CN104860972B - The preparation method of high-purity trimethyl indium - Google Patents
The preparation method of high-purity trimethyl indium Download PDFInfo
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- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 28
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000012043 crude product Substances 0.000 claims abstract description 17
- 238000000746 purification Methods 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 11
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 8
- 230000005484 gravity Effects 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000004587 chromatography analysis Methods 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- IHLVCKWPAMTVTG-UHFFFAOYSA-N lithium;carbanide Chemical compound [Li+].[CH3-] IHLVCKWPAMTVTG-UHFFFAOYSA-N 0.000 claims description 3
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- VNBLTKHUCJLFSB-UHFFFAOYSA-N n-(trimethoxysilylmethyl)aniline Chemical compound CO[Si](OC)(OC)CNC1=CC=CC=C1 VNBLTKHUCJLFSB-UHFFFAOYSA-N 0.000 claims description 2
- 230000003252 repetitive effect Effects 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 229920013822 aminosilicone Polymers 0.000 claims 1
- KOVKEDGZABFDPF-UHFFFAOYSA-N n-(triethoxysilylmethyl)aniline Chemical compound CCO[Si](OCC)(OCC)CNC1=CC=CC=C1 KOVKEDGZABFDPF-UHFFFAOYSA-N 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- 229910052814 silicon oxide Inorganic materials 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910000765 intermetallic Inorganic materials 0.000 abstract description 2
- 230000000737 periodic effect Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 6
- 238000005481 NMR spectroscopy Methods 0.000 description 5
- 238000009835 boiling Methods 0.000 description 5
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 5
- 238000011403 purification operation Methods 0.000 description 5
- 150000001350 alkyl halides Chemical class 0.000 description 4
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000004871 chemical beam epitaxy Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 1
- OKJPEAGHQZHRQV-UHFFFAOYSA-N Triiodomethane Natural products IC(I)I OKJPEAGHQZHRQV-UHFFFAOYSA-N 0.000 description 1
- JHYLKGDXMUDNEO-UHFFFAOYSA-N [Mg].[In] Chemical compound [Mg].[In] JHYLKGDXMUDNEO-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 125000002490 anilino group Chemical group [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- GZUXJHMPEANEGY-UHFFFAOYSA-N bromomethane Chemical compound BrC GZUXJHMPEANEGY-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 150000002835 noble gases Chemical class 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The present invention relates to a kind of preparation method of high-purity trimethyl indium, belong to the technical field of the periodic table of elements the IIIth race metallic compound preparation.The preparation method of the present invention comprises the following steps：1. with ether as solvent, prepare trimethyl indium crude product；2. the trimethyl indium crude product 1. step being obtained carries out purification, and described purification process includes the step described trimethyl indium crude product being purified using the first chromatographic column；And the fixing phase that described first chromatographic column adopts is grafted silica, described grafted silica has the silicon dioxide of tri-n-octyl amine for surface grafting.The preparation method of the present invention has obtained, using synthesis and two steps of separation, the trimethyl indium that purity can reach 6N；In particular by purification process combine the means of solid-liquid separation, specific complexant is loaded on silica, not only simple to operate, and further increase purification effect.
Description
Technical field
The invention belongs to the technical field of the periodic table of elements the IIIth race metallic compound preparation, in particular, the present invention
It is related to a kind of preparation method of high-purity trimethyl indium.
Background technology
High-purity trimethyl indium is widely used in growing semiconductor film material, is metal organic chemical vapor deposition technology
(MOCVD), grow the important source material of photoelectron material during chemical beam epitaxy (CBE).High-purity in order to meet photoelectron material
Spend, (the inadequate trimethyl indium of purity can have a huge impact high-precision prescription to the performance of chip, and MOCVD is set
Standby also have very big infringement) it is desirable to the purity of high-purity trimethyl indium reaches 99.9999%, otherwise it is accomplished by purifying further.
Chinese invention patent application CN102020668A discloses a kind of method of preparation of industrialization trimethyl indium, is being full of
In the reactor of noble gases, put into indium-magnesium alloy raw material, in the presence of ether, oxolane or methyltetrahydrofuran, stirring
It is gradually added alkyl halide (bromomethane or iodomethane) under the conditions of mixing, control solvent refluxing speed by controlling the rate of addition of alkyl halide
Degree, after the completion of reaction, solvent is steamed, then obtains the coordination compound of trimethyl indium and ether at reduced pressure conditions, finally de-coordinates and obtains
Trimethyl indium.The method adopts reactor mode detached with evaporating kettle, and unreacted alloy still continues reaction in a kettle.,
Close to 95%, by-product can recycle gross production rate, does not almost have waste material；And the raw material due to adopting in course of reaction does not have
Spontaneous combustible substance, course of reaction safety, it is particularly suitable for large-scale industrial production.
