CN104071817A - Method for coproducing aluminium sulfate, white carbon black and ammonium fluoride - Google Patents
Method for coproducing aluminium sulfate, white carbon black and ammonium fluoride Download PDFInfo
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- CN104071817A CN104071817A CN201410336895.6A CN201410336895A CN104071817A CN 104071817 A CN104071817 A CN 104071817A CN 201410336895 A CN201410336895 A CN 201410336895A CN 104071817 A CN104071817 A CN 104071817A
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- ammonium fluoride
- solution
- sulfuric acid
- carbon black
- white carbon
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Abstract
The invention discloses a method for coproducing aluminium sulfate, white carbon black and ammonium fluoride. The method is characterized in that monohydrallite, fluorite and sulfuric acid are used as raw materials and react in the same reactor at a certain temperature; aluminium oxide in the monohydrallite reacts with the sulfuric acid to generate aluminium sulfate and silicon dioxide, the fluorite reacts with the sulfuric acid to generate hydrogen fluoride and calcium sulfate, the hydrogen fluoride and the silicon dioxide react to generate silicon tetrafluoride, and the silicon tetrafluoride is absorbed by a ammonium hydrogen carbonate solution to generate the white carbon black and the ammonium fluoride. According to the invention, the method has the following effects: two original production technologies and two sets of production devices are combined, so that the production cost is lowered; the reaction is conducted at the normal pressure, so that the requirements for the production devices are lowered; the monohydrallite reacts with the sulfuric acid to release heat which supplies power for the reaction of the fluorite and the sulfuric acid, so that the energy is saved; the dumped silicon dioxide is fully used; a sinking agent doesn't need to be added, so that the post-processing is simple.
Description
Technical field
The present invention relates to a kind of method of co-producing sulfuric acid aluminium, white carbon black and Neutral ammonium fluoride.Be particularly related to a kind of method of utilizing bauxite, fluorite, producing sulfuric acid and jointly Tai-Ace S 150, white carbon black, Neutral ammonium fluoride.
Background technology
Tai-Ace S 150 white solid, molecular composition Al
2(SO
4)
316H
2o; White carbon black is water and silicon-dioxide, white powder, molecular composition SiO
2nH
2o, wherein nH
2o exists with the form of surface hydroxyl; Neutral ammonium fluoride white solid, molecular composition NH
4f.At present, industrial production Tai-Ace S 150 is taking bauxite and sulfuric acid as raw material, and under certain temperature and pressure, the aluminum oxide in bauxite and sulfuric acid reaction generate Tai-Ace S 150.After reaction, in alum liquor, add polyacrylamide sinking agent sedimentation residue (main component of residue is silicon-dioxide).After sedimentation, supernatant liquor is finite concentration alum liquor, is placed on that in vaporizer, heating evaporation is to finite concentration, and cooling, crystallization obtains solid sulphuric acid aluminium.Residue is discarded after washing, press filtration.Producing Neutral ammonium fluoride is that (main component is as CaF taking fluorite
2) and sulfuric acid be raw material production Neutral ammonium fluoride.First, fluorite and sulfuric acid reaction generate hydrogen fluoride.Then, hydrogen fluoride reacts with bicarbonate of ammonia and generates Neutral ammonium fluoride.
While producing Tai-Ace S 150, need certain pressure, equipment is had higher requirements; After reaction, remaining residue goes out of use, and silicon-dioxide wherein is not utilized effectively, not only contaminate environment but also cause the waste of resource.
Summary of the invention
The object of the present invention is to provide a kind of method of co-producing sulfuric acid aluminium, white carbon black and Neutral ammonium fluoride.The shortcoming existing in order to overcome above-mentioned industrial production Tai-Ace S 150, is fully used Mineral resources, adopts bauxite, fluorite, sulfuric acid under normal pressure, to use a set of device reaction, can produce Tai-Ace S 150, white carbon black, Neutral ammonium fluoride and calcium sulfate simultaneously.With the comparison of original production Tai-Ace S 150, have that technique is simple, reaction conditions is gentle, can also produce white carbon black.For achieving the above object, the present invention includes following technical scheme:
A, bauxite, fluorite, sulfuric acid raw material in mass ratio=0.9～1.1:1.3～1.6:2.5～3.0 are mixed, the reactor of putting into, reactor upper end is provided with gas duct, and gas duct connects and is equipped with in the gas receptor of ammonium bicarbonate soln;
B, under atmospheric pressure state, stir, heater, the temperature that makes to mix rear raw material arrives 100～125 DEG C, the gas of generation enters in gas receptor by conduit;
C, gained material in reactor in step b is filtered, gained solution is alum liquor, and alum liquor is heated to boiling, obtains solid sulphuric acid aluminium after cooling;
D, the material of gained in gas receptor in step c is filtered, after gained solid drying, be white carbon black, gained solution is ammonium fluoride solution; Described ammonium fluoride solution is heated to boiling, and cooling post crystallization obtains Neutral ammonium fluoride crystal.
