CN104860972A - Preparation method of high-purity trimethyl indium - Google Patents
Preparation method of high-purity trimethyl indium Download PDFInfo
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- CN104860972A CN104860972A CN201510239288.2A CN201510239288A CN104860972A CN 104860972 A CN104860972 A CN 104860972A CN 201510239288 A CN201510239288 A CN 201510239288A CN 104860972 A CN104860972 A CN 104860972A
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- trimethyl indium
- purity
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- chromatography column
- crude product
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- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 24
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000012043 crude product Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 15
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 8
- 230000005526 G1 to G0 transition Effects 0.000 claims abstract description 5
- 238000004587 chromatography analysis Methods 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 30
- 230000005484 gravity Effects 0.000 claims description 12
- 229960001866 silicon dioxide Drugs 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 6
- 238000000197 pyrolysis Methods 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 3
- ULRCHFVDUCOKTE-UHFFFAOYSA-N 3-[3-aminopropyl(diethoxy)silyl]oxybutan-1-amine Chemical compound NCCC[Si](OCC)(OCC)OC(C)CCN ULRCHFVDUCOKTE-UHFFFAOYSA-N 0.000 claims description 2
- ZDZYGYFHTPFREM-UHFFFAOYSA-N 3-[3-aminopropyl(dimethoxy)silyl]oxypropan-1-amine Chemical compound NCCC[Si](OC)(OC)OCCCN ZDZYGYFHTPFREM-UHFFFAOYSA-N 0.000 claims description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 2
- DVKNMIVLAGELBG-UHFFFAOYSA-N NCC[Si](OCC(OCC)(OCC)OCC)(OCC)CCCN Chemical compound NCC[Si](OCC(OCC)(OCC)OCC)(OCC)CCCN DVKNMIVLAGELBG-UHFFFAOYSA-N 0.000 claims description 2
- 239000003929 acidic solution Substances 0.000 claims description 2
- KOVKEDGZABFDPF-UHFFFAOYSA-N n-(triethoxysilylmethyl)aniline Chemical compound CCO[Si](OCC)(OCC)CNC1=CC=CC=C1 KOVKEDGZABFDPF-UHFFFAOYSA-N 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
- 238000004381 surface treatment Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000000737 periodic effect Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 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
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 150000001350 alkyl halides Chemical class 0.000 description 4
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000463 material Substances 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
- 238000004871 chemical beam epitaxy Methods 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
- 239000002245 particle Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 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
- JHYLKGDXMUDNEO-UHFFFAOYSA-N [Mg].[In] Chemical compound [Mg].[In] JHYLKGDXMUDNEO-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- RDHPKYGYEGBMSE-UHFFFAOYSA-N bromoethane Chemical compound CCBr RDHPKYGYEGBMSE-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 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
- 239000010409 thin film Substances 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 invention relates to a preparation method of high-purity trimethyl indium, belonging to the technical field of preparing group III metallic compounds in the periodic table of elements. The preparation method disclosed by the invention comprises the following steps: (1) taking diethyl ether as a solvent to prepare a trimethyl indium crude product; (2) carrying out purification to the trimethyl indium crude product obtained in step (1), wherein the purification method comprises the step of adopting a first chromatographic column to carry out purification to the trimethyl indium crude product; and the stationary phase adopted by the first chromatographic column is grafted silica, and the grafted silica is silica of which the surface is grafted with tri-n-octylamine. The preparation method disclosed by the invention adopts the two steps of synthesis and separation and obtains the trimethyl indium of which the purity can reach 6N; above all, the purity method adopted is combined with the solid-liquid separation means, a certain coordination agent is loaded on the silica, not only is the operation simple, but also the purification effect is improved further.
Description
Technical field
The invention belongs to technical field prepared by the periodic table of elements the IIIth race's metallic compound, in particular, the present invention relates to a kind of preparation method of high-purity trimethyl indium.
