CN104193773B - Trimethyl indium industrial purifying process - Google Patents
Trimethyl indium industrial purifying process Download PDFInfo
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- CN104193773B CN104193773B CN201410450769.3A CN201410450769A CN104193773B CN 104193773 B CN104193773 B CN 104193773B CN 201410450769 A CN201410450769 A CN 201410450769A CN 104193773 B CN104193773 B CN 104193773B
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- China
- Prior art keywords
- trimethyl indium
- ether
- purifying process
- cycloalkane
- cnh2n
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- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 19
- 230000008569 process Effects 0.000 title claims abstract description 16
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000012298 atmosphere Substances 0.000 claims abstract description 12
- 150000001924 cycloalkanes Chemical class 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- WJTCGQSWYFHTAC-UHFFFAOYSA-N cyclooctane Chemical compound C1CCCCCCC1 WJTCGQSWYFHTAC-UHFFFAOYSA-N 0.000 claims description 4
- 239000004914 cyclooctane Substances 0.000 claims description 4
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 4
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 claims description 2
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical group CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 1
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000010494 dissociation reaction Methods 0.000 abstract description 7
- 230000005593 dissociations Effects 0.000 abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 230000006872 improvement Effects 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009131 signaling function Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of trimethyl indium industrial purifying process, comprise the following steps：Trimethyl indium ether complex is added in the reactor of inert atmosphere protection; then cycloalkane CnH2n (n >=6) is added to be reacted; the temperature of reaction system is maintained at 30~100 DEG C; during dropwise addition; the condensed device cooling of the ether that is dissociated directly is received in receiving tank, realizes will be completely dissociated for ether and trimethyl indium；Reagent selected by the inventive method is conventional reagent, and inexpensive and be easy to get, course of reaction is gentle, no potential safety hazard, and as ether is constantly separated from reaction system, improves the efficiency of ether dissociation.No discarded object is reacted, cost is reduced, and to environment without any pollution.
Description
Technical field
The present invention relates to a kind of industrialized purification method in industrialization purification field, more particularly to trimethyl indium.
Background technology
Inp semiconductor material has electronics limit drift velocity high, radioresistance, the good advantage of heat conduction, with GaAs material
Material is compared, the characteristics of with breakdown electric field, thermal conductivity, high electronics average speed.Inp semiconductor material has wide-gap junction
Structure, the device made of this material, can amplify higher frequency, shorter wavelengths of signal.Indium phosphide is that one kind compares GaAs
More advanced semi-conducting material.Satellite communication industry is promoted to develop to higher frequency section.
Indium phosphide significantly shows the property more excellent compared with GaAs in terms of the even wireless application of fiber manufacturing, millimeter wave
Can, and the indium phosphide that these have something spaces out with other materials, so that finally substituting GaAs turns into compound semiconductor
The optimal selection of technology.In fiber optic communication field, only inp semiconductor technology can be by photo-detector and laser and other
Simulation and mixed signal functions are integrated into same substrate, have the advantages that high integration and low price so that optical device is realized
Important breakthrough.In wireless domain, indium phosphide amplifier is all improved in many aspects.
Trimethyl indium is metal organic chemical vapor deposition（MOCVD）The key raw material of technique epitaxial growth indium phosphide.
Though having at present about the report of trimethyl indium purification process, conventional purification process has：1st, coordinated with trimethyl indium ether
Thing is acted on the benzene through Non-aqueous processing, is dissociateed the ether in trimethyl indium ether complex, is then obtained high-purity through rectification under vacuum again
Spend trimethyl indium.Because the toxicity of benzene is very big, while requirement is again big, it certainly will bring hidden to operating personnel's safety and environmental protection
Suffer from；2nd, new part is formed with trimethyl indium ether complex and N, N, N', N'- tetramethyl -4,4'- MDA,
Dissociate ether, then de-coordinate, rectification under vacuum obtains high-purity trimethyl indium, due to N, N, N', N'- tetramethyl -4,4'- diaminourea hexichol first
Alkane is unconventional reagent, is difficult to obtain, and its operating process is also comparatively laborious, so it is pure to be also less suitable for use in industrialization
Change.
