CN102390853A - Preparation method for anhydrous aluminum fluoride - Google Patents
Preparation method for anhydrous aluminum fluoride Download PDFInfo
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- CN102390853A CN102390853A CN2011102218962A CN201110221896A CN102390853A CN 102390853 A CN102390853 A CN 102390853A CN 2011102218962 A CN2011102218962 A CN 2011102218962A CN 201110221896 A CN201110221896 A CN 201110221896A CN 102390853 A CN102390853 A CN 102390853A
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- aluminum fluoride
- aluminium chloride
- drying
- anhydrous aluminium
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Abstract
The invention relates to a preparation method for anhydrous aluminum fluoride. The method is characterized in that: analytically pure aluminum fluoride trihydrate and ammonium hydrogen fluoride are used as raw materials in a preparation process of the method; and the preparation process comprises the following steps of: (1) drying the aluminum fluoride trihydrate to obtain AlF3.H2O; (2) cooling the dried AlF3.H2O to room temperature and then adding the ammonium hydrogen fluoride to uniformly mix; and (3) roasting the mixture obtained in the step (2) to prepare aluminum fluoride. By using the method, the cost is low, and the anhydrous aluminum fluoride with purity of more than 99.7 percent and aluminum oxide content of less than 0.05 percent can be prepared.
Description
Technical field
The present invention relates to a kind of preparation method of Anhydrous Aluminium Chloride.
Background technology
ALUMNIUM FLUORIDE is used for the electrolysis of aluminum industry in industry, be used for adjusting electrolytical molecular ratio.Alumina content is up to 4-15% in the industry ALUMNIUM FLUORIDE, but because wherein aluminum oxide also is the raw material of electrolysis of aluminum, so can not exert an influence to electrolytic process.Yet in breadboard research, need the ALUMNIUM FLUORIDE of purity higher (purity is greater than 99.5%), be used for the fundamental research of electrolytical physical chemistry and electrochemical properties, industrial ALUMNIUM FLUORIDE can not meet the demands.Yet in commercially available reagent, the purity of analytically pure Anhydrous Aluminium Chloride is merely 85%-96%, can not satisfy the requirement of Basic Experiment Study.Highly purified Anhydrous Aluminium Chloride reagent costs an arm and a leg, purity in the Anhydrous Aluminium Chloride reagent price more than 99.5% up to 50-120 unit/gram.
Anhydrous Aluminium Chloride is generally by aluminum fluoride trihydrate (AlF
33H
2O) add and obtain after thermal bake-out is removed crystal water, but this method causes degree of purity of production to reduce owing to when maturing temperature is higher than 300 ℃, can cause the aluminum fluoride trihydrate hydrolysis to generate aluminum oxide (seeing 1 formula).General direct roasting aluminum fluoride trihydrate prepares content that Anhydrous Aluminium Chloride can cause aluminum oxide in the product up to 4%-15%.
2AlF
3?+?3H
2O?=?Al
2O
3?+?6HF (1)
Also have the method for human vacuum volatilization recrystallize to prepare Anhydrous Aluminium Chloride, this method can obtain purity and be higher than 99.5% ALUMNIUM FLUORIDE, but cost is higher, and preparation cycle is long, and output is lower.
Summary of the invention
The objective of the invention is provides a kind of cost low in order to overcome the deficiency of aforesaid method, and what purity was high is higher than 99.7, and alumina content is lower than the preparation method of 0.05% Anhydrous Aluminium Chloride.
The objective of the invention is to realize through following technical scheme.
A kind of preparation method of Anhydrous Aluminium Chloride is characterized in that pure aluminum fluoride trihydrate and the matt salt of its preparation process operational analysis is raw material, and the step of preparation process comprises:
(1) aluminum fluoride trihydrate is carried out drying, obtain AlF
3H
2O;
(2) AlF that obtains of above-mentioned drying
3H
2Behind the O cool to room temperature, add matt salt and mix;
(3) mixture with step (2) carries out roasting system ALUMNIUM FLUORIDE.
The preparation method of a kind of Anhydrous Aluminium Chloride of the present invention, the drying temperature that the aluminum fluoride trihydrate that it is characterized in that step (1) carries out drying process is 110-260 ℃, be 6-16 hour time of drying.
The preparation method of a kind of Anhydrous Aluminium Chloride of the present invention is characterized in that the AlF that drying obtains in the step (2)
3H
2Behind the O cool to room temperature, the matt salt quality of adding is 1:20-1:12 with the minimum mass ratio of initial aluminum fluoride trihydrate.