Because the restriction of preparation technology is so that it is difficult to separate with reaction dissolvent, existing mode is to select ether to trimethyl indium
The complexants such as class are coordinated, and then remove low boiling point solvent under intensification and vacuum condition, then again under elevated temperature in vacuo
De-coordination obtains crude product, is then passed through rectification and obtains high purity product again.Most of complexant broadly falls into macromole high boiling point liquid, and
Viscosity is higher, and small molecule low boiling impurity is easily wrapped in inside macromole high boiling point complexant it is not easy to be divided, purity
Typically it is only capable of reaching 95.0～99.0%.Another aspect prior art is the purity ensureing trimethyl indium, can select to abandon one
Divide trimethyl indium, allow it to be carried in the lump with low boiling impurity, but due to trimethyl indium self character, lead to this portion to work
Danger larger, not easy to operate, difficulty is higher.
Content of the invention
In order to solve above-mentioned technical problem of the prior art, it is an object of the invention to provide a kind of high-purity trimethyl indium
Preparation method and preparation method thereof.
To achieve these goals, present invention employs technical scheme below：
A kind of preparation method of high-purity trimethyl indium is it is characterised in that comprise the following steps：Comprise the following steps：(1) with
Ether is solvent, prepares trimethyl indium crude product；(2) the trimethyl indium crude product that step (1) is obtained carries out purification, described purification side
Method includes the step carrying out purification to described trimethyl indium crude product using the first chromatographic column；And described first chromatographic column adopts
Fixing phase is grafted silica, and described grafted silica has the silicon dioxide of tri-n-octyl amine for surface grafting；Described purification
Operation as follows：(2.1) trimethyl indium is poured in the second chromatographic column that fixing phase is silicon dioxide, rely under gravity nature
Stream, treats that liquid flow is complete, collects solution；(2.2) solution of collection is poured in the first chromatographic column, rely on gravity naturally dirty, treat
Liquid flow complete collection solution；Again the solution collected is poured in the first chromatographic column again, repetitive operation 2～5 times；(2.3) to process
(2.2) the first chromatographic column after processing carries out heating under the temperature conditionss being less than 120 DEG C more than 100 DEG C and de-coordinates, and in layer
Analysis column bottom evacuation collects the trimethyl indium that can get purification.
Wherein, the purity of described trimethyl indium is 80.0～85.0%.
Wherein, described trimethyl indium crude product is obtained by any one of following reaction (1)～(4)：
CH3MgX+InX3→In(CH3)3+MgX2, X is I or Br (1)
CH3X+In+Mg→In(CH3)3+MgX2+CH3MgX, X are I or Br (2)
CH3X+In+Li→In(CH3)3+ Li X, X are I or Br (3)
CH3Li+InX3→In(CH3)3+ Li X, X are I or Br (4)
Wherein, described grafted silica is prepared by the following method and obtains：First with amino silane to silicon dioxide
It is surface-treated, be then grafted tri-n-octyl amine again.
Wherein, described grafted silica is prepared by the following method and obtains：Silica white is scattered in acid solution,
60～120 DEG C of stirring 10～20h, are cooled to 40～60 DEG C, add amino silane to continue stirring 10～20h, are just being subsequently adding three
Octylame, stirs 4～8h, filters and can get grafted silica.
Wherein, the mass ratio of described silica white, amino silane and tri-n-octyl amine is：100：3～6：8～12.
Wherein, described amino silane is selected from gamma-aminopropyl-triethoxy-silane, γ-aminopropyltrimethoxysilane, phenylamino
Ylmethyl triethoxysilane, phenylaminomethyl trimethoxy silane, N- β (aminoethyl)-gamma-aminopropyl-triethoxy-silane,
In N- β (aminoethyl)-γ-aminopropyltrimethoxysilane or N- β (aminoethyl)-γ-aminopropyltriethoxy diethoxy silane
At least one, preferably gamma-aminopropyl-triethoxy-silane.
Compared with prior art, the preparation method of high-purity trimethyl indium of the present invention has the advantages that：
The preparation method of the present invention has obtained, using synthesis and two steps of separation, the trimethyl indium that purity can reach 6N；
In particular by purification process combine the means of solid-liquid separation, specific complexant is loaded on silica, not only
Simple to operate, and further increase purification effect.
Specific embodiment
Below with reference to specific embodiment, the preparation method of high-purity trimethyl indium of the present invention is further explained
State, so that more complete explanation is made to the inventive concept of the present invention and its effect.
