CN108003184A - A kind of Phosphine ligands and preparation method thereof, using and its extract high-purity alkyl aluminum compound method - Google Patents
A kind of Phosphine ligands and preparation method thereof, using and its extract high-purity alkyl aluminum compound method Download PDFInfo
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- CN108003184A CN108003184A CN201711455715.6A CN201711455715A CN108003184A CN 108003184 A CN108003184 A CN 108003184A CN 201711455715 A CN201711455715 A CN 201711455715A CN 108003184 A CN108003184 A CN 108003184A
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Abstract
The invention discloses a kind of Phosphine ligands of the load containing styrene polymer, and the preparation method and application of the Phosphine ligands, and the method for Phosphine ligands extraction high-purity alkyl aluminum compound.Technical solution of the present invention uses the Phosphine ligands of loaded by polystyrene, and ligand stability is good, and through de-coordinating, after rectifying, alkyl aluminum purity is not less than 99.99995% mass fraction；The Phosphine ligands of loaded by polystyrene so that later stage Phosphine ligands regenerative operation is simple.The method of the present invention, which can significantly improve the access times of ligand and solve ligand, is not easy regenerated deficiency, and this method has so that ligand circulation technology is simple in the alkyl aluminum crude product purification such as trimethyl aluminium, triethyl aluminum, reduces cost, it is suitable for scale production the advantages that.
Description
Technical field
The invention belongs to metal aluminum organic compound purification technique field, and in particular to a kind of metal aluminum organic compound carries
The pure preparation method with Phosphine ligands.The invention further relates to carried with Phosphine ligands from the alkyl aluminum crude product such as trimethyl aluminium, triethyl aluminum
The method for taking high-purity alkyl aluminum compound.
Background technology
Presoma of the high-purity alkyl aluminum compound as aluminium nitride, is widely used in growing semiconductor film material, and
And it is the basic raw material of third generation semiconductor.When high-purity alkyl aluminum compound purity is less than 99.9999%, will seriously it restrict
The lifting of third generation semiconducting behavior.The purification of alkyl aluminum crude product at present mainly selects amine and phosphine ligand to be coordinated again,
Then heat up again, after removing low boiling point solvent under vacuum condition, then de-coordinated under elevated temperature in vacuo and obtain higher degree product.
And ligand is recycled and reuses because boiling point is high, but at the same time higher boiling fixedness impurity also can because of the accumulation of cycle-index and
Content raises, and in order to reach more preferable refining effect, just needs to purify ligand after recycling for several times or more renews
Ligand, simultaneously because impurity and ligand boiling point are all higher, cause energy consumption needed for ligand purifying rectifying very high, and what is more renewed matches somebody with somebody
Body is again so that the increase of ligand usage amount, all causes production cost to remain high, it is often more important that can cause very big shadow to environment
Ring.
The content of the invention
The technical problem to be solved in the present invention is overcome the difficult life of complex in alkyl aluminum purification process in the prior art, give up
The intractable insufficient problem of gurry provides a kind of Novel phosphine ligand.The invention solves another problem be to provide a kind of extraction
The method of high-purity alkyl aluminum compound.
In order to realize the above object present invention employs following technical scheme：
A kind of Phosphine ligands, it is characterised in that the Phosphine ligands of the load containing styrene polymer.
A kind of preparation method of Phosphine ligands, its step include,
（1）Styrene polymer is dissolved in dichloromethane solvent, halogenating agent, catalyst is added, reacts 12-48h at room temperature, obtain
To halogenated styrenes polymer, the molar ratio of the styrene polymer and the halogenating agent is 1:1-2, the catalyst are institute
State the 1-5% of styrene polymerization amount of substance；The halogenating agent is bromine, iodine or bromo-succinimide；The catalyst is
Aluminium chloride, titanium chloride, aluminum acetate or acetic acid titanium；The styrene polymer is total to for polystyrene or styrene-divinylbenzene
Polymers, degree of cross linking 1-12%；
（2）Halogenated styrenes polymer is successively received into alkali cleaning through unsaturated carbonate hydrogen and saturated salt solution salt is washed, re-evaporation after separation
Solvent is removed, obtains halogenated styrenes polymer solids, drying for standby after again with methanol, ultra-pure water, methanol wash successively；
（3）Chlorodiphenylphosphine is added in THF solvents, butyl lithium or high activity magnesium powder are then added in THF solvents, finally
Halogenated styrenes polymer solids are added, under oxygen barrier atmosphere protection, 1-4h, then 10-30 DEG C of stirring are heated to reflux at 40-70 DEG C
React 12-48h；
（4）In the ratio 1 relative to THF solvent qualities: 3-4:After 1-2 adds methanol and hexane, consolidating for precipitation is separated by filtration
Body, under oxygen barrier atmosphere protection, milli-Q water and dry point of isolated solid, that is, be made the Phosphine ligands.