Background technology
High-purity trimethyl indium is widely used in growing semiconductor thin-film material, is the important source material of grow light electronic material in metal organic chemical vapor deposition technology (MOCVD), chemical beam epitaxy (CBE) process.In order to meet photoelectron material high purity, (trimethyl indium that purity is inadequate can have a huge impact the performance of chip high-precision specification of quality, very large infringement is also had to MOCVD device), require that the purity of high-purity trimethyl indium reaches 99.9999%, otherwise just need to purify further.
Chinese invention patent application CN102020668A discloses a kind of method of preparation of industrialization trimethyl indium, in the reactor being full of rare gas element, drop into indium-magnesium alloy raw material, under ether, tetrahydrofuran (THF) or methyltetrahydrofuran exist, progressively add haloalkane (monobromethane or methyl iodide) under agitation, solvent refluxing speed is controlled by the rate of addition controlling haloalkane, after having reacted, solvent is steamed, obtain the title complex of trimethyl indium and ether more at reduced pressure conditions, finally solution is joined and is obtained trimethyl indium.The mode that the method adopts reactor to be separated with evaporating kettle, unreacted alloy still continues reaction in a kettle., and overall yield is close to 95%, and by product can be recycled, and does not almost have waste material; And there is no spontaneous combustible substance due to the raw material adopted in reaction process, reaction process safety, is particularly suitable for large-scale industrial production.
Trimethyl indium is due to the restriction of preparation technology, itself and reaction solvent is made to be difficult to be separated, existing mode selects the coordination agents such as ethers to carry out coordination, then under intensification and vacuum condition, low boiling point solvent is removed, and then under elevated temperature in vacuo, solution is joined and is obtained crude product, then obtains high purity product again through rectifying.It is liquid that major part coordination agent all belongs to macromole high boiling point, and viscosity is higher, and small molecules lower-boiling impurity is easily wrapped in inside macromole high boiling point coordination agent, is not easy to be divided, and purity generally only can reach 95.0 ~ 99.0%.Prior art is the purity ensureing trimethyl indium on the other hand, can select to abandon a part of trimethyl indium, allow it be taken out of in the lump with lower-boiling impurity, but due to trimethyl indium self character, the danger causing this portion to work is comparatively large, and not easy to operate, difficulty is higher.
Summary of the invention
In order to solve above-mentioned technical problem of the prior art, the object of the present invention is to provide preparation method of a kind of high-purity trimethyl indium and preparation method thereof.
To achieve these goals, present invention employs following technical scheme:
A preparation method for high-purity trimethyl indium, is characterized in that comprising the following steps: comprise the following steps: (1) take ether as solvent, prepares trimethyl indium crude product; (2) carry out purifying to the trimethyl indium crude product that step (1) obtains, described purification process comprises employing first chromatography column carries out purifying step to described trimethyl indium crude product; And the stationary phase that described first chromatography column adopts is grafted silica, and described grafted silica is the silicon-dioxide that surface grafting has tri-n-octyl amine; The operation of described purifying is as follows: (2.1) pour stationary phase into trimethyl indium is in the second chromatography column of silicon-dioxide, relies on gravity naturally dirty, treats that liquid stream is complete, collect solution; (2.2) solution of collection is poured in the first chromatography column, rely on gravity naturally dirty, treat the complete collection solution of liquid stream; Again the solution collected is poured in the first chromatography column again, repetitive operation 2 ~ 5 times; (2.3) 100 DEG C and add pyrolysis under being less than the temperature condition of 120 DEG C and join are being greater than to the first chromatography column after (2.2) process, and bottom chromatography column, are vacuumizing the trimethyl indium collected and can obtain purifying.