The preparation method of a kind of Anhydrous Aluminium Chloride of the present invention; It is characterized in that mixture with step (3) carries out the process that roasting prepares ALUMNIUM FLUORIDE and in the crucible type electric furnace of sealing, carries out; And feed nitrogen or argon gas is protected; The temperature curve of roasting is following: room temperature-300 ℃, intensification 60-100 minute; 300-500 ℃, intensification 60-150 minute; 500-650 ℃, intensification 90-150 minute, be heated to 650 ℃ after naturally cooling.
The preparation method of a kind of Anhydrous Aluminium Chloride of the present invention is characterized in that the raw material of its preparation process is aluminum fluoride trihydrate and Neutral ammonium fluoride.
The preparation method of a kind of Anhydrous Aluminium Chloride of the present invention is characterized in that the AlF that drying obtains in the step (2)
3H
2Behind the O cool to room temperature, the quality and the initial aluminum fluoride trihydrate mass ratio that add Neutral ammonium fluoride are 1:15-1:8.
The preparation method of a kind of Anhydrous Aluminium Chloride of the present invention is a raw material with commercially available analytically pure aluminum fluoride trihydrate and matt salt (perhaps Neutral ammonium fluoride), prepares Anhydrous Aluminium Chloride through drying, adding matt salt (perhaps Neutral ammonium fluoride) and three steps of roasting.This method cost is lower, can prepare purity and be higher than 99.7%, and alumina content is lower than 0.05% Anhydrous Aluminium Chloride.
Embodiment
A kind of preparation method of Anhydrous Aluminium Chloride; Its preparation process is at first packed aluminum fluoride trihydrate reagent in the pallet into; Dry 8-16 is individual hour in 110-260 ℃ air dry oven, and this moment, aluminum fluoride trihydrate was sloughed most crystal water, had generated the compound (AlF that contains about 1 crystal water
3H
2O).Because drying temperature is lower than the hydrolysis temperature of ALUMNIUM FLUORIDE, in this process, can hydrolysis not generate aluminum oxide, guaranteed not generate in this process impurity.The rate of weight loss of this stage aluminum fluoride trihydrate is 20% ~ 26%.
Behind the ALUMNIUM FLUORIDE cool to room temperature that above-mentioned drying obtains; Adding matt salt mixes; The matt salt quality and the initial aluminum fluoride trihydrate mass ratio that add are 1:20-1:12, if add Neutral ammonium fluoride, then Neutral ammonium fluoride quality and initial aluminum fluoride trihydrate mass ratio are 1:15-1:8.The matt salt (perhaps Neutral ammonium fluoride) that adds decomposes in roasting process, generates hydrogen fluoride gas and ammonia, and the hydrogen fluoride gas of generation can effectively suppress the hydrolysis of ALUMNIUM FLUORIDE, prevents to generate aluminum oxide impurity.
After dried ALUMNIUM FLUORIDE and matt salt mix, place plumbago crucible, put into crucible type corundum boiler tube then, the corundum boiler tube is with stainless steel lid and the sealing of O type circle.Insert an alundum tube with tube stub on the stainless steel lid; When roasting begins, feed nitrogen or argon gas, get rid of the air in the boiler tube as far as possible, with the protection plumbago crucible through alundum tube; In roasting process, feed the nitrogen or the argon gas of low discharge; Make to keep malleation in the corundum boiler tube, prevent hydrochloric acid soln and sodium hydroxide solution, take away the crystal water of deviating from simultaneously.Insert a stainless steel tube with tube stub on the stainless steel lid, to get rid of the gas that produces in the roasting process.The gas that produces in the roasting process absorbs with hydrochloric acid soln and sodium hydroxide solution successively, to reclaim ammonia and hydrogen fluoride gas wherein.
The temperature curve of roasting is following: room temperature-300 ℃, intensification 60-100 minute; 300-500 ℃, intensification 60-150 minute; 500-650 ℃, intensification 90-150 minute.Naturally cooling after being heated to 650 ℃.
Embodiment 1
Get aluminum fluoride trihydrate 1500g, place in the stainless steel pallet, put into 130 ℃ air dry oven inner drying 16 hours, after the taking-up, be cooled to room temperature, add the 120g matt salt and mix, mixed material places to be put into High Temperature Furnaces Heating Apparatus behind the plumbago crucible and waits for roasting.The gas that produces in the roasting process absorbs with hydrochloric acid soln and sodium hydroxide solution successively.The temperature curve of roasting is following: room temperature ~ 300 ℃, heated up 90 minutes; 300 ~ 500 ℃, heated up 120 minutes; 500 ~ 650 ℃, heated up 120 minutes.
Embodiment 2
Get aluminum fluoride trihydrate 1500g, place in the stainless steel pallet, put into 170 ℃ air dry oven inner drying 12 hours, after the taking-up, be cooled to room temperature, add the 100g matt salt and mix, mixed material places to be put into High Temperature Furnaces Heating Apparatus behind the plumbago crucible and waits for roasting.The gas that produces in the roasting process absorbs with hydrochloric acid soln and sodium hydroxide solution successively.The temperature curve of roasting is following: room temperature ~ 300 ℃, heated up 70 minutes; 300 ~ 500 ℃, heated up 150 minutes; 500 ~ 650 ℃, heated up 90 minutes.
Embodiment 3
Get aluminum fluoride trihydrate 1500g, place in the stainless steel pallet, put into 250 ℃ air dry oven inner drying 6 hours, after the taking-up, be cooled to room temperature, add the 90g matt salt and mix, mixed material places to be put into High Temperature Furnaces Heating Apparatus behind the plumbago crucible and waits for roasting.The gas that produces in the roasting process absorbs with hydrochloric acid soln and sodium hydroxide solution successively.The temperature curve of roasting is following: room temperature ~ 300 ℃, heated up 100 minutes; 300 ~ 500 ℃, heated up 120 minutes; 500 ~ 650 ℃, heated up 120 minutes.
Embodiment 4
Get aluminum fluoride trihydrate 1500g, place in the stainless steel pallet, put into 230 ℃ air dry oven inner drying 8 hours, after the taking-up, be cooled to room temperature, add the 75g matt salt and mix, mixed material places to be put into High Temperature Furnaces Heating Apparatus behind the plumbago crucible and waits for roasting.The gas that produces in the roasting process absorbs with hydrochloric acid soln and sodium hydroxide solution successively.The temperature curve of roasting is following: room temperature ~ 300 ℃, heated up 70 minutes; 300 ~ 500 ℃, heated up 130 minutes; 500 ~ 650 ℃, heated up 150 minutes.
Embodiment 5
Get aluminum fluoride trihydrate 1500g, place in the stainless steel pallet, put into 230 ℃ air dry oven inner drying 8 hours, after the taking-up, be cooled to room temperature, add the 150g Neutral ammonium fluoride and mix, mixed material places to be put into High Temperature Furnaces Heating Apparatus behind the plumbago crucible and waits for roasting.The gas that produces in the roasting process absorbs with hydrochloric acid soln and sodium hydroxide solution successively.The temperature curve of roasting is following: room temperature ~ 300 ℃, heated up 60 minutes; 300 ~ 500 ℃, heated up 150 minutes; 500 ~ 650 ℃, heated up 150 minutes.
Claims (6)
1. the preparation method of an Anhydrous Aluminium Chloride is characterized in that pure aluminum fluoride trihydrate and the matt salt of its preparation process analysis is raw material, and the step of preparation process comprises:
(1) aluminum fluoride trihydrate is carried out drying, obtain AlF
3H
2O;
(2) AlF that obtains of above-mentioned drying
3H
2Behind the O cool to room temperature, add matt salt and mix;
(3) mixture with step (2) carries out roasting system ALUMNIUM FLUORIDE.
2. the preparation method of a kind of Anhydrous Aluminium Chloride according to claim 1, it is in air dry oven, to carry out that the aluminum fluoride trihydrate that it is characterized in that step (1) carries out drying process, and drying temperature is 110-260 ℃, and be 6-16 hour time of drying.
3. the preparation method of a kind of Anhydrous Aluminium Chloride according to claim 1 is characterized in that the AlF that drying obtains in the step (2)
3H
2Behind the O cool to room temperature, adding matt salt quality and initial aluminum fluoride trihydrate mass ratio is 1:20-1:12.
4. the preparation method of a kind of Anhydrous Aluminium Chloride according to claim 1; It is characterized in that mixture with step (3) carries out that roasting system ALUMNIUM FLUORIDE process feeds nitrogen or argon gas is protected; The temperature curve of roasting is following: room temperature-300 ℃, intensification 60-100 minute; 300-500 ℃, intensification 60-150 minute; 500-650 ℃, intensification 90-150 minute; Naturally cooling after being heated to 650 ℃.
5. the preparation method of a kind of Anhydrous Aluminium Chloride according to claim 1 is characterized in that the raw material of its preparation process is aluminum fluoride trihydrate and Neutral ammonium fluoride.