In order to obtain superior technique effect, step（1）Described in polystyrene be polystyrene or stryrene divinyl
Base benzene copolymer, degree of cross linking 2-8%；
In order to obtain superior technique effect, step（1）Described in halogenating agent be iodine；
In order to obtain superior technique effect, step（1）Described in catalyst be aluminium chloride；
In order to obtain superior technique effect, step（1）、（2）、（4）Described in dichloromethane solvent, the THF solvents, described
Methanol and hexane are pre-processed by rectifying.
A kind of application of Phosphine ligands, it is characterised in that applied to extraction high-purity alkyl aluminum compound.
A kind of method of Phosphine ligands extraction high-purity alkyl aluminum compound, its step include,
（1）The Phosphine ligands for taking the above method to prepare；
（2）Alkyl aluminum crude product is taken under oxygen barrier atmosphere protection, adds step（1）The Phosphine ligands are reacted, under oxygen barrier atmosphere
60-90 DEG C of reaction temperature, reaction time 36-72h, obtains complex, wherein, the alkyl aluminum crude product and the Phosphine ligands quality
Than for 1-3:3；Contain ether solvents of the mass fraction no more than 40% in the alkyl aluminum crude product solution；The alkyl aluminum crude product is molten
After liquid removes solvent, alkyl aluminum crude product purity is not less than 99% mass fraction；
（3）By step（2）Obtained complex, steams low-boiling compound at first vacuum 0-0.02Mpa, 60-120 DEG C, then
Vacuum 0-0.02Mpa, 120-200 DEG C heating de-coordinates, and is received after the alkyl aluminum evaporation generated after de-coordination with liquid nitrogen, alkyl aluminum exists again
Rectifying is carried out in rectifying column, rectification temperature is 125-200 DEG C, and pressure is normal pressure, obtains mass fraction and is not less than 99.99995%
High-purity alkyl aluminum.
In order to obtain superior technique effect, step（1）Described in alkyl aluminum be trimethyl aluminium or triethyl aluminum；
In order to obtain superior technique effect, step（3）The Phosphine ligands generated after middle de-coordination are directly by step（2）-（3）Repetition makes
With；
In order to obtain superior technique effect, step（3）The Phosphine ligands generated after middle de-coordination under oxygen barrier atmosphere through separation of solid and liquid,
Washed in order with the methanol of the methanol of rectification process, ultra-pure water, rectification process again, after finally being dried with oxygen barrier atmosphere thermal purging
By step（2）-（3）Reuse；
In order to obtain superior technique effect, above-mentioned oxygen barrier atmosphere is high pure nitrogen or argon gas.
Technical solution of the present invention uses the Phosphine ligands of loaded by polystyrene, and ligand stability is good, the alkyl after de-coordination, rectifying
Aluminium purity is not less than 99.99995% mass fraction；The Phosphine ligands of loaded by polystyrene so that later stage Phosphine ligands regenerative operation letter
It is single.The method of the present invention, which can significantly improve the access times of ligand and solve ligand, is not easy regenerated deficiency, and this method, which has, to be caused
Ligand circulation technology is simple in the purification of the alkyl aluminum such as trimethyl aluminium, triethyl aluminum crude product, reduces cost, suitable for scale production etc.
Advantage.