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):
CH
3mgX+InX
3→ In (CH
3)
3+ MgX
2, X is I or Br (1)
CH
3x+In+Mg → In (CH
3)
3+ MgX
2+ CH
3mgX, X are I or Br (2)
CH
3x+In+Li → In (CH
3)
3+ Li X, X are I or Br (3)
CH
3li+InX
3→ In (CH
3)
3+ Li X, X are I or Br (4)
Wherein, described grafted silica prepares by the following method: first utilize aminosilane to carry out surface treatment to silicon-dioxide, and then grafting tri-n-octyl amine.
Wherein, described grafted silica prepares by the following method: be scattered in by silica-gel powder in acidic solution, 10 ~ 20h is stirred at 60 ~ 120 DEG C, be cooled to 40 ~ 60 DEG C, add aminosilane and continue stirring 10 ~ 20h, then add tri-n-octyl amine, stir 4 ~ 8h, filtration can obtain grafted silica.
Wherein, the mass ratio of described silica-gel powder, aminosilane and tri-n-octyl amine is: 100:3 ~ 6:8 ~ 12.
Wherein, described aminosilane is selected from least one in γ-aminopropyl triethoxysilane, γ-aminopropyltrimethoxysilane, phenylaminomethyl triethoxyl silane, phenylaminomethyl Trimethoxy silane, N-β (aminoethyl)-γ-aminopropyl triethoxysilane, N-β (aminoethyl)-γ-aminopropyltrimethoxysilane or N-β (aminoethyl)-γ-aminopropyltriethoxy diethoxy silane, is preferably γ-aminopropyl triethoxysilane.
Compared with prior art, the preparation method of high-purity trimethyl indium of the present invention has following beneficial effect:
Preparation method of the present invention adopts synthesis and is separated two steps and obtains the trimethyl indium that purity can reach 6N; Especially the purification process adopted combines the means of solid-liquid separation, by specific coordination agent load on silica, not only simple to operate, and further increases purification effect.
Embodiment
Below with reference to specific embodiment, the preparation method to high-purity trimethyl indium of the present invention is further elaborated, to make more complete explanation to inventive concept of the present invention and effect thereof.
Embodiment 1
Be that to be scattered in concentration be in the aqueous hydrochloric acid of 1mol/L to 1000 object silica-gel powders by 100g particle diameter, acidification 15h under the condition of 80 DEG C, be cooled to 40 DEG C, add 5g γ-aminopropyl triethoxysilane to continue to stir 12h, then 10g tri-n-octyl amine is added, stir 8h, after filtration, can grafted silica be obtained.Loaded by the grafted silica obtained in chromatography column (internal diameter is 10mm), pressurization ensures to fill evenly, then adds normal hexane and rinses, can obtain the first chromatography column after rinsing well.Be that 400 object silica-gel powders load in chromatography column (internal diameter is 10mm) by 100g particle diameter, pressurization ensures to fill evenly, can obtain the second chromatography column.
Embodiment 2
With CH
3mgX and InX
3(X is I or Br) is raw material, is solvent with ether, through slightly raising the trimethyl indium that purity is 85.0% after building-up reactions.The purification operations comprised the following steps is carried out with this trimethyl indium crude product.
Step 2.1: this trimethyl indium is poured in the second chromatography column prepared by embodiment 1, relies on gravity naturally dirty, treats that liquid stream is complete, collection solution.
Step 2.2: solution step 2.1 collected all is poured in the first chromatography column prepared by embodiment 1, relies on gravity naturally dirty, treats the complete collection solution of liquid stream; Again the solution collected all is poured in this first chromatography column, the aforementioned operation of repeating step 26 times;
Step 2.3: add pyrolysis to the first chromatography column after step 2.2 processes and join, Heating temperature is 105 DEG C, and is power with vacuum pump evacuation bottom chromatography column, collects the trimethyl indium that solution is joined.
ICP-OES and NMR analysis is carried out to the trimethyl indium that step 2.3 obtains, can confirm that the purity of the trimethyl indium collected is 99.9999% (6N).
