CN102718784A - Decomplexation method of metal organic compound and ether complex - Google Patents

Decomplexation method of metal organic compound and ether complex Download PDF

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Publication number
CN102718784A
CN102718784A CN2012102326571A CN201210232657A CN102718784A CN 102718784 A CN102718784 A CN 102718784A CN 2012102326571 A CN2012102326571 A CN 2012102326571A CN 201210232657 A CN201210232657 A CN 201210232657A CN 102718784 A CN102718784 A CN 102718784A
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separate
still
join
ether
joining
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CN102718784B (en
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朱世会
朱刘
朱世明
刘留
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Kunming Forerunner New Material Technology Co ltd
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First Rare Materials Co Ltd
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Abstract

The invention provides a method for decomplexing a metal organic compound and an ether complex, which comprises the following steps: putting a raw material into a decomplexation kettle filled with inert gas, wherein the raw material contains a complex of an MO source and diethyl ether; adding a ligand substance selected from amine compounds or high polyether into a decomplexation kettle under the condition of stirring; after the ligand substance is added, a displacement reaction is carried out to obtain a ligand substance and MO source complex; evaporating ether formed by the displacement reaction of the decomplexation kettle, and condensing and recovering the ether; evaporating and condensing the unreacted MO source and ether complex in the decomplexation kettle for recycling; the ligand substance in the decomplexation kettle is decomplexed with the MO source complex, the ligand substance obtained after decomplexation is left in the decomplexation kettle, and the MO source overflows in a gaseous form and is condensed and recovered; evaporating and condensing the ligand substance left in the decomplexation kettle after decomplexation and recovering. The decomplexation method can simplify the process and is easy to control, the raw materials are easy to obtain, the recovery rate is high, the product purity is high, and the method is very suitable for large-scale industrial production.

Description

Organometallics and etherate separate method of completing the square
Technical field
Present method relates to a kind of method of completing the square of separating of title complex, relates in particular to the method for completing the square of separating of metallorganics and etherate.
Background technology
Compound semiconductor ultra-thin film material is the elementary sources material of preparation novel photoelectric compound semiconductor material, is widely used in metal organic chemical vapor deposition technology and the metal organic molecular beam epitaxy technology such as (being called for short MOMBE).Trimethyl-gallium, trimethylaluminium, trimethyl indium (MO source) are the major metal sources of making the photoelectricity compound semiconductor materials.
Although industry has certain research to preparation MO source, the purity in MO source is its high-quality key.On the method for purifying, await thus improving.
Summary of the invention
In view of the deficiency of prior art, the invention provides the method for completing the square of separating of a kind of organometallics and etherate, it can be simplified technology and be easy to control.
In order to realize the object of the invention, the present invention provides the method for completing the square of separating of a kind of organometallics and etherate, comprises step: step 1: raw material is placed be full of separating of rare gas element and join still, said raw material contains the title complex of MO source and ether; The part thing that under agitation condition, will be selected from aminated compounds or high polyethers adds to separate joins in the still; Add after the part thing, replacement(metathesis)reaction takes place, to obtain part thing and MO source title complex; Steam and condensing and recycling separating the ether of joining the formation of still replacement(metathesis)reaction; Step 2: will separate the title complex evaporation and the condensing and recycling of joining unreacted MO source and ether in the still; Step 3: will separate the part thing of joining in the still and MO source title complex and separate and join, and separate the part thing that obtains after joining and stay to separate and join in the still, MO overflows with gaseous form in the source, and condensing and recycling; Step 4: staying of Xie Peihou separated the part thing of joining in the still evaporate also condensing and recycling.
Beneficial effect of the present invention is following.
Organometallics provided by the invention and etherate separate method of completing the square, it can be simplified technology and be easy to control, raw material be easy to get and the recovery high, product purity is high, is fit to very much large-scale industrial production.
Embodiment
The method of completing the square of separating according to metallorganics of the present invention and etherate at first is described.
