CN104556156A - Preparation method of anhydrous magnesium chloride - Google Patents
Preparation method of anhydrous magnesium chloride Download PDFInfo
- Publication number
- CN104556156A CN104556156A CN201410833963.XA CN201410833963A CN104556156A CN 104556156 A CN104556156 A CN 104556156A CN 201410833963 A CN201410833963 A CN 201410833963A CN 104556156 A CN104556156 A CN 104556156A
- Authority
- CN
- China
- Prior art keywords
- magnesium chloride
- preparation
- dehydration
- socl
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/26—Magnesium halides
- C01F5/30—Chlorides
- C01F5/34—Dehydrating magnesium chloride containing water of crystallisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of anhydrous magnesium chloride. The method comprises the following steps: firstly, internally dehydrating magnesium chloride high hydrate under the protection of HCl gas, so as to obtain low hydrate, and then removing residual water through chemical reaction, so as to obtain the high-purity anhydrous magnesium chloride. The initial dehydrating temperature is low, so that the fact that the magnesium chloride is not hydrolyzed and the energy consumption is greatly reduced; a dehydrating agent adopted during the dehydrating in the chemical reaction is formed by the reaction of sulfur and chlorine, intermediate components are continuously recycled, the dehydrating in the chemical reaction ensures that the product anhydrous magnesium chloride is completely disengaged with water environment, and produced side reaction products SO2 and HCL are gases, so that the occurrence of hydrolysis reaction is thoroughly avoided. The method is wide in raw material resource and low in price, the whole technical process is good in economic benefit, and the method provided by the invention is high in operability and easy to realize industrialization.
Description
Technical field
The present invention relates to a kind of preparation method of magnesium compound, particularly relate to a kind of preparation method of Magnesium Chloride Anhydrous.
Background technology
Magnesium is one of the lightest structural metallic material, there is specific tenacity and specific rigidity is high, damping and amortization and machinability good, be easy to the advantages such as recovery, be widely used in automobile making, electronic product, space industry and military field etc.It is current development technique faster that electrolytic process prepares MAGNESIUM METAL, and its main raw material is Magnesium Chloride Anhydrous.Magnesium chloride hyperhydrate wide material sources, cheap, obtaining Magnesium Chloride Anhydrous by Dehydration will be a kind of desirable feedstock.For magnesium chloride hexahydrate, its dehydration preparing Magnesium Chloride Anhydrous is as follows:
MgCl
2·6H
2O＝MgCl
2·4H
2O+2H
2O↑
MgCl
2·4H
2O＝MgCl
2·2H
2O+2H
2O↑
MgCl
2·2H
2O＝MgCl
2·H
2O+H
2O↑
MgCl
2·H
2O＝MgCl
2+H
2O↑
Wherein easily there is hydrolysis reaction when the lower hydrate of magnesium chloride hexahydrate in dehydration:
MgCl
2·H
2O＝Mg(OH)Cl+HCl↑
Mg(OH)Cl＝MgO+HCl↑
The Thermal Decomposition Mechanism of being dewatered from magnesium chloride hexahydrate, MgC1
26H
2o takes off and is easier to low water, just can achieve the goal in warm air; But Magnesium chloride with low water dehydration is more difficult, during dehydration, part can be hydrolyzed.Because hydrolysis reaction generates magnesium oxide, product cannot meet the production requirement of electrolysis refining magnesium.What how to suppress hydrolysis reaction in dehydration is the key improving Magnesium Chloride Anhydrous purity.
Current magnesium chloride hexahydrate Dehydration mainly comprises following direction for the process study of Magnesium Chloride Anhydrous:
Protection thermal dehydration method, i.e. dehydration under chlorine or hydrogen chloride gas protection.This kind of method that patent CN1234608C, CN102275960B mainly adopt.At a certain temperature, maintain the concentration of chlorine or hydrogenchloride in heating systems, thus hydrolysis reaction during high temperature is reduced to minimum.Under HCl protective atmosphere dewatering process due to environmental pollution little, production process auto-control degree is high, therefore is relatively advanced dewatering.Dehydration can the generation of suppression hydrolysis reaction to a certain degree under protective gas; but in the industrial production; this kind of technique has certain limitation; need very high temperature, energy consumption larger in dehydration; and equipment seriously corroded under high temperature, part HC1 gas and water recovery are at MgC1
2on product, affect product quality.