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
Embodiment 1 prepares 1# Phosphine ligands
The preparation method of 1# Phosphine ligands, its step include,
（1）The polystyrene of the 2000g degrees of cross linking 2% is dissolved in 4000g dichloromethane solvents, adds 20g aluminum chloride catalysts,
700g bromine halogenating agents are added dropwise again, react 24h at room temperature；
（2）Product priority saturated sodium carbonate alkali cleaning and saturated salt solution salt are washed, solvent removed by evaporation at reduced pressure, then use again after separation
Methanol, water, methanol wash successively, after vacuum drying, obtain the light yellow brominated Polystyrene solids of 2140g；
（3）500g Chlorodiphenylphosphines are dissolved in 4000g THF, nitrogen protection, adds 500gn- Buli solution and previous step
Rapid obtained 1500g brominated Polystyrenes, under oxygen barrier atmosphere protection, after 50 DEG C are heated to reflux 4h, stir reaction at 10 DEG C
24h；
（4）Product is added after 12kg methanol and 4kg hexanes to the solid for being separated by filtration precipitation, it is ultrapure under oxygen barrier atmosphere protection
Water washing and dry point of isolated solid, that is, be made 1610g white 1# Phosphine ligands solids.
31P NMR（162 MHz, CDCl3）δ -5.85.Through elemental analysis, according to C, H, P content, estimation polystyrene is born
1.7mmolPPh in the Phosphine ligands of load3/g。
Embodiment 2 prepares 2# Phosphine ligands
The preparation method of 2# Phosphine ligands, its step include,
（1）The styrene diethylene benzene copoly mer of the 2000g degrees of cross linking 5% is dissolved in 4000g dichloromethane solvents, is added
50g acetic acid Al catalysts, then 1000g iodine halogenating agents are added dropwise, 24h is reacted at room temperature；
（2）Product priority saturated sodium carbonate alkali cleaning and saturated salt solution salt are washed, solvent removed by evaporation at reduced pressure, then use again after separation
Methanol, water, methanol wash successively, after vacuum drying, obtain the light yellow iodized polystyrene solids of 2070g；
（3）500g Chlorodiphenylphosphines are dissolved in 4000g THF, nitrogen protection, adds 60g high activities magnesium powder and previous step
Rapid obtained 1500g iodized polystyrenes, after 70 DEG C are heated to reflux 1h, the stirring reaction 12h at 30 DEG C；
（3）Product is added after 16kg methanol and 8kg hexanes to the solid for being separated by filtration precipitation, it is ultrapure under oxygen barrier atmosphere protection
Water washing and dry point of isolated solid, that is, be made 1530g white 2# Phosphine ligands solids.
31P NMR（162 MHz, CDCl3）δ -5.85.Through elemental analysis, according to C, H, P content, estimation polystyrene is born
1.5mmolPPh in the Phosphine ligands of load3/g。
Embodiment 3 prepares 3# Phosphine ligands
The preparation method of 3# Phosphine ligands, its step include,
（1）The polystyrene of the 2000g degrees of cross linking 8% is dissolved in 4000g dichloromethane solvents, adds 100g acetic acid titanium catalysts,
1000g N- bromo-succinimide halogenating agents are added dropwise again, react 24h at room temperature；
（2）Product priority saturated sodium carbonate alkali cleaning and saturated salt solution salt are washed, solvent removed by evaporation at reduced pressure, then use again after separation
Methanol, water, methanol wash successively, after vacuum drying, obtain the light yellow brominated Polystyrene solids of 2070g；
（3）500g Chlorodiphenylphosphines are dissolved in 4000g THF, nitrogen protection, adds 60g high activities magnesium powder and previous step
Rapid obtained 1500g brominated Polystyrenes, after 40 DEG C are heated to reflux 2h, in 20 DEG C of stirring reaction 48h；
（4）Product is added after 12kg methanol and 8kg hexanes to the solid for being separated by filtration precipitation, it is ultrapure under oxygen barrier atmosphere protection
Water washing and dry point of isolated solid, that is, be made 1530g white 3# Phosphine ligands solids.
31P NMR（162 MHz, CDCl3）δ -5.85.Through elemental analysis, according to C, H, P content, estimation polystyrene is born
1.4mmolPPh in the Phosphine ligands of load3/g。
Embodiment 4
The method that 1# Phosphine ligands extract high-purity alkyl aluminum compound, its step include,
（1）The 1# Phosphine ligands for taking 1500g embodiments 1 to prepare；
（2）Under oxygen barrier atmosphere protection, trimethyl aluminium crude products of the 1500g containing ether is added in 1500g 1# Phosphine ligands and is carried out instead
Should, 60 DEG C of reaction 36h are heated under oxygen barrier atmosphere, obtain complex, wherein, the trimethyl aluminium crude product is containing mass fraction
30% ether；After the alkyl aluminum crude product solution removes solvent, alkyl aluminum crude product purity is 99%；
（3）By step（2）Obtained complex steams low-boiling compound at vacuum 0.01Mpa, 90 DEG C, then
0.005Mpa, heat at 130 DEG C and de-coordinate, and is received after the trimethyl aluminium evaporation generated after de-coordination with liquid nitrogen, remaining as Phosphine ligands；Three
Aluminium methyl carries out rectifying, rectifying column oxygen barrier atmosphere protection in rectifying column again, and rectification temperature is 127 DEG C, and pressure is normal pressure, is obtained
It is not less than 99.99995% high-purity trimethyl aluminium to mass fraction, trimethyl aluminium yield is 90%.
