CN102492862A - Method of preparing aluminum-silicon alloy and cryolite from sodium fluorosilicate - Google Patents

Method of preparing aluminum-silicon alloy and cryolite from sodium fluorosilicate Download PDF

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CN102492862A
CN102492862A CN2011103901010A CN201110390101A CN102492862A CN 102492862 A CN102492862 A CN 102492862A CN 2011103901010 A CN2011103901010 A CN 2011103901010A CN 201110390101 A CN201110390101 A CN 201110390101A CN 102492862 A CN102492862 A CN 102492862A
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aluminum
sodium
silicon alloy
fluoride
preparation
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CN102492862B (en
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梁雪松
肖勇
吴立群
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Yunnan Chemical Research Institute
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Yunnan Chemical Research Institute
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Abstract

The invention relates to the technical field of materials and especially to a method of preparing aluminum-silicon alloy and cryolite through reaction between sodium fluorosilicate and aluminum. The method comprises the following steps: a, fusing 100 to 110 kg of industrial aluminum powder in a graphite crucible and maintaining the graphite crucible at a temperature of 800 to 900 DEG C; b, blowing 40 to 200 kg of industrial sodium fluorosilicate and sodium fluoride powder into the graphite crucible under the protection of a dry argon atmosphere at a speed of 3-5 kg/min for reaction with molten aluminum so as to obtain cryolite solid and molten aluminum-silicon alloy; c, separating the obtained cryolite solid from the molten aluminum-silicon alloy. The method provided in the invention enables the problems of three wastes, high energy consumption and the like appearing in traditional processes to be avoided and has small environmental load and high environmental benefits.