The content of the invention
It is an object of the invention to provide a kind of trimethyl indium industrial purifying process, to solve trimethyl indium industrialization purification
Operating process is bothered, the problem of cost is higher.
In order to solve the above problems, the invention provides a kind of trimethyl indium industrial purifying process, comprise the following steps：
Trimethyl indium ether complex is added in the reactor of inert atmosphere protection, cycloalkane is then added under conditions of stirring
CnH2n(n >=6) are reacted, and the temperature of reaction system is maintained at 30~100 DEG C, and the ether being dissociated in adition process is by condensation
Device cooling is collected in receiving tank, and the trimethyl indium for dissociateing ether obtains high-purity trimethyl indium through rectification under vacuum.
Further improvement is that：Ether in the trimethyl indium ether complex be selected from tetrahydrofuran, ether, isopropyl ether or
Methyltetrahydrofuran, preferably ether.
Further improvement is that：The cycloalkane CnH2n (n >=6) is selected from hexamethylene or cyclooctane.
Further improvement is that：The mol ratio of the cycloalkane CnH2n (n >=6) and trimethyl indium is 1~5 ︰ 1.
Further improvement is that：It is 30 that the rate of addition of the cycloalkane CnH2n (n >=6), which is controlled in maintenance system temperature,
~100 DEG C.
Further improvement is that：The rectification under vacuum, rectifying pressure is 80~200mmHg, and rectification temperature is 80 DEG C~150
℃。
Further improvement is that：The inert atmosphere is high pure nitrogen atmosphere or high-purity argon gas atmosphere.
The beneficial effects of the invention are as follows：1st, selected reagent is conventional reagent, is easily obtainable, while cheap；2、
Selected reagent is non-toxic, it is ensured that operating personnel's safety；3rd, course of reaction is more gentle, without potential safety hazard；4th, ether dissociation effect
Rate is very high, and cycloalkane CnH2n (n >=6) is reusable, environmentally safe without discarded object.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, the present embodiment
It is only used for explaining the present invention, is not intended to limit the scope of the present invention..
Embodiment 1
Under an inert atmosphere, 2500 grams of trimethyl indium etherates are added in a kettle., under agitation, to
3000 grams of hexamethylene is added dropwise in reactor, the speed that control is added dropwise is maintained the temperature between 70 DEG C, and dissociation is collected during dropwise addition
The ether gone out.After ether will be completely dissociated, through rectification under vacuum（Rectifying pressure is 150mmHg, and rectification temperature is 110 DEG C）, obtain high-purity
1590 grams of trimethyl indium, using trimethyl indium as calculating benchmark, yield 93.0%.
Embodiment 2
Under an inert atmosphere, 2500 grams of trimethyl galliums are added in a kettle., under agitation, are added dropwise into reactor
1500 grams of hexamethylene, the speed that control is added dropwise is maintained the temperature between 70 DEG C, and the ether dissociateed is collected during dropwise addition.Ether
After will be completely dissociated, through rectification under vacuum（Rectifying pressure is 150mmHg, and rectification temperature is 110 DEG C）, obtain high-purity trimethyl indium 1540
Gram, using trimethyl gallium as calculating benchmark, yield 90.1%.
Embodiment 3
Under an inert atmosphere, 2500 grams of trimethyl indium etherates are added in a kettle., under agitation, to
2800 grams of cyclooctane is added dropwise in reactor, the speed that control is added dropwise is maintained the temperature between 70 DEG C, and dissociation is collected during dropwise addition
The ether gone out.After ether will be completely dissociated, through rectification under vacuum（Rectifying pressure is 150mmHg, and rectification temperature is 110 DEG C）, obtain high-purity
1520 grams of trimethyl indium, using trimethyl indium as calculating benchmark, yield 89.0%.
Embodiment 4
Under an inert atmosphere, 2500 grams of trimethyl indium etherates are added in a kettle., under agitation, to
1700 grams of cyclooctane is added dropwise in reactor, the speed that control is added dropwise is maintained the temperature between 70 DEG C, and dissociation is collected during dropwise addition
The ether gone out.After ether will be completely dissociated, through rectification under vacuum（Rectifying pressure is 150mmHg, and rectification temperature is 110 DEG C）, obtain high-purity
1400 grams of trimethyl indium, using trimethyl indium as calculating benchmark, yield 81.9%.