The method of completing the square of separating according to organometallics of the present invention and etherate comprises step: step 1: raw material is placed be full of separating of rare gas element and join still, said raw material contains the title complex of MO source and ether; The part thing that under agitation condition, will be selected from aminated compounds or high polyethers adds to separate joins in the still; Add after the part thing, replacement(metathesis)reaction takes place, to obtain part thing and MO source title complex; Steam and condensing and recycling separating the ether of joining the formation of still replacement(metathesis)reaction; Step 2: will separate the title complex evaporation and the condensing and recycling of joining unreacted MO source and ether in the still; Step 3: will separate the part thing of joining in the still and MO source title complex and separate and join, and separate the part thing that obtains after joining and stay to separate and join in the still, MO overflows with gaseous form in the source, and condensing and recycling; Step 4: staying of Xie Peihou separated the part thing of joining in the still evaporate also condensing and recycling.
According to the separating in the method for completing the square of organometallics of the present invention and etherate, preferably, said rare gas element is nitrogen, argon gas or helium.
According to the separating in the method for completing the square of organometallics of the present invention and etherate, preferably, said MO source is trimethyl-gallium or trimethylaluminium or trimethyl indium; Said aminated compounds is tri-n-butylamine, quadrol, Diisopropylamine; Said high polyethers is NHD (CH 3O (CH 2CH 2O) nCH 3, n=3 ~ 8).
According to the separating in the method for completing the square of organometallics of the present invention and etherate, preferably, also comprise intermediate steps: after step 2 and before step 3, will separate and join unreacted part thing evaporation and condensing and recycling in the still.
According to the separating in the method for completing the square of organometallics of the present invention and etherate, preferably, also comprise step: after step 4, repeating step three and step 4 are at least once.
Separating in the method for completing the square according to organometallics of the present invention and etherate; Preferably; In step 1, with separate join ether that the still replacement(metathesis)reaction forms when steaming temperature be 50 ~ 80 ℃ and pressure be normal pressure or temperature be 50 ~ 80 ℃ down and vacuum tightness be 50 ~ 70KPa.
According to the separating in the method for completing the square of organometallics of the present invention and etherate, preferably, in step 2, temperature is that 60 ~ 80 ℃, vacuum tightness are 0.8 ~ 3KPa when separating the title complex evaporation of joining unreacted MO source and ether in the still.
According to the separating in the method for completing the square of organometallics of the present invention and etherate, preferably, in step 3, to separate the timing temperature be that 130 ~ 170 ℃, vacuum tightness are 7 ~ 20KPa with separating the part thing of joining in the still and MO source title complex.
According to the separating in the method for completing the square of organometallics of the present invention and etherate, preferably, in step 4, temperature was that 60 ~ 90 ℃, vacuum tightness are 0.7 ~ 1KPa when staying of Xie Peihou separated the part thing of joining in the still and evaporated.
According to the separating in the method for completing the square of organometallics of the present invention and etherate, preferably, in said intermediate steps, will separate when joining in the still unreacted part thing evaporation temperature and be 80 ℃, vacuum tightness is 0.7KPa.
Secondly explanation is according to the embodiment that separates method of completing the square of organometallics of the present invention and etherate.
Embodiment 1
Join the title complex that adds 1470g ether and trimethyl-gallium in the still toward being full of separating of nitrogen, under agitation condition, progressively add the 1620g tri-n-butylamine, be warming up to 70 ℃, vacuumize and be decompressed to 60KPa, evaporative condenser is recovered to the 270g ether;
To separate and join still and be warming up to 80 ℃, and vacuumize and be decompressed to 1KPa, evaporative condenser is recovered to the title complex of 300g ether and trimethyl-gallium;
To separate and join still and be warming up to 150 ℃, and be evacuated to and be 20KPa, trimethyl-gallium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 600g trimethyl-gallium;
Reduce to 80 ℃ with separating the temperature of joining still, be evacuated to 0.7KPa, evaporative condenser is recovered to the 1000g tri-n-butylamine;
To separate and join still and be warming up to 150 ℃, be evacuated to 20KPa, trimethyl-gallium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 240g trimethyl-gallium;
Reduce to 80 ℃ with separating the temperature of joining still, be evacuated to 0.7KPa, evaporative condenser is recovered to the 600g tri-n-butylamine.
