CN101134592A - Preparation method of aluminun fluoride - Google Patents
Preparation method of aluminun fluoride Download PDFInfo
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- CN101134592A CN101134592A CNA2006101069796A CN200610106979A CN101134592A CN 101134592 A CN101134592 A CN 101134592A CN A2006101069796 A CNA2006101069796 A CN A2006101069796A CN 200610106979 A CN200610106979 A CN 200610106979A CN 101134592 A CN101134592 A CN 101134592A
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- sodium silicofluoride
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Abstract
The process of producing aluminum fluoride with sodium fluorosilicate and aluminum hydroxide as material includes the following steps: 1. decomposing sodium fluorosilicate to produce solid sodium fluoride and silicon tetrafluoride gas; 2. absorbing silicon tetrafluoride gas with water and hydrolyzing, and washing and drying silica to obtain carbon white; 3. reacting fluorosilicic acid solution and solid sodium sulfate, filtering to obtain sodium fluorosilicate to be returned to the step 1, and treating waste sulfuric acid solution for draining; 4. reacting solid sodium fluoride and sulfuric acid, condensing, rectifying to obtain anhydrous hydrofluoric acid and solid sodium sulfate returned to the step 1; and 5. reacting anhydrous hydrofluoric acid and aluminum hydroxide to produce aluminum fluoride product. The process has low production cost and environment friendship.
Description
Technical field
The present invention relates to a kind of preparation method of aluminum fluoride, relating in particular to a kind of is the method for feedstock production aluminum fluoride with Sodium Silicofluoride and aluminium hydroxide.
Background technology
Aluminum fluoride as auxiliary agent, is used to reduce electrolytical fusing point, improves electrolytical electric conductivity in Aluminum Electrolysis Production.Its traditional processing technology is a hydrofluoric acid---dry process and hydrofluoric acid---wet processing.The raw material of hydrofluoric acid---dry process is hydrogen fluoride and aluminium hydroxide, its production technique is for comprising that aluminium hydroxide is carried out pre-treatment removes crystal water, the thorough mixing reaction under 500-600 ℃ temperature with powdery aluminium hydroxide and hydrogen fluoride gas then, generate aluminum trifluoride at reactor bottom, with aluminum trifluoride send into rotary drum cool off finished product; The raw material of hydrofluoric acid---wet processing is hydrofluoric acid and aluminium hydroxide, and production technique is that hydrofluoric acid and aluminum hydroxide slime react, crystallization, gets aluminum fluoride trihydrate, and drying dehydration again makes aluminium fluoride product.Above-mentioned two kinds of production technique cost of material height, the production cost height, and production technique is comparatively complicated.
Summary of the invention
At the problems referred to above, the object of the invention is to provide a kind of preparation method of aluminum fluoride, to reduce production costs simple production technology greatly.
To achieve these goals, having technical program of the present invention lies in adopting a kind of preparation method of aluminum fluoride, is raw material with Sodium Silicofluoride, aluminium hydroxide, specifically may further comprise the steps:
(1) Sodium Silicofluoride was decomposed under 300～800 ℃ temperature 1～5 hour, generate Sodium Fluoride solid and silicon tetrafluoride gas;
(2) the silicon tetrafluoride gas water is absorbed and hydrolysis, filtration makes silicate fluoride solution and removes to make Sodium Silicofluoride, and silica solid washing, drying obtain white carbon black;
(3) with silicate fluoride solution and sodium sulfate solid reaction 10～60 minutes, after reaction finishes, filter and obtain the Sodium Silicofluoride solid and return and carry out decomposition reaction, sulfuric acid waste is handled discharging;
(4) Sodium Fluoride solid that step (1) is generated and 98% above sulfuric acid reacted 2-5 hour under 150-3000 ℃ temperature, and the gas of generation obtains anhydrous hydrofluoric acid through condensation rectifying, and the sodium sulfate solid of generation returns the system Sodium Silicofluoride;
(5) anhydrous hydrofluoric acid is fed in thorough mixing and rapid reaction in the fluidized-bed reactor with the aluminium hydroxide solid by reaction ratio after heating up and gasifying, and temperature of reaction is controlled at 500-600 ℃, and reaction has generated the solid phase prod aluminum fluoride.
The concentration of described silicate fluoride solution is 10-40%.