Double salt method, first reacts by hydrated magnesium chloride and Repone K, ammonium chloride etc. to the Carnallite KClMgC1 making double salt structure
26H
2o, ammonium carnallite NH
4cIMgC1
26H
2o.Patent CN1326773C, CN1156398C, CN102491384B, CN 102491383B mainly adopt this method.Because the activity of magnesium chloride in carnallitite is less than the activity of magnesium chloride in hydrated magnesium chloride significantly, in dehydration, hydrolytic action obviously reduces, thus improves the quality of Magnesium Chloride Anhydrous.The dehydration proceed step by step of carnallitite, along with the rising of temperature, the water in carnallitite constantly loses, and last Magnesium Chloride Anhydrous.Due to the effect of double salt structure, make often to walk equilibrium vapor dividing potential drop in dehydration and, much larger than the equilibrium vapor partial pressure value of magnesium chloride hexahydrate, make dehydration more easily carry out and hydrolysis reaction not occur.This method partial oxidation when reclaiming ammonium chloride decomposes or hydrolysis generates corrosive hydrogenchloride, NH
4the trapping of CI dust, free NH
3recovery, improve NH
4the aspects such as the CI rate of recovery also exist a large amount of problem to be needed perfect.
Method of substitution, namely first uses ammonia, and alcohol equimolecular replaces MgC1
26H
2water molecules in O, forms MgC1
26NH
3, and then remove replacement molecule thus obtained Magnesium Chloride Anhydrous.Patent CN1043215C, CN101462746B mainly adopt this method.This method needs the alcoholic solution heating magnesium chloride in order to dewater, ammonia, alcoholic solution all partly can only replace water, to replace completely and need water molecules to need a large amount of alcohol, this not only consumes a large amount of energy, in heat-processed, solution can produce wax-like gathering simultaneously, make cannot being separated completely of magnesium chloride and alcohol, aforesaid method realizes industrialization as can be seen here a lot of difficulty.
Shortcoming for prior art is not enough, and this patent proposes to utilize a kind of technique adopting magnesium chloride hexahydrate to prepare high-purity anhydrous magnesium chloride.
Summary of the invention
When the technical problem that the present invention solves is to overcome and prepares Magnesium Chloride Anhydrous with magnesium chloride height hydrate in prior art, intermediate product Magnesium chloride with low water dewater difficult facile hydrolysis, be difficult to improve end product purity, the shortcoming such as power consumption, high cost, equipment are easily corroded, provide a kind of with low cost, technique simple and effectively suppress the generation of hydrolysis reaction in dehydration, improve the preparation method of Magnesium Chloride Anhydrous purity.
For solving the problems of the technologies described above, the present invention adopts following technical proposals:
A kind of preparation method of Magnesium Chloride Anhydrous; comprise physics heat up dehydration and chemical reaction dewater two stages; described physics intensification dehydration is under hci gas flow protection, slow intensification magnesium chloride hyperhydrate, tentatively removes part water and generates magnesium chloride lower hydrate MgC1
2xH
2the process of O; Described chemical reaction dehydration refers to the MgC1 of generation
2xH
2o generates the process of Magnesium Chloride Anhydrous under the effect of thionyl chloride.
Its concrete step of preparation process comprises:
1), under HCl air-flow protection, slow intensification magnesium chloride hyperhydrate, tentatively removes part water and generates magnesium chloride lower hydrate MgC1
2xH
2o;
2), by Cl
2with the S from follow-up rectification section
2cl
2mixing, makes S
2cl
2be converted into SCl
2;
3), by step 2) SCl of gained
2add in the reactor of jacketed, the SO returned with follow-up workshop section
2reactive Synthesis SOCl
2;
4), rectification step 3) product that obtains, be SOCl at the bottom of tower after rectifying
2, tower top is unreacted SCl
2;
5), by step 4) SOCl2 that obtains is passed into step 1) in the low hydrate MgC12xH2O of gained, chemical reaction dehydration occurs and obtains the high-pure anhydrous MgCl2 of product.