Embodiment 2
Join the title complex that adds 1470g ether and trimethyl-gallium in the still toward being full of separating of nitrogen, under agitation condition, progressively add the 1620g quadrol, be warming up to 70 ℃, evaporative condenser is recovered to the 220g ether under the normal pressure;
To separate and join still and be warming up to 80 ℃, and vacuumize and be decompressed to 1KPa, evaporative condenser is recovered to the title complex of 330g ether and trimethyl-gallium;
To separate and join still and be warming up to 150 ℃, be evacuated to 20KPa, trimethyl-gallium separate join that the back is overflowed with gaseous form and in holding tank condensation and collection to the 590g trimethyl-gallium;
Reduce to 80 ℃ with separating the temperature of joining still, be evacuated to 0.8KPa, evaporative condenser reclaims the 1000g quadrol;
To separate and join still and be warming up to 150 ℃, and be evacuated to and be 20KPa, trimethyl-gallium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 200g trimethyl-gallium;
Reduce to 80 ℃ with separating the temperature of joining still, be evacuated to 0.7KPa, evaporative condenser is recovered to the 600g quadrol.
Embodiment 3
Join the title complex that adds 1250g ether and trimethylaluminium in the still toward being full of separating of argon gas, under agitation condition, progressively add the 1600g tri-n-butylamine, be warming up to 80 ℃, evaporative condenser is recovered to the 300g ether under the normal pressure;
To separate and join still and remain on 80 ℃, and vacuumize and be decompressed to the title complex that 2KPa and evaporative condenser are recovered to 260g ether and trimethylaluminium;
To separate and join still and be warming up to 160 ℃, and be evacuated to and be 15KPa, trimethylaluminium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 460g trimethylaluminium;
Reduce to 80 ℃ with separating the temperature of joining still, be evacuated to 0.7KPa, evaporative condenser is recovered to the 1100g tri-n-butylamine;
To separate and join still and be warming up to 170 ℃, and be evacuated to and be 10KPa, trimethylaluminium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 200g trimethylaluminium;
Reduce to 70 ℃ with separating the temperature of joining still, be evacuated to 0.8KPa, evaporative condenser is recovered to the 450g tri-n-butylamine.
Embodiment 4
Join the title complex that adds 1530g ether and trimethyl indium in the still toward being full of separating of helium, under agitation condition, progressively add the 1800g tri-n-butylamine, be warming up to 50 ℃, after normal pressure evaporates down and reclaims the 300g ether;
To separate and join still and be warming up to 80 ℃, and vacuumize and be decompressed to 1KPa, evaporative condenser is recovered to the title complex of 300g ether and trimethyl indium;
Remain on 80 ℃ with separating the temperature of joining still, be evacuated to 0.7KPa, the 230g tri-n-butylamine is reclaimed in evaporation.
To separate and join still and be warming up to 160 ℃, and be evacuated to and be 15KPa, trimethyl indium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 600g trimethyl indium;
Reduce to 80 ℃ with separating the temperature of joining still, be evacuated to 0.9KPa, evaporative condenser is recovered to the 920g tri-n-butylamine;
To separate and join still and be warming up to 170 ℃, and be evacuated to and be 10KPa, trimethyl indium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 130g trimethyl indium;
Reduce to 60 ℃ with separating the temperature of joining still, be evacuated to 1.0KPa, evaporative condenser is recovered to the 620g tri-n-butylamine.