Reaction formula of the present invention is:
Na
2SiF
6→2NaF+SiF
4↑
3SiF
4+2H
2O→2H
2SiF
6+SiO
2↓
H
2SiF
6+Na
2SO
4→Na
2SiF
6+H
2SO
4
2NaF+H
2SO
4→2HF↑+Na
2SO
4
3HF-Al(OH)
3＝AlF
3+3H
2O
The present invention is that raw material replaces hydrogen fluoride with the Sodium Silicofluoride; Sodium Silicofluoride is the by-product harmful waste of phophatic fertilizer production process; purposes seldom; its environment protection caused have a strong impact on; and the present invention utilizes Sodium Silicofluoride to prepare aluminum fluoride for raw material just, and its influence to surrounding environment has been alleviated in the utilization of Sodium Silicofluoride greatly, and because the Sodium Silicofluoride cost is low; raw material is easy to get, thereby greatly reduces the production cost of aluminum fluoride.In addition, the product in the reaction process of the present invention can recycle, greatly reduces production cost to a certain extent, and the present invention has favorable social and economic worth, is easy to apply.
The aluminium fluoride product mass analysis result who utilizes method of the present invention to produce
| Grade | Chemical ingredients % | |||||||
| Be not less than | Impurity is not more than | |||||||
| F | Al | Na | SiO 2 | Fe 2O 3 | SO 4 2- | P 2O 5 | H 2O | |
| Special one-level | 61 | 30 | 0.5 | 0.28 | 0.10 | 0.5 | 0.04 | 0.5 |
| Special secondary | 60 | 30 | 0.5 | 0.30 | 0.13 | 0.8 | 0.04 | 1.0 |
| One-level | 58 | 28.2 | 3.0 | 0.30 | 0.13 | 1.1 | 0.04 | 6.0 |
| Secondary | 57 | 28.2 | 3.5 | 0.35 | 0.15 | 1.2 | 0.04 | 7.0 |
| Present method 1# | 61.8 | 31 | 0.2 | 0.05 | 0.01 | 0.1 | 0.01 | 0.3 |
| Present method 2# | 61.3 | 30.8 | 0.2 | 0.08 | 0.02 | 0.2 | 0.02 | 0.4 |
Embodiment
Embodiment 1
The preparation method of aluminum fluoride of the present invention is a raw material with Sodium Silicofluoride, aluminium hydroxide, specifically may further comprise the steps:
(1) Sodium Silicofluoride was decomposed 4 hours under 350 ℃ temperature, generate Sodium Fluoride solid and silicon tetrafluoride gas;
(2) the silicon tetrafluoride gas water is absorbed and hydrolysis, filtering and making concentration is that 15% silicate fluoride solution removes to make Sodium Silicofluoride, and silica solid washing, drying obtain white carbon black;
(3) with silicate fluoride solution and sodium sulfate solid reaction 30 minutes, after reaction finishes, filter the Sodium Silicofluoride solid that obtains and return and carry out decomposition reaction, sulfuric acid waste is handled discharging;
(4) Sodium Fluoride solid that step (1) is generated and 98% sulfuric acid reacted 5 hours under 150 ℃ temperature, and the gas of generation obtains anhydrous hydrofluoric acid through condensation rectifying, and the sodium sulfate solid of generation returns the system Sodium Silicofluoride;
(5) anhydrous hydrofluoric acid is fed in thorough mixing and rapid reaction in the fluidized-bed reactor with the aluminium hydroxide solid by reaction ratio after heating up and gasifying, and temperature of reaction is controlled at 500 ℃, and reaction has generated the solid phase prod aluminum fluoride.
Embodiment 2
The preparation method of aluminum fluoride of the present invention is a raw material with Sodium Silicofluoride, aluminium hydroxide, specifically may further comprise the steps:
(1) Sodium Silicofluoride was decomposed 3 hours under 450 ℃ temperature, generate Sodium Fluoride solid and silicon tetrafluoride gas;
(2) the silicon tetrafluoride gas water is absorbed and hydrolysis, filter, make concentration and be 25% silicate fluoride solution and remove to make Sodium Silicofluoride, silica solid washing, drying obtain white carbon black;
(3) with 25% silicate fluoride solution and solid sodium sulfate reaction 30 minutes, filter and obtain the Sodium Silicofluoride solid, the Sodium Silicofluoride that makes can return and carry out decomposition reaction again, sulfuric acid waste is handled discharging;
(4) Sodium Fluoride solid that step (1) is generated and 99% sulfuric acid reacted 4 hours under 250 ℃ temperature, and the gas of generation obtains anhydrous hydrofluoric acid through condensation rectifying, and solid sodium sulfate returns the system Sodium Silicofluoride;
(5) anhydrous hydrofluoric acid is fed in thorough mixing and rapid reaction in the fluidized-bed reactor with solid aluminum hydroxide by reaction ratio after heating up and gasifying, and temperature of reaction is controlled at 550 ℃, and reaction has generated the solid phase prod aluminum fluoride.