Preferably, the mass concentration of ammonium bicarbonate soln described in step a is 25%, mass ratio=8.9～10.8:0.9～1.1 of described ammonium bicarbonate soln and bauxite.
Preferably, fluorite described in step a and bauxite are first crushed to 60 orders, and then put into reactor.
Preferably, to be adopted as massfraction be 92% industrial sulphuric acid to sulfuric acid described in step a.
Preferably, when alum liquor Heating temperature is to 133-137 DEG C described in step c, stop heating and stir, obtaining Tai-Ace S 150 solid.
Preferably, when ammonium fluoride solution described in steps d is heated to liquid level and occurs epitaxial, stop heating, stirred solution, is distributed in solution as nucleus epitaxial, stops stirred solution, and solution is cooled to room temperature, can obtain described Neutral ammonium fluoride crystal.
Preferably, reactor described in step a is sealed vessel, and described silicon tetrafluoride gas imports in described gas receptor by conduit.
The invention has the beneficial effects as follows, organically combined by original two kinds of production technique, two cover production equipments, unite two into one, reduce production costs; Under normal pressure, react, production equipment is required to reduce; Bauxite and sulfuric acid reaction heat release provide energy, save energy for fluorite and sulfuric acid reaction; Discarded silicon-dioxide is fully used; Do not need with sinking agent, aftertreatment is simple.
Brief description of the drawings
Fig. 1 is that the present invention prepares Tai-Ace S 150, white carbon black and Neutral ammonium fluoride reaction unit schematic diagram.
In figure: well heater 1, closed reactor 2, reactant (bauxite, fluorite, sulfuric acid, water) 3, thermometer 4, agitator 5, prolong 6, gas receptor 7, absorption liquid (ammonium bicarbonate soln) 8.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, to make those skilled in the art can implement according to this with reference to specification sheets word.
Embodiment 1
Reactant 3 is according to following proportioning: get 100g and be crushed to 60 object bauxite (aluminum oxide by 35.7%, silicon-dioxide by 46.8%), add 142.7g fluorite (Calcium Fluoride (Fluorspan) is by 85.2%), fluorite is also crushed to 60 orders, then to add 277.7g massfraction according to aluminum oxide, Calcium Fluoride (Fluorspan) and sulfuric acid reaction relation be 92% sulphuric acid soln.
As shown in Figure 1, reactant 3 is placed in to closed reactor 2, turn on agitator 5 stirred solutions, heater 1 heated solution, make the temperature of solution remain on 100～125 DEG C, the gas that reaction generates to gas receptor 7, fills absorption liquid 8 (25% ammonium bicarbonate soln 984.3g) via prolong 6 in gas receptor 7.In the time no longer including bubble in gas receptor 7 and occur, close well heater 1 and stop heating, close agitator 5 and stop stirred solution.After reaction, in closed reactor 2, solution is alum liquor, is precipitated as calcium sulfate.In gas receptor 7, white precipitate is that white carbon black, solution are ammonium fluoride solution.Chemical equation is as follows:
Prepare Tai-Ace S 150:
Al
2o
3+ 3H
2sO
4=Al
2(SO
4)
3+ 3H
2o (reacting in the closed reactor 2 in Fig. 1)
Prepare white carbon black, Neutral ammonium fluoride:
CaF
2+H
2SO
4＝CaSO
4↓+2HF
SiO
2+4HF＝SiF
4↑+2H
2O
3SiF
4+2H
2O+nH
2O＝2H
2SiF
6+SiO
2·nH
2O↓
H
2SiF
6+2NH
4HCO
3＝(NH
4)
2SiF
6+2CO
2↑+2H
2O
(NH
4)
2SiF
6+4NH
4HCO
3+nH
2O＝6NH
4F+SiO
2·nH
2O↓+4CO
2↑+2H
2O
By the solution filter of gained in closed reactor 2, the solid of gained is calcium sulfate, and gained solution is alum liquor;
The alum liquor filtrate of gained is placed in to vaporizer, and turn on agitator and heater heats solution are to boiling, evaporating solvent.In the time that thermometer instruction solution temperature is 133～137 DEG C, stop heating, close agitator and stop stirring, after solution is cooling, obtain solid sulphuric acid aluminium.