Embodiment 5
Join the title complex that adds 1470g ether and trimethyl-gallium in the still toward being full of separating of argon gas, under agitation condition, progressively add the 1700g quadrol, be warming up to 80 ℃, vacuumize and be decompressed to 60KPa, evaporative condenser is recovered to the 270g ether;
To separate and join still and remain on 80 ℃, and vacuumize and be decompressed to 3KPa, evaporative condenser is recovered to the title complex of 280g ether and trimethyl-gallium;
To separate and join still and be warming up to 150 ℃, and be evacuated to and be 20KPa, trimethyl-gallium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 530g trimethyl-gallium;
Reduce to 60 ℃ with separating the temperature of joining still, be evacuated to 1KPa, evaporative condenser is recovered to the 1100g quadrol;
To separate and join still and be warming up to 150 ℃, and be evacuated to and be 20KPa, trimethyl-gallium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 180g trimethyl-gallium;
Reduce to 70 ℃ with separating the temperature of joining still, be evacuated to 0.7KPa, evaporative condenser is recovered to the 580g quadrol.
Embodiment 6
Join the title complex that adds 1470g ether and trimethyl-gallium in the still toward being full of separating of helium, under agitation condition, progressively add the 1700g Diisopropylamine, be warming up to 50 ℃, vacuumize and be decompressed to 60KPa, evaporative condenser is recovered to the 250g ether;
To separate and join still and be warming up to 60 ℃, and vacuumize and be decompressed to 3KPa, evaporation is recovered to the title complex of 300g ether and trimethyl-gallium;
To separate and join still and be warming up to 130 ℃, and be evacuated to and be 20KPa, trimethyl-gallium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 450g trimethyl-gallium;
Reduce to 60 ℃ with separating the temperature of joining still, be evacuated to 1KPa, evaporative condenser is recovered to the 1120g Diisopropylamine;
To separate and join still and be warming up to 140 ℃, and be evacuated to and be 10KPa, trimethyl-gallium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 190g trimethyl-gallium;
Reduce to 70 ℃ with separating the temperature of joining still, be evacuated to 0.7KPa, evaporative condenser is recovered to the 540g Diisopropylamine.
Embodiment 7
Join the title complex that adds 1470g ether and trimethyl-gallium in the still toward being full of separating of nitrogen, under agitation condition, progressively add 1700g NHD (CH 3O (CH 2CH 2O) nCH 3, n=4), be warming up to 60 ℃, vacuumize and be decompressed to 70KPa, evaporative condenser is recovered to the 280g ether;
To separate and join still and be warming up to 70 ℃, and vacuumize and be decompressed to 0.8KPa, evaporative condenser is recovered to the title complex of 300g ether and trimethyl-gallium;
To separate and join still and be warming up to 130 ℃, and be evacuated to and be 12KPa, trimethyl-gallium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 530g trimethyl-gallium;
Reduce to 90 ℃ with separating the temperature of joining still, be evacuated to 0.8KPa, evaporative condenser is recovered to the 1200g NHD;
To separate and join still and be warming up to 130 ℃, and be evacuated to and be 10KPa, trimethyl-gallium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 210g trimethyl-gallium;
Reduce to 60 ℃ with separating the temperature of joining still, be evacuated to 1KPa, evaporative condenser is recovered to the 480g NHD.
Embodiment 8
Join the title complex that adds 1500g ether and trimethyl indium in the still toward being full of separating of nitrogen, under agitation condition, progressively add 1700g NHD (CH 3O (CH 2CH 2O) nCH 3, n=3), be warming up to 60 ℃, vacuumize and be decompressed to 70KPa, evaporative condenser is recovered to the 260g ether;
To separate and join still and be warming up to 70 ℃, and vacuumize and be decompressed to 0.8KPa, evaporative condenser is recovered to the title complex of 280g ether and trimethyl indium;
To separate and join still and be warming up to 130 ℃, and be evacuated to and be 12KPa, trimethyl indium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 540g trimethyl indium;
Reduce to 80 ℃ with separating the temperature of joining still, be evacuated to 1KPa, evaporative condenser is recovered to the 1180g NHD;
To separate and join still and be warming up to 130 ℃, and be evacuated to and be 8KPa, trimethyl indium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 230g trimethyl indium;
Reduce to 60 ℃ with separating the temperature of joining still, be evacuated to 0.7KPa, evaporative condenser is recovered to the 500g NHD.