Embodiment 5
1# Phosphine ligands extract high-purity alkyl aluminum compound method after directly repeating 30 times, its step include,
（1）In embodiment 4, step（3）The step of Phosphine ligands generated after middle de-coordination are directly by embodiment 4（2）-（3）Repetition makes
With 29 times；
（2）Under oxygen barrier atmosphere protection, trimethyl aluminium crude products of the 500g containing ether is added into step（1）In 1# Phosphine ligands in into
Row reacts, and 60 DEG C of reaction 48h are heated under oxygen barrier atmosphere, obtain complex, wherein, the trimethyl aluminium crude product contains mass fraction
For 30% ether；After the alkyl aluminum crude product solution removes solvent, alkyl aluminum crude product purity is 99%；
（3）By step（2）Obtained complex steams low-boiling compound at vacuum 0.01Mpa, 90 DEG C, then
0.005Mpa, heat at 130 DEG C and de-coordinate, and is received after the trimethyl aluminium evaporation generated after de-coordination with liquid nitrogen, remaining as Phosphine ligands；Three
Aluminium methyl carries out rectifying, rectifying column oxygen barrier atmosphere protection in rectifying column again, and rectification temperature is 127 DEG C, and pressure is normal pressure, is obtained
It is not less than 99.99995% high-purity trimethyl aluminium to mass fraction, trimethyl aluminium yield is 68%.
Embodiment 6
The method that high-purity alkyl aluminum compound is extracted after being repeated 30 times after the processing of 1# Phosphine ligands, its step include,
（1）In embodiment 4, step（3）The Phosphine ligands generated after middle de-coordination first separation of solid and liquid under oxygen barrier atmosphere, then with rectifying
After methanol, ultra-pure water, the methanol of rectification process of reason wash in order, dried with oxygen barrier atmosphere thermal purging, then by embodiment 4
Step（2）-（3）Reuse 29 times；
（2）Under oxygen barrier atmosphere protection, trimethyl aluminium crude products of the 1000g containing ether is added into step（1）In 1# Phosphine ligands in
Reacted, 60 DEG C of reaction 48h are heated under oxygen barrier atmosphere, obtain complex, wherein, the trimethyl aluminium crude product is containing quality point
Number is 30% ether；After the alkyl aluminum crude product solution removes solvent, alkyl aluminum crude product purity is 99%；
（3）By step（2）Obtained complex steams low-boiling compound at vacuum 0.01Mpa, 90 DEG C, then
0.005Mpa, heat at 130 DEG C and de-coordinate, and is received after the trimethyl aluminium evaporation generated after de-coordination with liquid nitrogen, remaining as Phosphine ligands；Three
Aluminium methyl carries out rectifying, rectifying column oxygen barrier atmosphere protection in rectifying column again, and rectification temperature is 127 DEG C, and pressure is normal pressure, is obtained
It is not less than 99.99995% high-purity trimethyl aluminium to mass fraction, trimethyl aluminium yield is 85%.
Embodiment 7
The method that 2# Phosphine ligands extract high-purity alkyl aluminum compound, its step include,
（1）The 2# Phosphine ligands for taking 1500g embodiments 2 to prepare；
（2）Under oxygen barrier atmosphere protection, 1000g trimethyl aluminiums crude product liquid is added in 1500g 2# Phosphine ligands and is reacted,
60 DEG C of reaction 36h are heated under oxygen barrier atmosphere, obtain complex, wherein, the trimethyl aluminium crude product does not contain solvent, and purity is
99.99%；
（3）By step（2）Obtained complex steams low-boiling compound at vacuum 0.01Mpa, 90 DEG C, then
0.005Mpa, heat at 130 DEG C and de-coordinate, and is received after the trimethyl aluminium evaporation generated after de-coordination with liquid nitrogen, remaining as Phosphine ligands；Three
Aluminium methyl carries out rectifying, rectifying column oxygen barrier atmosphere protection in rectifying column again, and rectification temperature is 127 DEG C, and pressure is normal pressure, is obtained
It is not less than 99.99995% high-purity trimethyl aluminium to mass fraction, trimethyl aluminium yield is 93%.