The Advantages found of this preparation technology can reclaim or recycle at the byproduct of reaction of each step of preparation technology, is embodied in:
1), step of preparation process 1) in carry steam secretly after dehydration HCl become byproduct hydrochloric acid through absorbing;
2), step of preparation process 4) in unreacted SCl
2s is obtained by S bed
2cl
2, turn back to step of preparation process 2) and middle participation conversion and cycle;
3), step of preparation process 5) the middle SO generated
2gas turns back to step 3) in conversion and cycle, the HCl gas of generation turns back to step 1) in as physics heat up dehydration shielding gas.
The significant parameter of each step of this preparation technology is:
In the lower hydrate MgC12xH2O that physics intensification dehydration obtains, the numerical range of x is 0.5<x<2.5, and dehydration temperaturre is 100 ~ 300 DEG C; S
2cl
2be converted into SCl
2temperature be 55 ~ 75 DEG C; SO
2reactive Synthesis SOCl
2temperature be 150 ~ 250 DEG C, temperature maintenance method passes into thermal cycling oil in the reactor of described jacketed; SOCl
2rectification temperature be 50 ~ 150 DEG C; SOCl
2with MgC1
2xH
2the temperature of reaction of O is 60 ~ 100 DEG C.
Adopt technique scheme, beneficial effect of the present invention is:
Magnesium chloride hyperhydrate is prepared high-purity anhydrous magnesium chloride and is adopted two step dehydrations, preliminary hydro-extraction removes part water under hci gas flow protection, dehydration temperaturre is lower than traditional snead process about 200 DEG C, while hydrolysis does not occur guarantee magnesium chloride, greatly reduce energy consumption; Final dewatering is chemical reaction dehydration, the SO that reaction generates
2, HCl is gas, make product Magnesium Chloride Anhydrous thoroughly depart from water environment, fundamentally avoid the generation of hydrolysis reaction, the gas simultaneously generated is easy to and Magnesium Chloride Anhydrous product separation; This raw materials technology wide material sources are cheap, and the chlorine that can consume the serious surplus of chlorine industry is translated into byproduct hydrochloric acid, in technical process, sulphur is with different shape recycle, and whole technical process is good in economic efficiency, the method strong operability provided, is easy to realize industrialization.
Accompanying drawing explanation
The process flow sheet of the method for preparation of anhydrous magnesium chloride that Fig. 1 provides for the embodiment of the present invention.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and the specific embodiments, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only for explaining the present invention, being not intended to limit the present invention.
Refer to Fig. 1, the process flow sheet of the preparation method of the Magnesium Chloride Anhydrous that Fig. 1 provides for the embodiment of the present invention, as can be seen from Fig. 1, the preparation method of Magnesium Chloride Anhydrous comprises the steps:
1) magnesium chloride hyperhydrate is carried out physics intensification dehydration, obtain magnesium chloride lower hydrate MgC1
2xH
2o;
Particularly, under HCl air-flow protection, magnesium chloride hyperhydrate is slowly heated up in fluidized-bed, tentatively remove part water and generate low hydrate MgC1
2xH
2o;
Preferably, magnesium chloride hyperhydrate is MgC1
26H
2o, can be understood as magnesium chloride hyperhydrate of the present invention is MgC1
26H
2o;
Wherein, in the lower hydrate MgC12xH2O obtained, the numerical range of x is 0.5<x<2.5;
Wherein, the temperature of physics intensification dehydration is 100 ~ 300 DEG C;
Wherein, the HCl carrying steam after dehydration secretly becomes byproduct hydrochloric acid through absorbing.