Embodiment 9
Join the title complex that adds 1470g ether and trimethyl-gallium in the still toward being full of separating of nitrogen, under agitation condition, progressively add 1700g NHD (CH 3O (CH 2CH 2O) nCH 3, n=8), be warming up to 60 ℃, vacuumize and be decompressed to 50KPa, evaporative condenser is recovered to the 260g ether;
To separate and join still and remain on 60 ℃, and vacuumize and be decompressed to 1KPa, evaporative condenser is recovered to the title complex of 300g ether and trimethyl-gallium;
To separate and join still and be warming up to 130 ℃, and be evacuated to and be 15KPa, trimethyl-gallium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 530g trimethyl-gallium;
Reduce to 70 ℃ with separating the temperature of joining still, be evacuated to 1KPa, evaporative condenser is recovered to the 1150g NHD;
To separate and join still and be warming up to 130 ℃, and be evacuated to and be 8KPa, trimethyl-gallium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 220g trimethyl-gallium;
Reduce to 60 ℃ with separating the temperature of joining still, be evacuated to 0.8KPa, evaporative condenser is recovered to the 520g NHD.
Embodiment 10
Join the title complex that adds 1500g ether and trimethylaluminium in the still toward being full of separating of nitrogen, under agitation condition, progressively add 1700g NHD (CH 3O (CH 2CH 2O) nCH 3, n=4), be warming up to 60 ℃, vacuumize and be decompressed to 60KPa, evaporative condenser is recovered to the 270g ether;
To separate and join still and be warming up to 80 ℃, and vacuumize and be decompressed to 0.9KPa, evaporative condenser is recovered to the title complex of 300g ether and trimethylaluminium;
To separate and join still and be warming up to 140 ℃, and be evacuated to and be 10KPa, trimethylaluminium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 520g trimethylaluminium;
Reduce to 80 ℃ with separating the temperature of joining still, be evacuated to 1KPa, evaporative condenser is recovered to the 1150g NHD;
To separate and join still and be warming up to 140 ℃, and be evacuated to and be 7KPa, trimethylaluminium through separate join after with gaseous form overflow and in holding tank condensation and collection to the 210g trimethylaluminium;
Reduce to 60 ℃ with separating the temperature of joining still, be evacuated to 0.7KPa, evaporative condenser is recovered to the 480g NHD.
The detected result of last illustrative embodiment 1-10.
Through ICP-OES, magnetic resonance detection goes out the yield in MO source.Table 1 has provided the detected result of embodiment 1-10.
The detected result of table 1 embodiment 1-10
Visible from table 1, the separating method of completing the square and can obtain the high MO source of purity of organometallics of the present invention and etherate.

Claims (10)

  1. Organometallics and etherate separate method of completing the square, comprise step:
    Step 1: raw material placed be full of separating of rare gas element and join still, said raw material contains the title complex of MO source and ether; The part thing that under agitation condition, will be selected from aminated compounds or high polyethers adds to separate joins in the still; Add after the part thing, replacement(metathesis)reaction takes place, to obtain part thing and MO source title complex; Steam and condensing and recycling separating the ether of joining the formation of still replacement(metathesis)reaction;
    Step 2: will separate the title complex evaporation and the condensing and recycling of joining unreacted MO source and ether in the still;
    Step 3: will separate the part thing of joining in the still and MO source title complex and separate and join, and separate the part thing that obtains after joining and stay to separate and join in the still, MO overflows with gaseous form in the source, and condensing and recycling;
    Step 4: staying of Xie Peihou separated the part thing of joining in the still evaporate also condensing and recycling.
  2. 2. organometallics according to claim 1 and etherate separate method of completing the square, it is characterized in that said rare gas element is nitrogen, argon gas or helium.
  3. 3. organometallics according to claim 1 and etherate separate method of completing the square, it is characterized in that,
    Said MO source is trimethyl-gallium or trimethylaluminium or trimethyl indium;
    Said aminated compounds is tri-n-butylamine, quadrol, Diisopropylamine;
    Said high polyethers is NHD (CH 3O (CH 2CH 2O) nCH 3, n=3 ~ 8).
  4. 4. organometallics according to claim 1 and etherate separate method of completing the square, it is characterized in that, also comprise intermediate steps: after step 2 and before step 3, will separate and join unreacted part thing evaporation and condensing and recycling in the still.
  5. 5. organometallics according to claim 1 and etherate separate method of completing the square, it is characterized in that also comprise step: after step 4, repeating step three and step 4 are at least once.
  6. 6. organometallics according to claim 1 and etherate separate method of completing the square; It is characterized in that; In step 1, with separate join ether that the still replacement(metathesis)reaction forms when steaming temperature be 50 ~ 80 ℃ and pressure be normal pressure or temperature be 50 ~ 80 ℃ down and vacuum tightness be 50 ~ 70KPa.
  7. 7. organometallics according to claim 1 and etherate separate method of completing the square, it is characterized in that in step 2, temperature is that 60 ~ 80 ℃, vacuum tightness are 0.8 ~ 3KPa when separating the title complex evaporation of joining unreacted MO source and ether in the still.
  8. 8. organometallics according to claim 1 and etherate separate method of completing the square, it is characterized in that in step 3, to separate the timing temperature be that 130 ~ 170 ℃, vacuum tightness are 7 ~ 20KPa with separating the part thing of joining in the still and MO source title complex.
  9. 9. organometallics according to claim 1 and etherate separate method of completing the square, in step 4, temperature was that 60 ~ 90 ℃, vacuum tightness are 0.7 ~ 1KPa when staying of Xie Peihou separated the part thing of joining in the still and evaporated.
  10. 10. organometallics according to claim 5 and etherate separate method of completing the square, it is characterized in that in said intermediate steps, will separate when joining in the still unreacted part thing evaporation temperature and be 80 ℃, vacuum tightness is 0.7KPa.
CN201210232657.1A 2012-07-05 2012-07-05 Decomplexation method of metal organic compound and ether complex Active CN102718784B (en)

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN103145745A (en) * 2013-03-06 2013-06-12 江苏南大光电材料股份有限公司 Method for industrially preparing high-purity metal organic compound
CN103965227A (en) * 2013-01-30 2014-08-06 上海宏锐新材料科技有限公司 Industrial purification method of trimethyl gallium
CN103965228A (en) * 2013-01-30 2014-08-06 上海宏锐新材料科技有限公司 Industrial purification method of triethyl gallium
CN105254654A (en) * 2015-11-19 2016-01-20 河南承明光电新材料股份有限公司 Method for purifying alkyl indium
JP2016056160A (en) * 2014-02-07 2016-04-21 宇部興産株式会社 Method for producing trialkylgallium
CN106146540A (en) * 2015-03-26 2016-11-23 清远先导材料有限公司 A kind of production method of triethyl-gallium
CN108128955A (en) * 2017-12-27 2018-06-08 江苏南大光电材料股份有限公司 The retracting device and its method of the solvent of source containing MO

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103965227A (en) * 2013-01-30 2014-08-06 上海宏锐新材料科技有限公司 Industrial purification method of trimethyl gallium
CN103965228A (en) * 2013-01-30 2014-08-06 上海宏锐新材料科技有限公司 Industrial purification method of triethyl gallium
CN103145745A (en) * 2013-03-06 2013-06-12 江苏南大光电材料股份有限公司 Method for industrially preparing high-purity metal organic compound
JP2016056160A (en) * 2014-02-07 2016-04-21 宇部興産株式会社 Method for producing trialkylgallium
CN106146540A (en) * 2015-03-26 2016-11-23 清远先导材料有限公司 A kind of production method of triethyl-gallium
CN105254654A (en) * 2015-11-19 2016-01-20 河南承明光电新材料股份有限公司 Method for purifying alkyl indium
CN108128955A (en) * 2017-12-27 2018-06-08 江苏南大光电材料股份有限公司 The retracting device and its method of the solvent of source containing MO

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