Description

The method of preparation with sodium fluosilicate aluminum-silicon alloy and sodium aluminum fluoride
Technical field
The present invention relates to the material technology field, particularly a kind of method for preparing aluminum-silicon alloy and sodium aluminum fluoride by Sodium Silicofluoride 98min and reactive aluminum.
Background technology
Aluminum-silicon alloy is a kind of strong composite deoxidant, in steelmaking process, replaces fine aluminium can improve the reductor utilization ratio, but and cleaning molten steel, improve steel product quality.Aluminium-deoxidized steel ingot is commonly referred to as calm steel, owing to can be oxidized to aluminum oxide behind the aluminium deoxidation, aluminum oxide can refine austenite crystal grain, so the steel of aluminium deoxidation has better comprehensive mechanical property.Aluminum-silicon alloy density is little, and thermal expansivity is low, and castability and abrasion resistance are good, has very high resistance impact capacity and good high pressure compactness with its alloy-steel casting of casting, can improve work-ing life greatly.Aluminum-silicon alloy produces E material, space material as a kind of new E car material, senior skill electronics; Produce on the aviation E spare under E and the hot environment and have broad application prospects at E car wheel box, motor body, E valve, direction E, piston, wheel hub, senior skill electronics, commonly used its produced aerospacecraft and automobile component.
Sodium aluminum fluoride (Cryolite) mainly is used as the fusing assistant of electrolysis of aluminum, the wear-resistant filler of rubber, emery wheel, enamel opacifier, glass opalizer and metal flux, the agrochemical of farm crop.On Aluminium industry, do not find also that up to now another kind of compound can replace sodium aluminum fluoride.This is because sodium aluminum fluoride is except can also having some other indispensable character, as not containing than the more electropositive element of aluminium, good stability the dissolved oxygen aluminium; Under general condition do not decompose, non-volatile, deliquescence not; Fusing point is higher than aluminium, good conductivity, save power etc.We can say, if there is not sodium aluminum fluoride, the perhaps just so not large-scale aluminium industry in the whole world, price is just so not low yet, uses just so not extensive yet.Aluminum-silicon alloy is to use the widest y alloy y, and the used aluminum-silicon alloy in countries in the world all is that fine aluminium and pure silicon consolute are mixed production at present.Producing fine aluminium needs high-grade bauxite, and the static state of China's bauxite ensures that the time limit has only more than ten years, and this method production aluminum-silicon alloy technical process is long and complicated, and energy consumption is high.
Summary of the invention
The objective of the invention is to overcome the defective of prior art; A kind of aluminum-silicon alloy that utilizes phosphatic fertilizer company low value by-product sodium fluosilicate to prepare high added value is provided; And can not produce reluctant waste in the process; Utilize the Sodium Silicofluoride 98min of by-product in the phosphatic fertilizer company efficiently, adopt the method for molten state aluminium and Sodium Silicofluoride 98min prepared in reaction aluminum-silicon alloy and sodium aluminum fluoride.
The method of a kind of preparation with sodium fluosilicate aluminum-silicon alloy of the present invention and sodium aluminum fluoride may further comprise the steps:
A. with industrial aluminium powder fusion in plumbago crucible of 100-110kg, and maintain the temperature at 800 ℃-900 ℃;
B. the industrial Sodium Silicofluoride 98min of 40-200kg and sodium fluoride powder are blown in the plumbago crucible and the molten aluminum reaction with the speed of 3-5kg/min under the exsiccant argon shield, obtain the aluminum-silicon alloy of sodium aluminum fluoride solid and molten state;
C. the sodium aluminum fluoride solid that obtains is separated with the molten state aluminum-silicon alloy.
Step a is described to be that plumbago crucible is positioned in the closed reactor of band heating with the fusion in plumbago crucible of industrial aluminium powder.
The necessary excessive 2.3-10.3 of industrial aluminium powder doubly among the step a.
Industrial Sodium Silicofluoride 98min and Sodium Fluoride mix among the step b, and wherein the purity of Sodium Silicofluoride 98min is at 98%wt) more than, Fe content is no more than 0.3% wt..
The step b reaction times, temperature of reaction was between 660 ℃-1100 ℃ between 15min-60min.
Slowly being blown among the step b is to be blown into through the speed of sandblast apparatus with 3-5kg/min.
The described isolating mode of overflow that is separated into of step c.
The method of preparation with sodium fluosilicate aluminum-silicon alloy of the present invention and sodium aluminum fluoride is to utilize Sodium Silicofluoride 98min and reactive aluminum, under the excessive situation of aluminium, controls different mol ratio, reaction times and temperature of reaction, obtains the different aluminum-silicon alloy of silicone content.
Principle of the present invention can be described and explains according to following reaction equation:
Na 2SiF 6?→?2NaF?+?SiF 4 (1)
3SiF 4?+?4Al?→?4AlF 3?+?3Si (2)