2) by Cl
2with S
2cl
2mixing, makes S
2cl
2conversion obtains SCl
2;
Particularly, under the condition of 55 ~ 75 DEG C, Cl is passed into
2with the S from follow-up rectification section
2cl
2mixing, makes it reaction by S
2cl
2change into SCl
2.
3) by SCl
2with SO
2mixing, reaction generates SOCl
2;
Particularly, under the condition of 150 ~ 250 DEG C, make step 2) SCl of gained
2the SO returned with follow-up workshop section
2reactive Synthesis SOCl
2;
Wherein, SCl
2with SO
2mixing generates SOCl
2reaction be carry out in the reactor of jacketed;
Wherein, SCl
2with SO
2mixing generates SOCl
2temperature of reaction maintenance method be pass into thermal cycling oil in the reactor of described jacketed.
4) rectifying SOCl
2,make it and unreacted SCl
2be separated;
Concrete, under the condition of 50 ~ 150 DEG C, by step 3) reaction product that obtains passes into rectifying tower and carries out rectifying, obtains SOCl at the bottom of tower
2, top gaseous phase light constituent is mainly SCl
2;
Wherein, tower top light constituent obtains S by S bed
2cl
2, turn back to step 2) and middle participation conversion and cycle;
5) SOCl
2with low hydrate MgC1
2xH
2o is obtained by reacting high-pure anhydrous MgCl
2;
Particularly, under the condition of 60 ~ 100 DEG C, by step 4) SOCl that obtains
2be passed into step 1) the low hydrate MgC1 of gained
2xH
2in O, there is chemical reaction dehydration and obtain the high-pure anhydrous MgCl of product
2;
Wherein, byproduct of reaction SO
2gas turns back to step 3) middle conversion and cycle;
Wherein, byproduct of reaction HCl gas turns back to step 1) in as magnesium chloride hyperhydrate physics heat up dehydration shielding gas.
Embodiment 1:
Under HCl air-flow protection, magnesium chloride hyperhydrate is slowly warming up to 100 DEG C in fluidized-bed, tentatively removes part water and generate low hydrate MgC1
2xH
2o; Cl is passed under the condition of 55 DEG C
2with the S from follow-up rectification section
2cl
2mixing, makes it reaction by S
2cl
2change into SCl
2; Under the condition of 150 DEG C, by the above-mentioned SCl be obtained by reacting
2the SO returned with follow-up workshop section
2reactive Synthesis SOCl
2; Under the condition of 50 DEG C, the reaction product that above-mentioned steps obtains is passed into rectifying tower and carries out rectifying, at the bottom of tower, obtain SOCl
2; Under the condition of 60 DEG C, by the SOCl obtained
2pass into the low hydrate MgC1 that physics biologically dehydrating obtains
2xH
2in O, there is chemical reaction dehydration and obtain the high-pure anhydrous MgCl of product
2.
Embodiment 2:
Under HCl air-flow protection, magnesium chloride hyperhydrate is slowly warming up to 200 DEG C in fluidized-bed, tentatively removes part water and generate low hydrate MgC1
2xH
2o; Cl is passed under the condition of 65 DEG C
2with the S from follow-up rectification section
2cl
2mixing, makes it reaction by S
2cl
2change into SCl
2; Under the condition of 200 DEG C, by the above-mentioned SCl be obtained by reacting
2the SO returned with follow-up workshop section
2reactive Synthesis SOCl
2; Under the condition of 100 DEG C, the reaction product that above-mentioned steps obtains is passed into rectifying tower and carries out rectifying, at the bottom of tower, obtain SOCl
2; Under the condition of 80 DEG C, by the SOCl obtained
2pass into the low hydrate MgC1 that physics biologically dehydrating obtains
2xH
2in O, there is chemical reaction dehydration and obtain the high-pure anhydrous MgCl of product
2.