Embodiment 3
With haloalkane CH
3x (X is I or Br), indium and magnesium are raw material, are solvent with ether, through slightly raising the trimethyl indium that purity is 85.0% after building-up reactions.The purification operations comprised the following steps is carried out with this trimethyl indium crude product.
Step 2.1: this trimethyl indium is poured in the second chromatography column prepared by embodiment 1, relies on gravity naturally dirty, treats that liquid stream is complete, collection solution.
Step 2.2: solution step 2.1 collected all is poured in the first chromatography column prepared by embodiment 1, relies on gravity naturally dirty, treats the complete collection solution of liquid stream; Again the solution collected all is poured in this first chromatography column, the aforementioned operation of repeating step 26 times;
Step 2.3: add pyrolysis to the first chromatography column after step 2.2 processes and join, Heating temperature is 115 DEG C, and is power with vacuum pump evacuation bottom chromatography column, collects the trimethyl indium that solution is joined.
ICP-OES and NMR analysis is carried out to the trimethyl indium that step 2.3 obtains, can confirm that the purity of the trimethyl indium collected is 99.9999% (6N).
Embodiment 4
With CH
3li and InX
3(X is I or Br) is raw material, is solvent with ether, through slightly raising the trimethyl indium that purity is 85.0% after building-up reactions.The purification operations comprised the following steps is carried out with this trimethyl indium crude product.
Step 2.1: this trimethyl indium is poured in the second chromatography column prepared by embodiment 1, relies on gravity naturally dirty, treats that liquid stream is complete, collection solution.
Step 2.2: solution step 2.1 collected all is poured in the first chromatography column prepared by embodiment 1, relies on gravity naturally dirty, treats the complete collection solution of liquid stream; Again the solution collected all is poured in this first chromatography column, the aforementioned operation of repeating step 26 times;
Step 2.3: add pyrolysis to the first chromatography column after step 2.2 processes and join, Heating temperature is 105 DEG C, and is power with vacuum pump evacuation bottom chromatography column, collects the trimethyl indium that solution is joined.
ICP-OES and NMR analysis is carried out to the trimethyl indium that step 2.3 obtains, can confirm that the purity of the trimethyl indium collected is 99.9999% (6N).
Embodiment 5
With haloalkane CH
3x (X is I or Br), indium and lithium are raw material, are solvent with ether, through slightly raising the trimethyl indium that purity is 85.0% after building-up reactions.The purification operations comprised the following steps is carried out with this trimethyl indium crude product.
Step 2.1: this trimethyl indium is poured in the second chromatography column prepared by embodiment 1, relies on gravity naturally dirty, treats that liquid stream is complete, collection solution.
Step 2.2: solution step 2.1 collected all is poured in the first chromatography column prepared by embodiment 1, relies on gravity naturally dirty, treats the complete collection solution of liquid stream; Again the solution collected all is poured in this first chromatography column, the aforementioned operation of repeating step 26 times;
Step 2.3: add pyrolysis to the first chromatography column after step 2.2 processes and join, Heating temperature is 115 DEG C, and is power with vacuum pump evacuation bottom chromatography column, collects the trimethyl indium that solution is joined.
ICP-OES and NMR analysis is carried out to the trimethyl indium that step 2.3 obtains, can confirm that the purity of the trimethyl indium collected is 99.9999% (6N).
Comparative example
Chromatography column is made with the tri-n-octyl amine of Di-n-Butyl Amine, tripropyl amine alternate embodiment 1, adopt the purification operations of embodiment, analyze through ICP-OES and NMR and find, not only can not remove ether wherein or methyl-tetrahydrofuran solvent, and metallic impurity ion, but also Di-n-Butyl Amine and tripropyl amine can be introduced.
For the ordinary skill in the art; specific embodiment is just to invention has been exemplary description; specific implementation of the present invention is not subject to the restrictions described above; as long as have employed the improvement of the various unsubstantialities that method of the present invention is conceived and technical scheme is carried out; or design of the present invention and technical scheme directly applied to other occasion, all within protection scope of the present invention without to improve.