3NaF?+?AlF 3?→?Na 3AlF 6 (3)
Figure 106747DEST_PATH_IMAGE001
4Al?+?3Na 2SiF 6?+?6NaF?→?4?Na 3AlF 6?+?3Si
When Al is excessive, form the Al-Si alloy.
Outstanding advantage of the present invention is its economy and environmental value.Economic worth has been to extend the industrial chain of phosphatic fertilizer company low value by-product sodium fluosilicate, and Sodium Silicofluoride 98min and reactive aluminum are obtained high value added product aluminum-silicon alloy and sodium aluminum fluoride, makes the distinctive fluorine of phosphatic fertilizer company, silicon resource obtain fully, utilize efficiently.
Environmental value of the present invention is for phosphatic fertilizer company a kind of environmentally friendly innovative technology method that is different from traditional fluorine, silicon resource utilization to be provided; Sodium Silicofluoride 98min and reactive aluminum, the different mol ratio of control; Different aluminum-silicon alloy and the sodium aluminum fluoride products of preparation silicone content; Avoided problems such as " three wastes " that the traditional technology route produces and high energy consumption, carrying capacity of environment is less, and environmental benefit is higher.
The unit equipment that innovative technology method of the present invention can adopt existing technology and process large-scale commercial prodn to verify is implemented and is realized.
Embodiment
The method of preparation with sodium fluosilicate aluminum-silicon alloy of the present invention and sodium aluminum fluoride will specify in following embodiment, but be not limited to embodiment.
Embodiment 1
Earlier 102kg industry aluminium powder is placed plumbago crucible, again plumbago crucible is put into the closed reactor heating and make industrial aluminium powder fusion, and maintain the temperature between 800 ℃-900 ℃.Then 47kg industry Sodium Silicofluoride 98min slowly is blown under the exsiccant argon shield in the plumbago crucible with the dry in advance also sodium fluoride powder of mixing of 21kg and reacts with molten aluminum; Temperature keeps 700 ℃, reaction 30min; Obtain the aluminum-silicon alloy of 70kg sodium aluminum fluoride solid and 100kg molten state, wherein silicone content is 7%.Mode through overflow is separated the aluminum-silicon alloy of sodium aluminum fluoride solid and molten state at last.
Embodiment 2
Earlier 103.6kg industry aluminium powder is placed plumbago crucible, again plumbago crucible is put into the closed reactor heating and make industrial aluminium powder fusion, and maintain the temperature between 800 ℃-900 ℃.Then 84.1kg industry Sodium Silicofluoride 98min slowly is blown under the exsiccant argon shield in the plumbago crucible with the dry in advance also sodium fluoride powder of mixing of 37.6kg and reacts with molten aluminum; Temperature keeps 800 ℃, reaction 20min; Obtain the aluminum-silicon alloy of 125kg sodium aluminum fluoride solid and 100kg molten state, wherein silicone content is 12.5%.Mode through overflow is separated the aluminum-silicon alloy of sodium aluminum fluoride solid and molten state at last.
Embodiment 3
Earlier 104.3kg industry aluminium powder is placed plumbago crucible, again plumbago crucible is put into the closed reactor heating and make industrial aluminium powder fusion, and maintain the temperature between 800 ℃-900 ℃.Then 100.8kg industry Sodium Silicofluoride 98min slowly is blown under the exsiccant argon shield in the plumbago crucible with the dry in advance also sodium fluoride powder of mixing of 45kg and reacts with molten aluminum; Temperature keeps 900 ℃, reaction 15min; Obtain the aluminum-silicon alloy of 150kg sodium aluminum fluoride solid and 100kg molten state, wherein silicone content is 15%.Mode through overflow is separated the aluminum-silicon alloy of sodium aluminum fluoride solid and molten state at last.
Embodiment 4
Earlier 105.7kg industry aluminium powder is placed plumbago crucible, again plumbago crucible is put into the closed reactor heating and make industrial aluminium powder fusion, and maintain the temperature between 800 ℃-900 ℃.Then 134.2kg industry Sodium Silicofluoride 98min slowly is blown under the exsiccant argon shield in the plumbago crucible with the dry in advance also sodium fluoride powder of mixing of 60kg and reacts with molten aluminum; Temperature keeps 750 ℃, reaction 40min; Obtain the aluminum-silicon alloy of 200kg sodium aluminum fluoride solid and 100kg molten state, wherein silicone content is 20%.Mode through overflow is separated the aluminum-silicon alloy of sodium aluminum fluoride solid and molten state at last.
Embodiment 5
Earlier 107.1kg industry aluminium powder is placed plumbago crucible, again plumbago crucible is put into the closed reactor heating and make industrial aluminium powder fusion, and maintain the temperature between 800 ℃-900 ℃.Then 167.6kg industry Sodium Silicofluoride 98min slowly is blown under the exsiccant argon shield in the plumbago crucible with the dry in advance also sodium fluoride powder of mixing of 74.9kg and reacts with molten aluminum; Temperature keeps 850 ℃, reaction 25min; Obtain the aluminum-silicon alloy of 250kg sodium aluminum fluoride solid and 100kg molten state, wherein silicone content is 25%.Mode through overflow is separated the aluminum-silicon alloy of sodium aluminum fluoride solid and molten state at last.

