CN103708518B - Anhydrous aluminum chloride preparation method - Google Patents
Anhydrous aluminum chloride preparation method Download PDFInfo
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- CN103708518B CN103708518B CN201210372972.4A CN201210372972A CN103708518B CN 103708518 B CN103708518 B CN 103708518B CN 201210372972 A CN201210372972 A CN 201210372972A CN 103708518 B CN103708518 B CN 103708518B
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- chloride
- aluminum chloride
- anhydrous aluminum
- thionyl chloride
- gas
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- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 title claims abstract description 127
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007789 gas Substances 0.000 claims abstract description 26
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 238000002425 crystallisation Methods 0.000 claims abstract description 19
- 230000008025 crystallization Effects 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000012065 filter cake Substances 0.000 claims abstract description 7
- 230000018044 dehydration Effects 0.000 claims abstract description 6
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000004806 packaging method and process Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 239000006227 byproduct Substances 0.000 claims abstract description 3
- 238000005516 engineering process Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 5
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 4
- 239000006096 absorbing agent Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 4
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 210000003298 dental enamel Anatomy 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002826 coolant Substances 0.000 claims description 2
- 238000007667 floating Methods 0.000 claims description 2
- 239000003595 mist Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000004781 supercooling Methods 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 229940063656 aluminum chloride Drugs 0.000 abstract 5
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 abstract 2
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 abstract 2
- 239000013078 crystal Substances 0.000 abstract 2
- 238000004064 recycling Methods 0.000 abstract 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- 229910052782 aluminium Inorganic materials 0.000 description 9
- 239000004411 aluminium Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000005868 electrolysis reaction Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- SOZVEOGRIFZGRO-UHFFFAOYSA-N [Li].ClS(Cl)=O Chemical compound [Li].ClS(Cl)=O SOZVEOGRIFZGRO-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000013032 Hydrocarbon resin Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 239000002168 alkylating agent Substances 0.000 description 1
- 229940100198 alkylating agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012320 chlorinating reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920006270 hydrocarbon resin Polymers 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses an anhydrous aluminum chloride preparation method. The method comprises the following steps: respectively adding an aluminum chloride hexahydrate crystal solid and liquid thionyl chloride into a dehydration reactor as raw materials under normal pressure or a tiny negative pressure at a temperature of below 76DEG C; carrying out a reaction of crystallization water and thionyl chloride to generate a sulfur dioxide gas and a hydrogen chloride gas, and converting aluminum chloride hexahydrate crystals into anhydrous aluminum chloride; filtering a slurry, recycling the obtained filtered filtrate-thionyl chloride, distilling the filtered anhydrous aluminum chloride filter cake in a distiller to obtain purified anhydrous aluminum chloride, packaging the finished anhydrous aluminum chloride, and storing; and cooling the distilled thionyl chloride gas, recycling the cooled thionyl chloride gas as a raw material, and carrying out absorbing treatment of a reaction byproduct hydrogen chloride-and-sulfur dioxide mixed gas. The method has the characteristics of cheap and easily available raw materials, simple flow, less energy consumption, easy industrial large-scale production and the like.
Description
Technical field
The present invention relates to a kind of anhydrous Aluminum chloride preparation method, belong to anhydrous chlorides of rase salt preparation field, be particularly useful for the preparation that aluminium chloride fused salt electrolysis process produces anhydrous Aluminum chloride in metallic aluminium, be applicable to six water crystallization aluminium chloride that petrochemical industry reclaims simultaneously and regenerate and prepare anhydrous Aluminum chloride.
Background technology
Anhydrous Aluminum chloride, molecular formula AlCl
3, English name Aluminum trichloride, density 2.44, sour corrosion product risk markings 20.Anhydrous Aluminum chloride is one of a kind of important inorganic chemical product, mainly for the manufacture of the alkylating agent of washing agent, organic catalyst compound, hydrocarbon resin, titanium dioxide nucleator, dyestuff intermediate and cosmetics and medicine etc.Simultaneously anhydrous Aluminum chloride is also a kind of very important catalyst, particularly as Fei Ruide-gram Lay Ford reaction catalyst and be able to extensive use.In addition, pure anhydrous Aluminum chloride is analyzed also as lithium-thionyl chloride battery (Li/SOCl
2) the anhydrous tetrachloro-lithium aluminate (LiAlCl of electrolyte
4) important raw materials for production.Anhydrous Aluminum chloride is mainly used for electrolysis aluminium in recent years, and the great advantage of aluminium chloride electrolysis aluminium is energy consumption low (9000 ~ 10000KWh/t), and anode does not consume, and chlorine also can be accomplished to recycle.
The present inventor searches out one by years of researches and to dewater by force material-thionyl chloride, another name: thionyl chloride, molecular formula: SOCl
2, English name: sulfurous oxychloride, fusing point :-104.5 DEG C, boiling point: 76 DEG C, density: 1.630-1.650t/m
3, colourless or faint yellow fuming liquids, has strong and stimulating smell.Chance water or alcohol resolve into sulfur dioxide and hydrogen chloride.Thionyl chloride is mainly used in medicine, agricultural chemicals, dye industry and organic synthesis industry, is also used as chlorinating agent lithium-thionyl chloride (Li/SOCl
2) battery.
From the report of document and patent, current anhydrous Aluminum chloride preparation mainly contains following several technology.
One is aluminium ingot method, namely adopts chlorine directly by motlten metal aluminium, and make both directly contact and produce, its reaction equation is:
, the feature of aluminium ingot method is that technological process is simple, and equipment is few, invests low, but owing to adopting metallic aluminium to make production cost higher as raw material.
Another kind is alumdum method, namely adopts aluminium oxide, chlorine and carbon as raw material, and at a certain temperature, three jointly reacts and produces, and its reaction equation is:
, wherein m+2n=3.The feature of alumdum method is that cost of material is low, but the anhydrous Aluminum chloride purity produced is low, often needs sublimed method to refine and just can obtain the high anhydrous Aluminum chloride of purity.
In addition, there is patent to propose to adopt unitary and polyalcohols (C1 ~ C4) to remove the crystallization water in six water crystallization aluminium chloride, but have no actual production report.
For the deficiency of current anhydrous Aluminum chloride technology of preparing, the present invention searches out a kind of material-thionyl chloride that can remove molecular crystalline water through research for many years, and according to thionyl chloride, this proposes a kind of six water crystallization aluminium chloride and prepares anhydrous chlorides of rase aluminum technology.
Summary of the invention
object of the present inventionbe to provide that a kind of raw material is cheap and easy to get, flow process simple, be easy to the anhydrous Aluminum chloride technology of preparing that maximizes.
technical scheme of the present invention is as follows: a kind of anhydrous Aluminum chloride preparation method, six water crystallization aluminum chloride solids and liquid thionyl chloride, as raw material, join in dehydration reactor by six water crystallization aluminium chloride and thionyl chloride respectively, and pressure is normal pressure or tiny structure, temperature <76 DEG C; The crystallization water and thionyl chloride react and generate sulfur dioxide gas and hydrogen chloride gas, and six water crystallization aluminium chloride change anhydrous Aluminum chloride into; Filtered by slurries, the filtrate-thionyl chloride after filtration returns use, and the anhydrous Aluminum chloride filter cake after filtration distills in distiller, obtains pure anhydrous Aluminum chloride, stores after finished product anhydrous Aluminum chloride packaging; The thionyl chloride gas distilled out returns use as raw material after supercooling, and byproduct of reaction hydrogen chloride and sulfur dioxide mixture gas are through absorbing process.
Described charge proportion is thionyl chloride: six water crystallization aluminium chloride >3:1,
What described dehydration reactor adopted is chuck glass lined stirring reactor, and heat medium is steam or conduction oil.
What described slurries filtered employing is centrifugal separation technology or vacuum filtration technology, controls filter cake attached liquid rate <5%, filtrate floating material content <10g/L.
Described distillation is carried out in enamel distiller, and heat medium is steam or conduction oil.
Described distillation condition is temperature is < 180 DEG C, and pressure is≤0.25MPa(G).
The described thionyl chloride gas distilled out cools in water cooling tower, and cooling medium is liquid thionyl chloride, liquid thionyl chloride temperature < 70 DEG C.
Described mist adopts air-introduced machine to extract out, and adopt the first absorbing hydrogen chloride gas of 2 ~ 4 countercurrent absorbers, absorbing liquid is water or solution of sodium bisulfite; Adopt 2 ~ 4 countercurrent absorber sulfur dioxide absorption gases again, absorbing liquid is water or soda lye.
beneficial effect of the present invention:
Compared with prior art, the technology that the present invention adopts has that raw material is cheap and easy to get, flow process is simple, energy resource consumption is few, be easy to the features such as industrial large-sizedization production.Because These characteristics the present invention is particularly useful for the preparation that aluminium chloride fused salt electrolysis process produces anhydrous Aluminum chloride in metallic aluminium, be applicable to six water crystallization aluminium chloride that petrochemical industry reclaims simultaneously and regenerate and prepare anhydrous Aluminum chloride.
Accompanying drawing explanation
Fig. 1 adopts water as absorbing liquid anhydrous Aluminum chloride preparation flow figure;
Fig. 2 adopts caustic soda as absorbing liquid anhydrous Aluminum chloride preparation flow figure.
Detailed description of the invention
Embodiments of the invention: adopt chuck glass lined stirring reactor, take steam as heat medium, quantitative spiral conveyor is adopted slowly to add in liquid thionyl chloride by six water crystallization aluminum chloride solids, control dehydration condition: material rate is thionyl chloride: six water crystallization aluminium chloride=4:1, pressure are 80KPa(absolute pressure), temperature is 50 DEG C, the sulfur dioxide gas that reaction generates and hydrogen chloride gas are extracted to after-treatment system.Adopt centrifuge to filter after six water crystallization aluminium chloride change anhydrous Aluminum chloride into, the filtrate after filtration uses as spray liquid, and the anhydrous Aluminum chloride filter cake obtained is transported to enamel distiller, and filter cake moisture content is about 3%.Adopt Steam Heating that anhydrous Aluminum chloride is heated to 100 DEG C, attached liquid thionyl chloride is distilled, and the gas after distillation send chuck glass lined stirring reactor after adopting liquid thionyl chloride spraying cooling to absorb, and stores after the anhydrous Aluminum chloride obtained packaging after distillation.Enter the hydrogen chloride of after-treatment system and sulfur dioxide mixture gas through 3 stage countercurrent absorption towers first absorbing hydrogen chloride gases, absorbing liquid is solution of sodium bisulfite; Again through 3 stage countercurrent absorption tower sulfur dioxide absorption gases, absorbing liquid soda lye, the solution of sodium bisulfite obtained after absorption is as the absorbing liquid of hydrogen chloride gas.
Claims (8)
1. an anhydrous Aluminum chloride preparation method, it is characterized in that: adopt six water crystallization aluminium chloride and thionyl chloride as raw material, six water crystallization aluminum chloride solids and liquid thionyl chloride are joined respectively in dehydration reactor, pressure is normal pressure or tiny structure, temperature <76 DEG C; The crystallization water and thionyl chloride react and generate sulfur dioxide gas and hydrogen chloride gas, and six water crystallization aluminium chloride change anhydrous Aluminum chloride into; Filtered by slurries, the filtrate-thionyl chloride after filtration returns use, and the anhydrous Aluminum chloride filter cake after filtration distills in distiller, obtains pure anhydrous Aluminum chloride, stores after finished product anhydrous Aluminum chloride packaging; The thionyl chloride gas distilled out returns use as raw material after supercooling, and byproduct of reaction hydrogen chloride and sulfur dioxide mixture gas are through absorbing process.