Claims (7)
1. a preparation method for high-purity trimethyl indium, is characterized in that: comprise the following steps: (1) is solvent with ether, prepares trimethyl indium crude product; (2) carry out purifying to the trimethyl indium crude product that step (1) obtains, described purification process comprises employing first chromatography column carries out purifying step to described trimethyl indium crude product; And the stationary phase that described first chromatography column adopts is grafted silica, and described grafted silica is the silicon-dioxide that surface grafting has tri-n-octyl amine; The operation of described purifying is as follows: (2.1) pour stationary phase into trimethyl indium is in the second chromatography column of silicon-dioxide, relies on gravity naturally dirty, treats that liquid stream is complete, collect solution; (2.2) solution of collection is poured in the first chromatography column, rely on gravity naturally dirty, treat the complete collection solution of liquid stream; Again the solution collected is poured in the first chromatography column again, repetitive operation 3 ~ 6 times; (2.3) 100 DEG C and add pyrolysis under being less than the temperature condition of 120 DEG C and join are being greater than to the first chromatography column after (2.2) process, and bottom chromatography column, are vacuumizing the trimethyl indium collected and can obtain purifying.
2. the preparation method of high-purity trimethyl indium according to claim 1, is characterized in that: the purity of described trimethyl indium crude product is 80.0 ~ 85.0%.
3. the preparation method of high-purity trimethyl indium according to claim 1, is characterized in that: described trimethyl indium crude product is obtained by any one of following reaction (1) ~ (4):
CH
3mgX+InX
3→ In (CH
3)
3+ MgX
2, X is I or Br (1)
CH
3x+In+Mg → In (CH
3)
3+ MgX
2+ CH
3mgX, X are I or Br (2)
CH
3x+In+Li → In (CH
3)
3+ Li X, X are I or Br (3)
CH
3li+InX
3→ In (CH
3)
3+ Li X, X are I or Br (4).
4. the preparation method of high-purity trimethyl indium according to claim 1, is characterized in that: described grafted silica prepares by the following method: first utilize aminosilane to carry out surface treatment to silicon-dioxide, and then grafting tri-n-octyl amine.
5. the preparation method of high-purity trimethyl indium according to claim 1, it is characterized in that: described grafted silica prepares by the following method: described grafted silica prepares by the following method: silica-gel powder is scattered in acidic solution, 10 ~ 20h is stirred at 60 ~ 120 DEG C, be cooled to 40 ~ 60 DEG C, add aminosilane and continue stirring 10 ~ 20h, then add tri-n-octyl amine, stir 4 ~ 8h, filtration can obtain grafted silica.
6. the preparation method of high-purity trimethyl indium according to claim 5, is characterized in that: the mass ratio of described silica-gel powder, aminosilane and tri-n-octyl amine is: 100:3 ~ 6:8 ~ 12.
7. the preparation method of high-purity trimethyl indium according to claim 4, it is characterized in that: described aminosilane is selected from least one in γ-aminopropyl triethoxysilane, γ-aminopropyltrimethoxysilane, phenylaminomethyl triethoxyl silane, phenylaminomethyl Trimethoxy silane, N-β (aminoethyl)-γ-aminopropyl triethoxysilane, N-β (aminoethyl)-γ-aminopropyltrimethoxysilane or N-β (aminoethyl)-γ-aminopropyltriethoxy diethoxy silane, be preferably γ-aminopropyl triethoxysilane.
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Citations (2)
| 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 |
| CN103849165A (en) * | 2012-11-28 | 2014-06-11 | 中国科学院化学研究所 | Functionalized nanometer silica with ultraviolet ray absorption function group grafted on surface, and preparation method thereof |
-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103849165A (en) * | 2012-11-28 | 2014-06-11 | 中国科学院化学研究所 | Functionalized nanometer silica with ultraviolet ray absorption function group grafted on surface, and preparation method thereof |
| 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 |
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