that the sulfuric acid of baked oxidation bauxite and 7-11mol/L is placed in temperature range is 80-120 DEG C, pressure range is 2-5atm reactor and fully stirs by the ratio of 0.8:1-1.6:1 in liquid-solid ratio, wherein said sulfuric acid adopts jet flow gradation to add: the sulfuric acid first adding 10-11mol/L, and its atomizing particle size is 3000-5000 μm; Add the sulfuric acid of 8-9mol/L after stirring, its atomizing particle size is 2000-3000 μm; Add the sulfuric acid of 7-8mol/L after stirring again, its atomizing particle size is 1500-2000 μm; Described stablizer P/ [Fe+Al] is 0.08-0.1, is selected from the one in phosphoric acid, Sodium phosphate dibasic, dipotassium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC or potassium primary phosphate; Described oxygenant is selected from the one in concentrated nitric acid, hydrogen peroxide, sodium chlorate or Potcrate; The described acid-soluble time is 40-60min; Described hydrolysis time is 30-40min.
2. the method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate as claimed in claim 1, is characterized in that, before it is also included in the roasting of described oxidation bauxite, carries out pulverizing and cross 100-200 mesh sieve.
3. the method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate as claimed in claim 1, it is characterized in that, described basifier [OH]/[Fe+Al] is 0.8-1.6, is selected from the one in sodium hydroxide, calcium hydroxide, sodium bicarbonate or saleratus.
CN201310703446.6A 2013-12-19 2013-12-19 A kind of method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate Expired - Fee Related CN103803662B (en)

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CN110040825A (en) * 2019-04-03 2019-07-23 广西大学 The method that " one-step method " prepares solid rare earth lanthanum improved PFS

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CN104803460B (en) * 2015-03-26 2018-07-06 徐颖惠 The method that sour self coupling balances quasi- dry process polymeric aluminum sulfate iron
CN104724804B (en) * 2015-03-26 2018-07-06 徐颖惠 The method that sour self coupling balancing method prepares polymeric aluminum sulfate iron
CN104961217A (en) * 2015-06-26 2015-10-07 开平市开物化工建材有限公司 Preparing and solidifying device for polymeric aluminum ferric sulfate
CN104961214A (en) * 2015-06-26 2015-10-07 开平市开物化工建材有限公司 Preparing device for polymeric aluminum ferric sulfate

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN110040825A (en) * 2019-04-03 2019-07-23 广西大学 The method that " one-step method " prepares solid rare earth lanthanum improved PFS
CN110040825B (en) * 2019-04-03 2021-08-17 广西大学 Method for preparing solid rare earth lanthanum modified polymeric ferric sulfate by one-step method

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