Embodiment 8
The method that 3# Phosphine ligands extract high-purity alkyl aluminum compound, its step include,
（1）3# Phosphine ligands prepared by Example 3；
（2）Under oxygen barrier atmosphere protection, 500g triethyl aluminums crude product is added in 1500g 3# Phosphine ligands and is reacted, oxygen barrier gas
90 DEG C of reaction 36h are heated under atmosphere, obtain complex, wherein, the trimethyl aluminium crude product does not contain solvent, and purity is
99.99%；
（3）By step（2）Obtained complex steams low-boiling compound at vacuum 0.01Mpa, 100 DEG C, then
0.005Mpa, heat at 140 DEG C and de-coordinate, and is received after the triethyl aluminum evaporation generated after de-coordination with liquid nitrogen, remaining as Phosphine ligands；Three
Aluminium ethide carries out rectifying in rectifying column again, and rectification temperature is 194 DEG C, and pressure is normal pressure, obtains mass fraction and is not less than
99.99995% high-purity triethyl aluminum, triethyl aluminum yield are 93%.
Comparative example
（1）Under oxygen barrier atmosphere protection, by trimethyl aluminium crude products of the 500g containing ether add in 1500g triphenylphosphine ligands into
Row reacts, and 60 DEG C of reaction 48h are heated under oxygen barrier atmosphere, obtain complex, wherein, the trimethyl aluminium crude product contains mass fraction
For 30% ether, trimethyl aluminium purity is 99%；
（2）Step（1）Obtained complex steams low-boiling compound at vacuum 0.01Mpa, 90 DEG C, then 0.005Mpa,
Heat and de-coordinate at 130 DEG C, received after the trimethyl aluminium evaporation generated after de-coordination with liquid nitrogen, trimethyl aluminium carries out in rectifying column again
Rectifying, rectifying column oxygen barrier atmosphere protection, rectification temperature are 127 DEG C, and pressure is normal pressure, obtains mass fraction and is not less than
99.99995% high-purity trimethyl aluminium, trimethyl aluminium yield are 90%；
（3）Step（2）The Phosphine ligands generated after middle de-coordination first separation of solid and liquid under oxygen barrier atmosphere, then with the methanol of rectification process,
After ultra-pure water, the methanol of rectification process wash in order, dried with oxygen barrier atmosphere thermal purging, then by above step（1）-（2）Weight
Use 15 times again；The high-purity trimethyl aluminium that mass fraction is not less than 99.9993% is obtained, trimethyl aluminium yield is 60%.
Claims (10)
- A kind of 1. Phosphine ligands, it is characterised in that the Phosphine ligands of the load containing styrene polymer.
- 2. the preparation method of Phosphine ligands as claimed in claim 1, its step includes,（1）Styrene polymer is dissolved in dichloromethane solvent, halogenating agent, catalyst is added, reacts 12-48h at room temperature, obtain To halogenated styrenes polymer, the molar ratio of the styrene polymer and the halogenating agent is 1:1-2, the catalyst are institute State the 1-5% of styrene polymerization amount of substance；The halogenating agent is bromine, iodine or bromo-succinimide；The catalyst is Aluminium chloride, titanium chloride, aluminum acetate or acetic acid titanium；The styrene polymer is total to for polystyrene or styrene-divinylbenzene Polymers, degree of cross linking 1-12%；（2）Halogenated styrenes polymer is successively received into alkali cleaning through unsaturated carbonate hydrogen and saturated salt solution salt is washed, re-evaporation after separation Solvent is removed, obtains halogenated styrenes polymer solids, drying for standby after again with methanol, ultra-pure water, methanol wash successively；（3）Chlorodiphenylphosphine is added in THF solvents, butyl lithium or high activity magnesium powder are then added in THF solvents, finally Halogenated styrenes polymer solids are added, under oxygen barrier atmosphere protection, 1-4h, then 10-30 DEG C of stirring are heated to reflux at 40-70 DEG C React 12-48h；（4）In the ratio 1 relative to THF solvent qualities: 3-4:After 1-2 adds methanol and hexane, consolidating for precipitation is separated by filtration Body, under oxygen barrier atmosphere protection, milli-Q water and dry point of isolated solid, that is, be made the Phosphine ligands.