In invented technology, the condition of reaction and dissociation ether is steady, it is easy to control, with conventional use benzene or N, N, N', N'- tetra-
Methyl -4,4'- MDA purifying trimethyl indium compare, stablize with materials safety, be readily obtained, it is cheap,
The advantages such as dissociation efficiency height.Gross production rate can reach more than 90%., cycloalkane CnH2n (n >=6) is nontoxic, may be reused, will not
Any discarded object is produced, is particularly suitable for industrialized purification.
Claims (7)
1. a kind of trimethyl indium industrial purifying process, it is characterised in that：Comprise the following steps：In the reaction of inert atmosphere protection
Trimethyl indium ether complex is added in device, cycloalkane CnH2n is then added under conditions of stirring, n >=6 are reacted, is reacted
The temperature of system is maintained at 30~100 DEG C, and the ether being dissociated in adition process is collected in receiving tank by condenser cooling, solution
The trimethyl indium for separating out ether obtains high-purity trimethyl indium through rectification under vacuum.
2. trimethyl indium industrial purifying process as claimed in claim 1, it is characterised in that：The trimethyl indium ether coordinates
Ether in thing is selected from tetrahydrofuran, ether, isopropyl ether or methyltetrahydrofuran.
3. trimethyl indium industrial purifying process as claimed in claim 1, it is characterised in that：The cycloalkane CnH2n, n >=6
Selected from hexamethylene or cyclooctane.
4. trimethyl indium industrial purifying process as claimed in claim 1, it is characterised in that：The cycloalkane CnH2n, n >=6
Mol ratio with trimethyl indium is 1~5 ︰ 1.
5. trimethyl indium industrial purifying process as claimed in claim 1, it is characterised in that：The cycloalkane CnH2n, n >=6
Rate of addition control maintenance system temperature be 30~100 DEG C.
6. trimethyl indium industrial purifying process as claimed in claim 1, it is characterised in that：The rectification under vacuum, rectifying pressure
Power is 80~200mmHg, and rectification temperature is 80 DEG C~150 DEG C.
7. trimethyl indium industrial purifying process as claimed in claim 1, it is characterised in that：The inert atmosphere is High Purity Nitrogen
Gas atmosphere or high-purity argon gas atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410450769.3A CN104193773B (en) | 2014-09-05 | 2014-09-05 | Trimethyl indium industrial purifying process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410450769.3A CN104193773B (en) | 2014-09-05 | 2014-09-05 | Trimethyl indium industrial purifying process |
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| Publication Number | Publication Date |
|---|---|
| CN104193773A CN104193773A (en) | 2014-12-10 |
| CN104193773B true CN104193773B (en) | 2017-11-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410450769.3A Active CN104193773B (en) | 2014-09-05 | 2014-09-05 | Trimethyl indium industrial purifying process |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109553632A (en) * | 2018-12-29 | 2019-04-02 | 贵州威顿晶磷电子材料股份有限公司 | A kind of method of purification of trimethyl aluminium |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1854147A (en) * | 2005-04-12 | 2006-11-01 | 罗门哈斯电子材料有限公司 | Purification of metal-containing 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 |
-
2014
- 2014-09-05 CN CN201410450769.3A patent/CN104193773B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1854147A (en) * | 2005-04-12 | 2006-11-01 | 罗门哈斯电子材料有限公司 | Purification of metal-containing 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 |
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| CN104193773A (en) | 2014-12-10 |
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Address after: No. 88 Baoshun Road, Economic and Technological Development Zone, Wuhu City, Anhui Province, 241000 Patentee after: Anhui Yagesheng Electronic New Materials Co.,Ltd. Address before: 241009 Third Floor, Management Committee of Wuhu Economic and Technological Development Zone, Anhui Province Patentee before: ANHUI ARGOSUN NEW ELECRONIC MATERIALS Co.,Ltd. |
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