6. the preparation method of a kind of Anhydrous Aluminium Chloride according to claim 1 is characterized in that the AlF that drying obtains in the step (2)
3H
2Behind the O cool to room temperature, the quality and the initial aluminum fluoride trihydrate mass ratio that add Neutral ammonium fluoride are 1:15-1:8.
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|---|---|---|---|
| CN2011102218962A CN102390853A (en) | 2011-08-04 | 2011-08-04 | Preparation method for anhydrous aluminum fluoride |
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|---|---|---|---|
| CN2011102218962A CN102390853A (en) | 2011-08-04 | 2011-08-04 | Preparation method for anhydrous aluminum fluoride |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107233903A (en) * | 2017-05-18 | 2017-10-10 | 浙江工业大学 | A kind of mechanical mixture roasting preparation method and applications of aluminum fluoride catalyst |
| CN107827132A (en) * | 2017-11-23 | 2018-03-23 | 达州励志环保科技有限公司 | A kind of preparation method of aluminum fouoride |
| CN113501536A (en) * | 2021-07-28 | 2021-10-15 | 中南大学 | Method for preparing aluminum fluoride product by multi-waste combined treatment and aluminum fluoride product |
| CN114349034A (en) * | 2022-02-08 | 2022-04-15 | 东北大学 | Preparation method of anhydrous aluminum fluoride |
| CN114772627A (en) * | 2022-03-30 | 2022-07-22 | 蜂巢能源科技(无锡)有限公司 | Dehydration purification method and application of solid electrolyte |
| CN114988449A (en) * | 2022-06-18 | 2022-09-02 | 灵宝市民生高新材料有限公司 | Preparation method of low-oxygen-content anhydrous aluminum fluoride |
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|---|---|---|---|---|
| SU632652A1 (en) * | 1977-05-03 | 1978-11-15 | Предприятие П/Я А-7125 | Method of obtaining aluminium fluoride |
| CN101077786A (en) * | 2006-05-22 | 2007-11-28 | 多氟多化工股份有限公司 | Method for preparing aluminum fluoride |
| CN101134590A (en) * | 2006-09-01 | 2008-03-05 | 多氟多化工股份有限公司 | Method for producing aluminun fluoride with combined production of white carbon black and ammonia sulfate |
-
2011
- 2011-08-04 CN CN2011102218962A patent/CN102390853A/en active Pending
Patent Citations (3)
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|---|---|---|---|---|
| SU632652A1 (en) * | 1977-05-03 | 1978-11-15 | Предприятие П/Я А-7125 | Method of obtaining aluminium fluoride |
| CN101077786A (en) * | 2006-05-22 | 2007-11-28 | 多氟多化工股份有限公司 | Method for preparing aluminum fluoride |
| CN101134590A (en) * | 2006-09-01 | 2008-03-05 | 多氟多化工股份有限公司 | Method for producing aluminun fluoride with combined production of white carbon black and ammonia sulfate |
Non-Patent Citations (1)
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|---|
| 铁军等: "一种制备无水氟化铝的新方法", 《有色金属》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107233903A (en) * | 2017-05-18 | 2017-10-10 | 浙江工业大学 | A kind of mechanical mixture roasting preparation method and applications of aluminum fluoride catalyst |
| CN107233903B (en) * | 2017-05-18 | 2019-09-17 | 浙江工业大学 | A kind of mechanical mixture roasting preparation method and applications of aluminum fluoride catalyst |
| CN107827132A (en) * | 2017-11-23 | 2018-03-23 | 达州励志环保科技有限公司 | A kind of preparation method of aluminum fouoride |
| CN113501536A (en) * | 2021-07-28 | 2021-10-15 | 中南大学 | Method for preparing aluminum fluoride product by multi-waste combined treatment and aluminum fluoride product |
| CN114349034A (en) * | 2022-02-08 | 2022-04-15 | 东北大学 | Preparation method of anhydrous aluminum fluoride |
| CN114772627A (en) * | 2022-03-30 | 2022-07-22 | 蜂巢能源科技(无锡)有限公司 | Dehydration purification method and application of solid electrolyte |
| CN114772627B (en) * | 2022-03-30 | 2024-02-13 | 蜂巢能源科技(无锡)有限公司 | Dehydration purification method and application of solid electrolyte |
| CN114988449A (en) * | 2022-06-18 | 2022-09-02 | 灵宝市民生高新材料有限公司 | Preparation method of low-oxygen-content anhydrous aluminum fluoride |
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Application publication date: 20120328 |