Embodiment 3:
Under HCl air-flow protection, magnesium chloride hyperhydrate is slowly warming up to 300 DEG C in fluidized-bed, tentatively removes part water and generate low hydrate MgC1
2xH
2o; Cl is passed under the condition of 75 DEG C
2with the S from follow-up rectification section
2cl
2mixing, makes it reaction by S
2cl
2change into SCl
2; Under the condition of 250 DEG C, by the above-mentioned SCl be obtained by reacting
2the SO returned with follow-up workshop section
2reactive Synthesis SOCl
2; Under the condition of 150 DEG C, the reaction product that above-mentioned steps obtains is passed into rectifying tower and carries out rectifying, at the bottom of tower, obtain SOCl
2; Under the condition of 100 DEG C, by the SOCl obtained
2pass into the low hydrate MgC1 that physics biologically dehydrating obtains
2xH
2in O, there is chemical reaction dehydration and obtain the high-pure anhydrous MgCl of product
2.
Embodiment 4:
Under HCl air-flow protection, by MgC1
26H
2o is slowly warming up to 150 DEG C and keeps 10 minutes in fluidized-bed, and continue to be warming up to 250 DEG C and keep 20 minutes, dehydration generates low hydrate MgC1
22H
2o; By Cl
2with the S from follow-up rectification section
2cl
2mixing, control temperature is 60 DEG C, S
2cl
2be converted into SCl
2; The SCl of gained
2add in the reactor of jacketed, the SO returned with follow-up workshop section
2reactive Synthesis SOCl
2, pass into the heat that thermal cycling oil generates to derive reaction in reacting kettle jacketing, maintaining temperature of reaction is 200 DEG C; By the SOCl obtained
2with unreacted SCl
2carry out rectifying separation, rectification temperature is obtain SOCl at the bottom of 80 DEG C of towers
2, top gaseous phase light constituent is mainly SCl
2; The SOCl obtained
2be passed into the low hydrate MgC1 of physics intensification dehydration gained
22H
2in O, issue biochemical reaction 80 DEG C of conditions, dewatered and obtain the anhydrous MgCl that product purity is 99.6%
2.
Embodiment 5:
Under HCl air-flow protection, by MgC1
26H
2o is slowly warming up to 180 DEG C and keeps 20 minutes in fluidized-bed, and continue to be warming up to 250 DEG C and keep 30 minutes, dehydration generates low hydrate MgC1
2h
2o; By Cl
2with the S from follow-up rectification section
2cl
2mixing, control temperature is 70 DEG C, S
2cl
2be converted into SCl
2; The SCl of gained
2add in the reactor of jacketed, the SO returned with follow-up workshop section
2reactive Synthesis SOCl
2, pass into the heat that thermal cycling oil generates to derive reaction in reacting kettle jacketing, maintaining temperature of reaction is 180 DEG C; By the SOCl obtained
2with unreacted SCl
2carry out rectifying separation, rectification temperature is 70 DEG C, obtains SOCl at the bottom of tower
2, top gaseous phase light constituent is mainly SCl
2; By the SOCl obtained
2be passed into the low hydrate MgC1 that physics intensification dehydration obtains
2h
2in O, issue biochemical reaction 100 DEG C of conditions, dewatered and obtain the anhydrous MgCl that product purity is 99.8%
2.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to invention, although the present invention discloses as above with preferred embodiment, but be not intended to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, make a little change when the technology contents of above-mentioned announcement can be utilized or be modified to the Equivalent embodiments of equivalent variations, in every case be do not depart from technical solution of the present invention content, according to any simple modification that technical spirit of the present invention is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (9)
1. the preparation method of a Magnesium Chloride Anhydrous; comprise physics heat up dehydration and chemical reaction dewater two stages; it is characterized in that: described physics intensification dehydration is under hci gas flow protection, slow intensification magnesium chloride hyperhydrate, tentatively remove part water and generate magnesium chloride lower hydrate MgC1
2xH
2the process of O; Described chemical reaction dehydration refers to the MgC1 of generation
2xH
2o generates the process of Magnesium Chloride Anhydrous under the effect of thionyl chloride.
