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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- aluminum chloride
- anhydrous aluminum
- thionyl chloride
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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.
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| 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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| 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 |
| CN101155759A (en) * | 2005-04-04 | 2008-04-02 | 日本轻金属株式会社 | High-purity anhydrous aluminum 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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