Embodiment 1
The silica white that 100g particle diameter is 1000 mesh is scattered in the aqueous hydrochloric acid solution that concentration is 1mol/L, in 80 DEG C of bar
Acidification 15h under part, is cooled to 40 DEG C, adds 5g gamma-aminopropyl-triethoxy-silane to continue stirring 12h, is subsequently adding 10g
Tri-n-octyl amine, stirs 8h, can get grafted silica after filtration.The grafted silica obtaining is loaded chromatographic column (interior
Footpath is 10mm) in, pressurization ensures that filling uniformly, is subsequently adding normal hexane and is rinsed, can get ground floor after rinsing well
Analysis post.The silica white that 100g particle diameter is 400 mesh loads in chromatographic column (internal diameter is 10mm), and pressurization ensures filling uniformly, you can
Obtain the second chromatographic column.
Embodiment 2
With CH3MgX and InX3(X is I or Br) is raw material, with ether as solvent, through slightly raising purity after synthetic reaction
Trimethyl indium for 85.0%.The purification operations being comprised the following steps with this trimethyl indium crude product.
Step 2.1：This trimethyl indium is poured in the second chromatographic column prepared by embodiment 1, relies on gravity naturally dirty, treat
Liquid flow is complete, collects solution.
Step 2.2：The solution that step 2.1 is collected all is poured in the first chromatographic column prepared by embodiment 1, relies on gravity
Naturally dirty, treat liquid flow complete collection solution；Again the solution collected all is poured in this first chromatographic column, repeat step 2
Aforementioned operation 6 times；
Step 2.3：Carry out heating to the first chromatographic column after step 2.2 is processed to de-coordinate, heating-up temperature is 105 DEG C,
And in chromatography column bottom with vacuum pump evacuation as power, collect the trimethyl indium de-coordinating.
The trimethyl indium that step 2.3 is obtained carries out ICP-OES and NMR analysis, can confirm that the trimethyl indium collected
Purity be 99.9999% (6N).
Embodiment 3
With alkyl halide CH3X (X is I or Br), indium and magnesium are raw material, with ether as solvent, through slightly raising after synthetic reaction
The trimethyl indium being 85.0% to purity.The purification operations being comprised the following steps with this trimethyl indium crude product.
Step 2.1：This trimethyl indium is poured in the second chromatographic column prepared by embodiment 1, relies on gravity naturally dirty, treat
Liquid flow is complete, collects solution.
Step 2.2：The solution that step 2.1 is collected all is poured in the first chromatographic column prepared by embodiment 1, relies on gravity
Naturally dirty, treat liquid flow complete collection solution；Again the solution collected all is poured in this first chromatographic column, repeat step 2
Aforementioned operation 6 times；
Step 2.3：Carry out heating to the first chromatographic column after step 2.2 is processed to de-coordinate, heating-up temperature is 115 DEG C,
And in chromatography column bottom with vacuum pump evacuation as power, collect the trimethyl indium de-coordinating.
The trimethyl indium that step 2.3 is obtained carries out ICP-OES and NMR analysis, can confirm that the trimethyl indium collected
Purity be 99.9999% (6N).
Embodiment 4
With CH3Li and InX3(X is I or Br) is raw material, with ether as solvent, through slightly raising purity after synthetic reaction
Trimethyl indium for 85.0%.The purification operations being comprised the following steps with this trimethyl indium crude product.
Step 2.1：This trimethyl indium is poured in the second chromatographic column prepared by embodiment 1, relies on gravity naturally dirty, treat
Liquid flow is complete, collects solution.
Step 2.2：The solution that step 2.1 is collected all is poured in the first chromatographic column prepared by embodiment 1, relies on gravity
Naturally dirty, treat liquid flow complete collection solution；Again the solution collected all is poured in this first chromatographic column, repeat step 2
Aforementioned operation 6 times；
Step 2.3：Carry out heating to the first chromatographic column after step 2.2 is processed to de-coordinate, heating-up temperature is 105 DEG C,
And in chromatography column bottom with vacuum pump evacuation as power, collect the trimethyl indium de-coordinating.
The trimethyl indium that step 2.3 is obtained carries out ICP-OES and NMR analysis, can confirm that the trimethyl indium collected
Purity be 99.9999% (6N).
Embodiment 5
With alkyl halide CH3X (X is I or Br), indium and lithium are raw material, with ether as solvent, through slightly raising after synthetic reaction
The trimethyl indium being 85.0% to purity.The purification operations being comprised the following steps with this trimethyl indium crude product.
Step 2.1：This trimethyl indium is poured in the second chromatographic column prepared by embodiment 1, relies on gravity naturally dirty, treat
Liquid flow is complete, collects solution.