2. the preparation method of a kind of Magnesium Chloride Anhydrous according to claim 1, is characterized in that comprising following preparation technology:
1), under HCl air-flow protection, slow intensification magnesium chloride hyperhydrate, tentatively removes part water and generates magnesium chloride lower hydrate MgC1
2xH
2o;
2), by Cl
2with the S from follow-up rectification section
2cl
2mixing, makes S
2cl
2be converted into SCl
2;
3), by step 2) SCl of gained
2add in the reactor of jacketed, the SO returned with follow-up workshop section
2reactive Synthesis SOCl
2;
4), rectification step 3) product that obtains, be SOCl at the bottom of tower after rectifying
2, tower top is unreacted SCl
2;
5), by step 4) SOCl that obtains
2be passed into step 1) the low hydrate MgC1 of gained
2xH
2in O, there is chemical reaction dehydration and obtain the high-pure anhydrous MgCl of product
2.
3. the preparation method of a kind of Magnesium Chloride Anhydrous according to claim 2, is characterized in that the byproduct of reaction of each step of preparation technology can reclaim or recycle, comprising:
1), step of preparation process 1) in carry steam secretly after dehydration HCl become byproduct hydrochloric acid through absorbing;
2), step of preparation process 4) in unreacted SCl
2s is obtained by S bed
2cl
2, turn back to step of preparation process 2) and middle participation conversion and cycle;
3), step of preparation process 5) the middle SO generated
2gas turns back to step 3) in conversion and cycle, the HCl gas of generation turns back to step 1) in as physics heat up dehydration shielding gas.
4. the preparation method of a kind of Magnesium Chloride Anhydrous according to claim 1 and 2, is characterized in that, in lower hydrate MgC12xH2O, the numerical range of x is 0.5<x<2.5.
5. the preparation method of a kind of Magnesium Chloride Anhydrous according to claim 1 and 2, is characterized in that, the temperature of physics intensification dehydration is 100 ~ 300 DEG C.
6. the preparation method of a kind of Magnesium Chloride Anhydrous according to claim 2, is characterized in that, S
2cl
2be converted into SCl
2temperature be 55 ~ 75 DEG C.
7. the preparation method of a kind of Magnesium Chloride Anhydrous according to claim 2, is characterized in that, SO
2reactive Synthesis SOCl
2temperature be 150 ~ 250 DEG C, temperature maintenance method passes into thermal cycling oil in the reactor of described jacketed.
8. the preparation method of a kind of Magnesium Chloride Anhydrous according to claim 2, is characterized in that, SOCl
2rectification temperature be 50 ~ 150 DEG C.
9. the preparation method of a kind of Magnesium Chloride Anhydrous according to claim 2, is characterized in that, SOCl
2with MgC1
2xH
2the temperature of reaction of O is 60 ~ 100 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410833963.XA CN104556156B (en) | 2014-12-29 | 2014-12-29 | A kind of preparation method of anhydrous magnesium chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410833963.XA CN104556156B (en) | 2014-12-29 | 2014-12-29 | A kind of preparation method of anhydrous magnesium chloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104556156A true CN104556156A (en) | 2015-04-29 |
| CN104556156B CN104556156B (en) | 2017-04-05 |
Family
ID=53073361
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410833963.XA Active CN104556156B (en) | 2014-12-29 | 2014-12-29 | A kind of preparation method of anhydrous magnesium chloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104556156B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105386082A (en) * | 2015-11-06 | 2016-03-09 | 中国天辰工程有限公司 | Manufacturing method of magnesium metal |
| CN106673029A (en) * | 2017-03-07 | 2017-05-17 | 辽宁工程技术大学 | Method for producing high-purity anhydrous magnesium chloride by using bischofite |
| CN111115579A (en) * | 2020-01-12 | 2020-05-08 | 浙江博瑞电子科技有限公司 | Reactive ultrasonic rectification purification method for HCL electronic gas |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1132199A (en) * | 1995-03-25 | 1996-10-02 | 山东淄川双凤化工厂 | Method for prodn. of sulfoxide chloride |