Gained solution in gas receptor 7 is filtered, the solid drying of gained is to white carbon black, gained solution is ammonium fluoride solution.
Ammonium fluoride solution is placed in to vaporizer, and heater heating ammonium fluoride solution to solution seethes with excitement, and evaporating solvent, in the time that epitaxial appears in liquid level, stops heating.Turn on agitator stirred solution, is distributed in solution as nucleus epitaxial.Close agitator and stop stirred solution.Solution is cooled to room temperature, obtains Neutral ammonium fluoride crystal.
Ammonium fluoride solution after crystallization filters.After filtration, obtain Neutral ammonium fluoride crystal in funnel, filtrate is Neutral ammonium fluoride saturated solution, retains filtrate same with other evaporative crystallization recovery more together.
Embodiment 2
Reactant 3 is according to following proportioning: get 90g and be crushed to 60 object bauxite (aluminum oxide by 35.7%, silicon-dioxide by 46.8%), add 130g fluorite (Calcium Fluoride (Fluorspan) is by 85.2%), fluorite is also crushed to 60 orders, then to add 250g massfraction according to aluminum oxide, Calcium Fluoride (Fluorspan) and sulfuric acid reaction relation be 92% sulphuric acid soln.
As shown in Figure 1, reactant 3 is placed in to closed reactor 2, turn on agitator 5 stirred solutions, heater 1 heated solution, make the temperature of solution remain on 100～125 DEG C, the gas that reaction generates to gas receptor 7, fills absorption liquid 8 (25% ammonium bicarbonate soln 890g) via prolong 6 in gas receptor 7.In the time no longer including bubble in gas receptor 7 and occur, close well heater 1 and stop heating, close agitator 5 and stop stirred solution.After reaction, in closed reactor 2, solution is alum liquor, is precipitated as calcium sulfate.In gas receptor 7, white precipitate is that white carbon black, solution are ammonium fluoride solution.
By the solution filter of gained in closed reactor 2, the solid of gained is calcium sulfate, and gained solution is alum liquor;
The alum liquor filtrate of gained is placed in to vaporizer, and turn on agitator and heater heats solution are to boiling, evaporating solvent.In the time that thermometer instruction solution temperature is 133～137 DEG C, stop heating, close agitator and stop stirring, after solution is cooling, obtain solid sulphuric acid aluminium.
Gained solution in gas receptor 7 is filtered, the solid drying of gained is to white carbon black, gained solution is ammonium fluoride solution.
Ammonium fluoride solution is placed in to vaporizer, and heater heating ammonium fluoride solution to solution seethes with excitement, and evaporating solvent, in the time that epitaxial appears in liquid level, stops heating.Turn on agitator stirred solution, is distributed in solution as nucleus epitaxial.Close agitator and stop stirred solution.Solution is cooled to room temperature, obtains Neutral ammonium fluoride crystal.
Ammonium fluoride solution after crystallization filters.After filtration, obtain Neutral ammonium fluoride crystal in funnel, filtrate is Neutral ammonium fluoride saturated solution, retains filtrate same with other evaporative crystallization recovery more together.
Embodiment 3
Reactant 3 is according to following proportioning: get 110g and be crushed to 60 object bauxite (aluminum oxide by 35.7%, silicon-dioxide by 46.8%), add 160g fluorite (Calcium Fluoride (Fluorspan) is by 85.2%), fluorite is also crushed to 60 orders, then to add 300g massfraction according to aluminum oxide, Calcium Fluoride (Fluorspan) and sulfuric acid reaction relation be 92% sulphuric acid soln.
As shown in Figure 1, reactant 3 is placed in to closed reactor 2, turn on agitator 5 stirred solutions, heater 1 heated solution, make the temperature of solution remain on 100～125 DEG C, the gas that reaction generates to gas receptor 7, fills absorption liquid 8 (25% ammonium bicarbonate soln 1080g) via prolong 6 in gas receptor 7.In the time no longer including bubble in gas receptor 7 and occur, close well heater 1 and stop heating, close agitator 5 and stop stirred solution.After reaction, in closed reactor 2, solution is alum liquor, is precipitated as calcium sulfate.In gas receptor 7, white precipitate is that white carbon black, solution are ammonium fluoride solution.
By the solution filter of gained in closed reactor 2, the solid of gained is calcium sulfate, and gained solution is alum liquor;
The alum liquor filtrate of gained is placed in to vaporizer, and turn on agitator and heater heats solution are to boiling, evaporating solvent.In the time that thermometer instruction solution temperature is 133～137 DEG C, stop heating, close agitator and stop stirring, after solution is cooling, obtain solid sulphuric acid aluminium.
Gained solution in gas receptor 7 is filtered, the solid drying of gained is to white carbon black, gained solution is ammonium fluoride solution.
Ammonium fluoride solution is placed in to vaporizer, and heater heating ammonium fluoride solution to solution seethes with excitement, and evaporating solvent, in the time that epitaxial appears in liquid level, stops heating.Turn on agitator stirred solution, is distributed in solution as nucleus epitaxial.Close agitator and stop stirred solution.Solution is cooled to room temperature, obtains Neutral ammonium fluoride crystal.
Ammonium fluoride solution after crystallization filters.After filtration, obtain Neutral ammonium fluoride crystal in funnel, filtrate is Neutral ammonium fluoride saturated solution, retains filtrate same with other evaporative crystallization recovery more together.
Embodiment 4
Reactant 3 is according to following proportioning: get 105g and be crushed to 60 object bauxite (aluminum oxide by 35.7%, silicon-dioxide by 46.8%), add 150g fluorite (Calcium Fluoride (Fluorspan) is by 85.2%), fluorite is also crushed to 60 orders, then to add 292g massfraction according to aluminum oxide, Calcium Fluoride (Fluorspan) and sulfuric acid reaction relation be 92% sulphuric acid soln.
As shown in Figure 1, reactant 3 is placed in to closed reactor 2, turn on agitator 5 stirred solutions, heater 1 heated solution, make the temperature of solution remain on 100～125 DEG C, the gas that reaction generates to gas receptor 7, fills absorption liquid 8 (25% ammonium bicarbonate soln 1034g) via prolong 6 in gas receptor 7.In the time no longer including bubble in gas receptor 7 and occur, close well heater 1 and stop heating, close agitator 5 and stop stirred solution.After reaction, in closed reactor 2, solution is alum liquor, is precipitated as calcium sulfate.In gas receptor 7, white precipitate is that white carbon black, solution are ammonium fluoride solution.
By the solution filter of gained in closed reactor 2, the solid of gained is calcium sulfate, and gained solution is alum liquor;
The alum liquor filtrate of gained is placed in to vaporizer, and turn on agitator and heater heats solution are to boiling, evaporating solvent.In the time that thermometer instruction solution temperature is 133～137 DEG C, stop heating, close agitator and stop stirring, after solution is cooling, obtain solid sulphuric acid aluminium.
Gained solution in gas receptor 7 is filtered, the solid drying of gained is to white carbon black, gained solution is ammonium fluoride solution.
Ammonium fluoride solution is placed in to vaporizer, and heater heating ammonium fluoride solution to solution seethes with excitement, and evaporating solvent, in the time that epitaxial appears in liquid level, stops heating.Turn on agitator stirred solution, is distributed in solution as nucleus epitaxial.Close agitator and stop stirred solution.Solution is cooled to room temperature, obtains Neutral ammonium fluoride crystal.
Ammonium fluoride solution after crystallization filters.After filtration, obtain Neutral ammonium fluoride crystal in funnel, filtrate is Neutral ammonium fluoride saturated solution, retains filtrate same with other evaporative crystallization recovery more together.
By the method for co-producing sulfuric acid aluminium, white carbon black and Neutral ammonium fluoride involved in the present invention.The final Tai-Ace S 150 purity obtaining is 84.4%, and white carbon black purity is 95.8%, and Neutral ammonium fluoride purity is 98.8%.
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in bright book and embodiment, 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.
Claims (7)
1. a method for co-producing sulfuric acid aluminium, white carbon black and Neutral ammonium fluoride, is characterized in that, comprises the following steps:
A, bauxite, fluorite, sulfuric acid raw material in mass ratio=0.9～1.1:1.3～1.6:2.5～3.0 are mixed, the reactor of putting into, reactor upper end is provided with gas duct, and gas duct connects and is equipped with in the gas receptor of ammonium bicarbonate soln;
B, under atmospheric pressure state, stir, heater, the temperature that makes to mix rear raw material arrives 100～125 DEG C, the gas of generation enters in gas receptor by conduit;
C, gained material in reactor in step b is filtered, gained solution is alum liquor, and alum liquor is heated to boiling, obtains solid sulphuric acid aluminium after cooling;
D, the material of gained in gas receptor in step c is filtered, after gained solid drying, be white carbon black, gained solution is ammonium fluoride solution; Described ammonium fluoride solution is heated to boiling, and cooling post crystallization obtains Neutral ammonium fluoride crystal.
2. the method for co-producing sulfuric acid aluminium according to claim 1, white carbon black and Neutral ammonium fluoride, it is characterized in that: the mass concentration of ammonium bicarbonate soln described in step a is 25%, mass ratio=8.9～10.8:0.9～1.1 of described ammonium bicarbonate soln and bauxite.
3. the method for co-producing sulfuric acid aluminium according to claim 1, white carbon black and Neutral ammonium fluoride, is characterized in that: fluorite described in step a and bauxite are first crushed to 60 orders, and then puts into reactor.
4. the method for co-producing sulfuric acid aluminium according to claim 1, white carbon black and Neutral ammonium fluoride, is characterized in that: it is 92% industrial sulphuric acid that sulfuric acid described in step a is adopted as massfraction.
5. the method for co-producing sulfuric acid aluminium according to claim 1, white carbon black and Neutral ammonium fluoride, is characterized in that: when alum liquor Heating temperature is to 133-137 DEG C described in step c, stop heating and stir, obtaining Tai-Ace S 150 solid.
6. the method for co-producing sulfuric acid aluminium according to claim 1, white carbon black and Neutral ammonium fluoride, it is characterized in that: when ammonium fluoride solution described in steps d is heated to liquid level and occurs epitaxial, stop heating, stirred solution, epitaxial is distributed in solution as nucleus, stop stirred solution, solution is cooled to room temperature, can obtain described Neutral ammonium fluoride crystal.
7. the method for co-producing sulfuric acid aluminium according to claim 1, white carbon black and Neutral ammonium fluoride, is characterized in that: reactor described in step a is sealed vessel, and described silicon tetrafluoride gas imports in described gas receptor by conduit.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495856A (en) * | 2015-01-14 | 2015-04-08 | 辽宁石化职业技术学院 | Method for preparing white carbon black using bauxite acidolysis waste residues |
| CN105197959A (en) * | 2015-09-09 | 2015-12-30 | 洛阳国兴矿业科技有限公司 | Method of recovering fluorine resource in process of processing low-grade bauxite by chemical floatation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1884077A (en) * | 2006-07-07 | 2006-12-27 | 贵州省化工研究院 | Method for aminolysis of fluorosilicone compounds and separation of fluorine and silicon |
| CN103539130A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Technological method for preparing white carbon black from potassium feldspar |
| CN103896215A (en) * | 2012-12-31 | 2014-07-02 | 天津市泰亨气体有限公司 | Fluorite-sulfuric acid method for preparing hydrogen fluoride |
-
2014
- 2014-07-15 CN CN201410336895.6A patent/CN104071817B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1884077A (en) * | 2006-07-07 | 2006-12-27 | 贵州省化工研究院 | Method for aminolysis of fluorosilicone compounds and separation of fluorine and silicon |
| CN103896215A (en) * | 2012-12-31 | 2014-07-02 | 天津市泰亨气体有限公司 | Fluorite-sulfuric acid method for preparing hydrogen fluoride |
| CN103539130A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Technological method for preparing white carbon black from potassium feldspar |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495856A (en) * | 2015-01-14 | 2015-04-08 | 辽宁石化职业技术学院 | Method for preparing white carbon black using bauxite acidolysis waste residues |
| CN105197959A (en) * | 2015-09-09 | 2015-12-30 | 洛阳国兴矿业科技有限公司 | Method of recovering fluorine resource in process of processing low-grade bauxite by chemical floatation method |
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| CN104071817B (en) | 2015-11-18 |
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