Claims (7)

1. the method for preparation with sodium fluosilicate aluminum-silicon alloy and sodium aluminum fluoride is characterized in that may further comprise the steps:
A. with industrial aluminium powder fusion in plumbago crucible of 100-110kg, and maintain the temperature at 800 ℃-900 ℃;
B. the industrial Sodium Silicofluoride 98min of 40-200kg and sodium fluoride powder are blown in the plumbago crucible and the molten aluminum reaction with the speed of 3-5kg/min under the exsiccant argon shield, obtain the aluminum-silicon alloy of sodium aluminum fluoride solid and molten state;
C. the sodium aluminum fluoride solid that obtains is separated with the molten state aluminum-silicon alloy.
2. the method for preparation with sodium fluosilicate aluminum-silicon alloy as claimed in claim 1 and sodium aluminum fluoride is characterized in that, step a is described to be that plumbago crucible is positioned in the closed reactor of band heating with the fusion in plumbago crucible of industrial aluminium powder.
3. the method for preparation with sodium fluosilicate aluminum-silicon alloy as claimed in claim 1 and sodium aluminum fluoride is characterized in that, the necessary excessive 2.3-10.3 of industrial aluminium powder doubly among the step a.
4. the method for preparation with sodium fluosilicate aluminum-silicon alloy as claimed in claim 1 and sodium aluminum fluoride is characterized in that industrial Sodium Silicofluoride 98min and Sodium Fluoride mix among the step b, and wherein the purity of Sodium Silicofluoride 98min is more than 98%wt., and Fe content is no more than 0.3% wt..
5. the method for preparation with sodium fluosilicate aluminum-silicon alloy as claimed in claim 1 and sodium aluminum fluoride is characterized in that, the step b reaction times, temperature of reaction was between 660 ℃-1100 ℃ between 15min-60min.
6. the method for preparation with sodium fluosilicate aluminum-silicon alloy as claimed in claim 1 and sodium aluminum fluoride is characterized in that, slowly being blown among the step b is to be blown into through the speed of sandblast apparatus with 3-5kg/min.
7. the method for preparation with sodium fluosilicate aluminum-silicon alloy as claimed in claim 1 and sodium aluminum fluoride is characterized in that, the described isolating mode of overflow that is separated into of step c.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020218237A1 (en) * 2019-04-23 2020-10-29 国立大学法人東北大学 Dross generation suppression method, metal refinement method, and metal refinement apparatus

Citations (4)

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Publication number Priority date Publication date Assignee Title
US3656894A (en) * 1970-05-08 1972-04-18 Central Glass Co Ltd Process for the production of high quality synthetic cryolite
CN1225897A (en) * 1998-08-29 1999-08-18 李世江 Production of high molecular-ration cryolite by sodium-fluorosilicate sodium-aluminate method
CN1300879A (en) * 1999-12-19 2001-06-27 张国臣 One-step process for preparing cryolite with high molecular ratio from sodium fluosilicate
CN101269816A (en) * 2008-05-16 2008-09-24 夏克立 Method for producing fluorine series compounds and white carbon black

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3656894A (en) * 1970-05-08 1972-04-18 Central Glass Co Ltd Process for the production of high quality synthetic cryolite
CN1225897A (en) * 1998-08-29 1999-08-18 李世江 Production of high molecular-ration cryolite by sodium-fluorosilicate sodium-aluminate method
CN1300879A (en) * 1999-12-19 2001-06-27 张国臣 One-step process for preparing cryolite with high molecular ratio from sodium fluosilicate
CN101269816A (en) * 2008-05-16 2008-09-24 夏克立 Method for producing fluorine series compounds and white carbon black

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
周新泉: "用氟硅酸钠、铝酸钠为原料合成冰晶石的研究", 《轻金属》, no. 11, 30 November 1991 (1991-11-30), pages 17 - 20 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020218237A1 (en) * 2019-04-23 2020-10-29 国立大学法人東北大学 Dross generation suppression method, metal refinement method, and metal refinement apparatus

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