| CN1613770A (en) * | 2004-07-24 | 2005-05-11 | 陈瑜 | Process for producing anhydrous magnesium chloride by microwave energy |
-
2014
- 2014-12-29 CN CN201410833963.XA patent/CN104556156B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1132199A (en) * | 1995-03-25 | 1996-10-02 | 山东淄川双凤化工厂 | Method for prodn. of sulfoxide chloride |
| CN1613770A (en) * | 2004-07-24 | 2005-05-11 | 陈瑜 | Process for producing anhydrous magnesium chloride by microwave energy |
Non-Patent Citations (1)
| Title |
|---|
| 张祥麟: "《无机化学（下册）》", 30 September 1983, 湖南教育出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105386082A (en) * | 2015-11-06 | 2016-03-09 | 中国天辰工程有限公司 | Manufacturing method of magnesium metal |
| CN106673029A (en) * | 2017-03-07 | 2017-05-17 | 辽宁工程技术大学 | Method for producing high-purity anhydrous magnesium chloride by using bischofite |
| CN111115579A (en) * | 2020-01-12 | 2020-05-08 | 浙江博瑞电子科技有限公司 | Reactive ultrasonic rectification purification method for HCL electronic gas |
| CN111115579B (en) * | 2020-01-12 | 2021-12-17 | 浙江博瑞电子科技有限公司 | Reactive ultrasonic rectification purification method for HCL electronic gas |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104556156B (en) | 2017-04-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106865500B (en) | A kind of cycle production process preparing hydrogen fluoride with fluosilicic acid | |
| CN103614576B (en) | Method for recycling germanium from germanium-containing glass | |
| CN103638688B (en) | A kind of recoverying and utilizing method synthesizing phosgene in n-butyl isocyanate thermo-optical reaction end gas | |
| CN103991882B (en) | The fluorine in phosphoric acid by wet process liquid phase is utilized to prepare the method for Potassium monofluoride | |
| CN104556156A (en) | Preparation method of anhydrous magnesium chloride | |
| CN103641748B (en) | A kind of recycle by-product hydrochloric acid prepares the method for methylsulphonic acid | |
| CN105645358A (en) | Method for preparing hydrogen fluoride from fluosilicic acid | |
| CN104164577B (en) | A kind of method of Ti recovery from the tail gas that rectifying germanium tetrachloride produces | |
| CN108163812B (en) | Preparation method of hydrogen fluoride and preparation method of hydrofluoric acid | |
| CN103382032A (en) | Preparation method for trichlorosilane from silicon tetrachloride | |
| CN101134590B (en) | Method for producing aluminun fluoride with combined production of white carbon black and ammonia sulfate | |
| CN101555028A (en) | Method for preparing high purity anhydrous magnesium chloride by gas-solid reaction | |
| CN107500319A (en) | A kind of preparation method of anhydrous magnesium chloride | |
| CN110041299A (en) | A kind of method that the continuous gas phase catalytic fluorination of fixed bed prepares fluorinated ethylene carbonate | |
| CN102923716A (en) | Process for producing trichlorosilane through inverse disporportionation of dichlorosilane | |
| CN204779413U (en) | Production perchlorethylene's reaction gas processing system | |
| CN105386082B (en) | A kind of preparation method of magnesium metal | |
| CN104671270A (en) | Anhydrous aluminum chloride preparation method | |
| CN112551531A (en) | Method for coproducing hydrogen fluoride, white carbon black and potassium sulfate | |
| CN108033472A (en) | A kind of electrode foil produces spent acid Zero-discharge treating process | |
| CN106829876A (en) | The recoverying and utilizing method of oil plant sulfur removal plant sulphur steam | |
| CN104150517B (en) | The useless comprehensive utilization production method of a kind of process two | |
| CN102766017A (en) | Preparation method of tetrachloro-1,2-difluoroethane | |
| CN102145903A (en) | Method for preparing anhydrous magnesium chloride for electrolyzing magnesium | |
| CN102030332B (en) | Application of byproducts in preparation of silane through magnesium silicide process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |