CN102718784A - Decomplexation method of metal organic compound and ether complex - Google Patents
Decomplexation method of metal organic compound and ether complex Download PDFInfo
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- 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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Claims (10)
- 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. 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. 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. 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. 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. 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. 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. 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. 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. 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.
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CN201210232657.1A CN102718784B (en) | 2012-07-05 | 2012-07-05 | Decomplexation method of metal organic compound and ether complex |
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CN201210232657.1A CN102718784B (en) | 2012-07-05 | 2012-07-05 | Decomplexation method of metal organic compound and ether complex |
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CN102718784B CN102718784B (en) | 2015-09-02 |
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Cited By (7)
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 |
Citations (2)
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GB2201418A (en) * | 1987-02-27 | 1988-09-01 | Plessey Co Plc | Preparation of metal alkyls |
TW217415B (en) * | 1991-11-19 | 1993-12-11 | Shell Internat Res Schappej B V |
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2012
- 2012-07-05 CN CN201210232657.1A patent/CN102718784B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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GB2201418A (en) * | 1987-02-27 | 1988-09-01 | Plessey Co Plc | Preparation of metal alkyls |
TW217415B (en) * | 1991-11-19 | 1993-12-11 | Shell Internat Res Schappej B V |
Non-Patent Citations (1)
Title |
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SHU WANGEN ET AL.: "Synthesis and purification of trialkyl compounds of gallium and indium", 《RARE METALS》 * |
Cited By (7)
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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CN102718784B (en) | 2015-09-02 |
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Inventor after: Zhu Shihui Inventor after: Zhu Liu Inventor after: Zhu Shiming Inventor after: Liu Liu Inventor after: Zhu Shihui, Zhu Liu, Zhu Shiming, Liu Liuzhao, love Ting Inventor before: Zhu Shihui Inventor before: Zhu Liu Inventor before: Zhu Shiming Inventor before: Liu Liu |
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Effective date of registration: 20220516 Address after: No. 1116-1, building 1, Dianzhong Business Plaza, Dianzhong new area, Kunming, Yunnan 650212 Patentee after: Kunming forerunner New Material Technology Co.,Ltd. Address before: 511500 Industrial Zone, wo Yun town, Qingxin County, Qingyuan, Guangdong (beside the fish dam road) Patentee before: FIRST RARE MATERIALS Co.,Ltd. |
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