Step 2.2：The solution that step 2.1 is collected all is poured in the first chromatographic column prepared by embodiment 1, relies on gravity
Naturally dirty, treat liquid flow complete collection solution；Again the solution collected all is poured in this first chromatographic column, repeat step 2
Aforementioned operation 6 times；
Step 2.3：Carry out heating to the first chromatographic column after step 2.2 is processed to de-coordinate, heating-up temperature is 115 DEG C,
And in chromatography column bottom with vacuum pump evacuation as power, collect the trimethyl indium de-coordinating.
The trimethyl indium that step 2.3 is obtained carries out ICP-OES and NMR analysis, can confirm that the trimethyl indium collected
Purity be 99.9999% (6N).
Comparative example
Chromatographic column is made with the tri-n-octyl amine of di-n-butylamine, tripropyl amine (TPA) alternate embodiment 1, using the purification behaviour of embodiment
Make, find through ICP-OES and NMR analysis, not only can not remove ether therein or methyl-tetrahydrofuran solvent, and metal
Foreign ion, but also di-n-butylamine and tripropyl amine (TPA) can be introduced.
For the ordinary skill in the art, specific embodiment is simply exemplarily described to the present invention,
The present invention implements and is not subject to the restrictions described above, as long as employing method of the present invention design and technical scheme is carried out
The improvement of various unsubstantialities, or the not improved design by the present invention and technical scheme directly apply to other occasions, all
Within protection scope of the present invention.
Claims (6)
1. a kind of preparation method of high-purity trimethyl indium it is characterised in that：Comprise the following steps：(1) with ether as solvent, preparation
Trimethyl indium crude product；(2) the trimethyl indium crude product that step (1) is obtained carries out purification, and described purification process includes adopting first
The step that chromatographic column carries out purification to described trimethyl indium crude product；And the fixing phase that described first chromatographic column adopts is grafting two
Silicon oxide, described grafted silica has the silicon dioxide of tri-n-octyl amine for surface grafting；The operation of described purification is as follows：
(2.1) trimethyl indium is poured in the second chromatographic column that fixing phase is silicon dioxide, rely on gravity naturally dirty, treat liquid flow
Complete, collect solution；(2.2) solution of collection is poured in the first chromatographic column, rely on gravity naturally dirty, treat the complete collection of liquid flow
Solution；Again the solution collected is poured in the first chromatographic column again, repetitive operation 3～6 times；(2.3) to after (2.2) are processed
First chromatographic column carries out heating under the temperature conditionss being less than 120 DEG C more than 100 DEG C and de-coordinates, and in chromatography column bottom evacuation
Collect the trimethyl indium that can get purification；The purity of described trimethyl indium crude product is 80.0～85.0%.
2. high-purity trimethyl indium according to claim 1 preparation method it is characterised in that：Described trimethyl indium crude product leads to
Any one crossing following reaction (1)～(4) obtains：
CH3MgX+InX3→In(CH3)3+MgX2, X is I or Br (1)；
CH3X+In+Mg→In(CH3)3+MgX2+CH3MgX, X are I or Br (2)；
CH3X+In+Li→In(CH3)3+ Li X, X are I or Br (3)；
CH3Li+InX3→In(CH3)3+ Li X, X are I or Br (4).
3. high-purity trimethyl indium according to claim 1 preparation method it is characterised in that：Described grafted silica leads to
Cross following methods to prepare：First with amino silane, silicon dioxide is surface-treated, is then grafted tri-n-octyl amine again.
4. high-purity trimethyl indium according to claim 1 preparation method it is characterised in that：Described grafted silica leads to
Cross following methods to prepare：Silica white is scattered in acid solution, stirs 10～20h at 60～120 DEG C, it is cooled to 40～
60 DEG C, add amino silane to continue stirring 10～20h, be subsequently adding tri-n-octyl amine, stir 4～8h, filter and can be grafted
Silicon dioxide.
5. high-purity trimethyl indium according to claim 4 preparation method it is characterised in that：Described silica white, amino silicone
The mass ratio of alkane and tri-n-octyl amine is：100：3～6：8～12.
6. high-purity trimethyl indium according to claim 3 preparation method it is characterised in that：Described amino silane is selected from
Gamma-aminopropyl-triethoxy-silane, γ-aminopropyltrimethoxysilane, phenylaminomethyl triethoxysilane, phenylaminomethyl
Trimethoxy silane, N- β (aminoethyl)-gamma-aminopropyl-triethoxy-silane, N- β (aminoethyl)-γ-aminopropyl trimethoxy
At least one in silane or N- β (aminoethyl)-γ-aminopropyltriethoxy diethoxy silane.
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