Embodiment 3
(1) Sodium Silicofluoride was decomposed 2 hours under 750 ℃ temperature, generate Sodium Fluoride solid and silicon tetrafluoride gas;
(2) the silicon tetrafluoride gas water is absorbed and hydrolysis, filter and make 35% silicate fluoride solution and remove to make Sodium Silicofluoride, silica solid washing, drying obtain white carbon black;
(3) be 35% silicate fluoride solution and solid sodium sulfate reaction 30 minutes with concentration, filter and obtain the Sodium Silicofluoride solid that sulfuric acid waste is handled discharging;
(4) Sodium Fluoride solid that step (1) is generated and 100% sulfuric acid reacted 2 hours under 300 ℃ temperature, and the gas of generation obtains anhydrous hydrofluoric acid through condensation rectifying, and solid sodium sulfate returns the system Sodium Silicofluoride;
(5) anhydrous hydrofluoric acid is fed in thorough mixing and rapid reaction in the fluidized-bed reactor with solid aluminum hydroxide by reaction ratio after heating up and gasifying, and temperature of reaction is controlled at 600 ℃, and reaction has generated the solid phase prod aluminum fluoride.
It should be noted last that: above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although the present invention is had been described in detail with reference to the foregoing description, those of ordinary skill in the art is to be understood that: still can make amendment or be equal to replacement the present invention, and not breaking away from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (2)
1. the preparation method of an aluminum fluoride, it is characterized in that: with Sodium Silicofluoride, aluminium hydroxide is raw material, specifically may further comprise the steps:
(1) Sodium Silicofluoride was decomposed under 300～800 ℃ temperature 1～5 hour, generate Sodium Fluoride solid and silicon tetrafluoride gas;
(2) the silicon tetrafluoride gas water is absorbed and hydrolysis, filtration makes silicate fluoride solution and removes to make Sodium Silicofluoride, and silica solid washing, drying obtain white carbon black;
(3) with silicate fluoride solution and sodium sulfate solid reaction 10～60 minutes, after reaction finishes, filter and obtain the Sodium Silicofluoride solid and return and carry out decomposition reaction, sulfuric acid waste is handled discharging;
(4) Sodium Fluoride solid that step (1) is generated and 98% above sulfuric acid reaction, the gas of generation obtains anhydrous hydrofluoric acid through condensation rectifying, and the sodium sulfate solid of generation returns the system Sodium Silicofluoride;
(5) anhydrous hydrofluoric acid is fed in thorough mixing and rapid reaction in the fluidized-bed reactor with the aluminium hydroxide solid by reaction ratio after heating up and gasifying, and temperature of reaction is controlled at 500-600 ℃, and reaction has generated the solid phase prod aluminum fluoride.
2. the preparation method of aluminum fluoride according to claim 1, it is characterized in that: the concentration of described silicate fluoride solution is 10-40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101069796A CN101134592A (en) | 2006-09-01 | 2006-09-01 | Preparation method of aluminun fluoride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101069796A CN101134592A (en) | 2006-09-01 | 2006-09-01 | Preparation method of aluminun fluoride |
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| Publication Number | Publication Date |
|---|---|
| CN101134592A true CN101134592A (en) | 2008-03-05 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006101069796A Pending CN101134592A (en) | 2006-09-01 | 2006-09-01 | Preparation method of aluminun fluoride |
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|---|---|
| CN (1) | CN101134592A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992370A (en) * | 2011-09-14 | 2013-03-27 | 山东博丰利众化工有限公司 | High-purity aluminum fluoride production technology |
| CN114715849A (en) * | 2022-03-31 | 2022-07-08 | 贵州省化工研究院 | Method and device for preparing hydrogen fluoride by taking silicon tetrafluoride as raw material through electric field polarization hydrolysis |
-
2006
- 2006-09-01 CN CNA2006101069796A patent/CN101134592A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992370A (en) * | 2011-09-14 | 2013-03-27 | 山东博丰利众化工有限公司 | High-purity aluminum fluoride production technology |
| CN102992370B (en) * | 2011-09-14 | 2014-09-10 | 山东博丰利众化工有限公司 | High-purity aluminum fluoride production technology |
| CN114715849A (en) * | 2022-03-31 | 2022-07-08 | 贵州省化工研究院 | Method and device for preparing hydrogen fluoride by taking silicon tetrafluoride as raw material through electric field polarization hydrolysis |
| CN114715849B (en) * | 2022-03-31 | 2023-05-23 | 贵州省化工研究院 | Method and device for preparing hydrogen fluoride by electric field polarized hydrolysis by taking silicon tetrafluoride as raw material |
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Open date: 20080305 |