2. a kind of anhydrous Aluminum chloride preparation method according to claim 1, is characterized in that: charge proportion is thionyl chloride: six water crystallization aluminium chloride >3:1.
3. a kind of anhydrous Aluminum chloride preparation method according to claim 1, is characterized in that: what dehydration reactor adopted is chuck glass lined stirring reactor, and heat medium is steam or conduction oil.
4. a kind of anhydrous Aluminum chloride preparation method according to claim 1, it is characterized in that: what slurries filtered employing is centrifugal separation technology or vacuum filtration technology, control filter cake attached liquid rate <5%, filtrate floating material content <10g/L.
5. a kind of anhydrous Aluminum chloride preparation method according to claim 1, is characterized in that: distill and carry out in enamel distiller, and heat medium is steam or conduction oil.
6. a kind of anhydrous Aluminum chloride preparation method according to claim 1, is characterized in that: distillation condition is temperature is < 180 DEG C, and pressure is≤0.25MPa(G).
7. a kind of anhydrous Aluminum chloride preparation method according to claim 1, it is characterized in that: the thionyl chloride gas distilled out cools in water cooling tower, cooling medium is liquid thionyl chloride, liquid thionyl chloride temperature < 70 DEG C.
8. a kind of anhydrous Aluminum chloride preparation method according to claim 1, is characterized in that: mist adopts air-introduced machine to extract out, and adopt the first absorbing hydrogen chloride gas of 2 ~ 4 countercurrent absorbers, absorbing liquid is water or solution of sodium bisulfite; Adopt 2 ~ 4 countercurrent absorber sulfur dioxide absorption gases again, absorbing liquid is water or soda lye.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210372972.4A CN103708518B (en) | 2012-09-29 | 2012-09-29 | Anhydrous aluminum chloride preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210372972.4A CN103708518B (en) | 2012-09-29 | 2012-09-29 | Anhydrous aluminum chloride preparation method |
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| Publication Number | Publication Date |
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| CN103708518A CN103708518A (en) | 2014-04-09 |
| CN103708518B true CN103708518B (en) | 2015-04-29 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105776294B (en) * | 2016-04-06 | 2018-01-30 | 衢州信步化工科技有限公司 | A kind of energy-efficient alchlor production method |
| CN110484289A (en) * | 2019-09-24 | 2019-11-22 | 济宁黑猫炭黑有限责任公司 | A kind of tar negative pressure dewatering system and method |
| CN112408443A (en) * | 2020-11-20 | 2021-02-26 | 衡阳鸿宇化工有限责任公司 | Preparation method of anhydrous aluminum trichloride |
| CN113941227A (en) * | 2021-11-26 | 2022-01-18 | 西安西热水务环保有限公司 | Method and system for selectively removing HCl in flue gas |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP3528424B2 (en) * | 1996-05-09 | 2004-05-17 | 日本軽金属株式会社 | Method for producing high-purity anhydrous aluminum chloride |
| CN1209290C (en) * | 2002-09-10 | 2005-07-06 | 章浩龙 | Method of preparing anhydrous aluminium chloride |
| CN1683247A (en) * | 2005-03-14 | 2005-10-19 | 章浩龙 | Process for producing anhydrous aluminium chloride |
| US20090028766A1 (en) * | 2005-04-04 | 2009-01-29 | Nippon Light Metal Company, Ltd. | High Purity Anhydrous Aluminium Chloride and Process for Production Thereof |
| CN101311118A (en) * | 2007-05-21 | 2008-11-26 | 杨风春 | Aluminum trichloride (anhydrous) sublimation purification and preparation method |
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