- 3. the preparation method of Phosphine ligands as claimed in claim 2, it is characterised in that step（1）Described in polystyrene be polyphenyl Ethene or styrene diethylene benzene copoly mer, degree of cross linking 2-8%；The halogenating agent is iodine；The catalyst is chlorination Aluminium.
- 4. the preparation method of Phosphine ligands as claimed in claim 2, it is characterised in that step（1）、（2）、（4）Described in dichloromethane Alkane solvents, the THF solvents, the methanol and hexane are pre-processed by rectifying.
- 5. the application of Phosphine ligands as claimed in claim 1, it is characterised in that applied to extraction high-purity alkyl aluminum compound.
- 6. the method for Phosphine ligands extraction high-purity alkyl aluminum compound as claimed in claim 1, its step include,（1）The Phosphine ligands for taking the above method to prepare；（2）Alkyl aluminum crude product is taken under oxygen barrier atmosphere protection, adds step（1）The Phosphine ligands are reacted, under oxygen barrier atmosphere 60-90 DEG C of reaction temperature, reaction time 36-72h, obtains complex, wherein, the alkyl aluminum crude product and the Phosphine ligands quality Than for 1-3:3；Contain ether solvents of the mass fraction no more than 40% in the alkyl aluminum crude product solution；The alkyl aluminum crude product is molten After liquid removes solvent, alkyl aluminum crude product purity is not less than 99% mass fraction；（3）By step（2）Obtained complex, steams low-boiling compound at first vacuum 0-0.02Mpa, 60-120 DEG C, then Vacuum 0-0.02Mpa, 120-200 DEG C heating de-coordinates, and is received after the alkyl aluminum evaporation generated after de-coordination with liquid nitrogen, alkyl aluminum exists again Rectifying is carried out in rectifying column, rectification temperature is 125-200 DEG C, and pressure is normal pressure, obtains mass fraction and is not less than 99.99995% High-purity alkyl aluminum.
- 7. the method for extraction high-purity alkyl aluminum compound as claimed in claim 6, it is characterised in that step（1）Described in alkane Base aluminium is trimethyl aluminium or triethyl aluminum.
- 8. the method for extraction high-purity alkyl aluminum compound as claimed in claim 6, it is characterised in that step（3）After middle de-coordination The Phosphine ligands of generation directly press step（2）-（3）Reuse.
- 9. the method for extraction high-purity alkyl aluminum compound as claimed in claim 6, it is characterised in that step（3）After middle de-coordination The Phosphine ligands of generation are pressed under oxygen barrier atmosphere through separation of solid and liquid, then with the methanol of the methanol of rectification process, ultra-pure water, rectification process Sequential purge, step is pressed after finally being dried with oxygen barrier atmosphere thermal purging（2）-（3）Reuse.
- 10. the method for extraction high-purity alkyl aluminum compound as claimed in claim 6, it is characterised in that the oxygen barrier atmosphere is High pure nitrogen, high-purity helium or high-purity argon gas.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110526937A (en) * | 2019-08-15 | 2019-12-03 | 江苏南大光电材料股份有限公司 | The preparation method of ultra-pure triethyl aluminum |
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| CN105175440A (en) * | 2015-09-30 | 2015-12-23 | 江西佳因光电材料有限公司 | Preparation method of trimethylaluminium |
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- 2017-12-28 CN CN201711455715.6A patent/CN108003184A/en active Pending
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| CN105175440A (en) * | 2015-09-30 | 2015-12-23 | 江西佳因光电材料有限公司 | Preparation method of trimethylaluminium |
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| M. JEAN FARRALL等: "Bromination and Lithiation: Two Important Steps in the Functionalization of Polystyrene Resins", 《J. ORG. CHEM.》 * |
| MARGARET BERNARD等: "Wittig Reagents Bound to Cross-Linked Polystyrenes", 《J. ORG. CHEM.》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110526937A (en) * | 2019-08-15 | 2019-12-03 | 江苏南大光电材料股份有限公司 | The preparation method of ultra-pure triethyl aluminum |
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