CN112552321B - Lanthanum-containing organic compound and application thereof - Google Patents
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- 229910052746 lanthanum Inorganic materials 0.000 title claims abstract description 47
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 150000002894 organic compounds Chemical class 0.000 title claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000010992 reflux Methods 0.000 claims abstract description 13
- 239000005051 trimethylchlorosilane Substances 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 42
- 239000007788 liquid Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 12
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 239000002243 precursor Substances 0.000 abstract description 11
- 229910052744 lithium Inorganic materials 0.000 abstract description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 5
- 230000009257 reactivity Effects 0.000 abstract description 4
- 235000019988 mead Nutrition 0.000 abstract description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 4
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000012266 salt solution Substances 0.000 description 4
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 4
- 229910003002 lithium salt Inorganic materials 0.000 description 3
- 159000000002 lithium salts Chemical class 0.000 description 3
- BDNKZNFMNDZQMI-UHFFFAOYSA-N 1,3-diisopropylcarbodiimide Chemical compound CC(C)N=C=NC(C)C BDNKZNFMNDZQMI-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- -1 R' is one of H Chemical group 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- VHHHONWQHHHLTI-UHFFFAOYSA-N hexachloroethane Chemical compound ClC(Cl)(Cl)C(Cl)(Cl)Cl VHHHONWQHHHLTI-UHFFFAOYSA-N 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 239000012263 liquid product Substances 0.000 description 2
- IHLVCKWPAMTVTG-UHFFFAOYSA-N lithium;carbanide Chemical compound [Li+].[CH3-] IHLVCKWPAMTVTG-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- NOFQQSNEWLROSA-UHFFFAOYSA-N [Li]C(N)=N Chemical class [Li]C(N)=N NOFQQSNEWLROSA-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012788 optical film Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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- 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
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C267/00—Carbodiimides
-
- 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
- C07F17/00—Metallocenes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses a lanthanum-containing organic compound and application thereof, wherein the chemical formula of the organic compound is LaCl 3 1.5THF, the organic compound is prepared by reflux reaction of lanthanum powder, trimethylchlorosilane and ethanol in THF solution; the application of the lanthanum-containing organic compound leads to LaCl 3 Preparation of La (R) by reaction of THF with lithium amidinate 2 ‑R’AMD) 3 LaCl is added 3 1.5 preparation by reaction of THF with M (RCp), lithium diisopropylacetamidinate (RCp) 2 La( i Pr 2 -mead). The invention prepares the lanthanum-containing organic compound LaCl through reflux reaction of lanthanum powder, trimethylchlorosilane and ethanol in THF solution 3 1.5THF, the lanthanum-containing organic compound prepared in high yield and high reactivity, and the lanthanum precursor La (R 2 ‑R’AMD) 3 And (RCp) 2 La( i Pr 2 Mead) can greatly shorten the production time while also increasing the yield of the product.
Description
Technical Field
The invention relates to the field of semiconductor materials, in particular to a lanthanum-containing organic compound and application thereof.
Background
Lanthanum is a metal rare earth element, and has active chemical property and is easy to oxidize in air. Lanthanum oxide (La) 2 O 3 ) Is an oxide of lanthanum, is widely used in semiconductor processes due to its high dielectric constant (hexagonal phase La 2 O 3 The dielectric constant of 27), the band gap width (-5.5 eV), so that the film can be used for a gate oxide film alone or with HfO 2 、Y 2 O 3 Doping forms a high dielectric constant (high-k) layer in the DRAM memory chip. At the same time La 2 O 3 Also used for HfO 2 Capping layer of gate oxide film layer, la/La 2 O 3 As a passivation layer of germanium (Ge). La (La) 2 O 3 Is "transparent" over a wide range of wavelengths and is also a good optical film.
To deposit high quality La 2 O 3 Thin films, la precursor materials have been widely studied, and conventional La precursors include: la (thd) 3 ，La(Cp) 3 ，La( i PrCp) 3 And La [ N (SiMe) 3 ) 2 ] 3 . Wherein: la (thd) 3 Is low, only 0.36A/cycle; la (Cp) 3 And La (a ] i PrCp) 3 Is not suitable for film deposition at the temperature of more than 250 ℃ and has carbon residue; la [ N (SiMe) 3 ) 2 ] 3 There is no stable ALD saturation curve and Si remains in the film. Therefore, la precursor materials with high thermal stability and high vapor pressure: la (La) i Pr 2 -MeAMD) 3 、La( i Pr 2 -FMD) 3 And (RCp) 2 La( i Pr 2 -mead) gradually replaced the conventional La precursor.
Preparing La precursor La% i Pr 2 -MeAMD) 3 、La( i Pr 2 -FMD) 3 And (RCp) 2 La( i Pr 2 -MeAMD), due to the steric nature of the metal La and its very easy ability to bind oxygen, results in LaCl 3 Is extremely easy to be fully or partially hydrolyzed to generate La-O bonds with high stability, and coordination bonds can not be further formed. Therefore, laCl cannot be used simply in the preparation of the above-mentioned molecules 3 Tetrahydrofuran coordinated LaCl is generally used 3 THFx. There are generally two methods reported in the literature: 1. directly using LaCl 3 Stirred with THF to form LaCl 3 THFx;2. reacting lanthanum powder with hexachloroethane to obtain LaCl 3 THFx. LaCl prepared in the first route 3 THFx has low reactivity and low yield of La complex. Such asLa was prepared in document ALD of LanthanumAluminate Using Lanthanum Formamidinate Precursor, mater.Res.Soc.Symp.Proc.Vol.1036 i Pr 2 -FMD) 3 When the final yield is less than 60%. Prepared in the document US9099301-Preparation of lanthanum-containing precursors and deposition of lanthanum-containing films i PrCp) 2 La( i Pr 2 -mead) yields were only 36%. LaCl prepared in the second route 3 The productivity of the product prepared by taking THFx as the raw material is improved, la # i Pr 2 -MeAMD) 3 The yield of the product can reach 77 percent. However, in the preparation of LaCl 3 In THFx, the La powder and hexachloroethane are required to be continuously sonicated in THF solution for 3-5 days to achieve a yield of 84-90% in document Synthesis and Characterization ofVolatile, thermally Stable, reactive Transition MetalAmidinates, inorganic Chemistry,2003,42,7951-7958. The efficiency is low, and the method is not suitable for production and application.
There is therefore a need to develop a new LaCl 3 The preparation method of THFx raw material is used for preparing La-based precursor material, so that the time is shortened, the efficiency is improved, and the yield can be improved.
Disclosure of Invention
In order to solve the above-mentioned shortcomings in the prior art, the present invention aims to provide a lanthanum-containing organic compound and application thereof, which is prepared by reflux reaction of lanthanum powder, trimethylchlorosilane and ethanol in THF solution 3 1.5THF, the lanthanum-containing organic compound prepared in high yield and high reactivity, and the lanthanum precursor La (R 2 -R’AMD) 3 And (RCp) 2 La( i Pr 2 Mead) can greatly shorten the production time while also increasing the yield of the product.
The aim of the invention can be achieved by the following technical scheme:
an organic compound containing lanthanum, the chemical formula of the organic compound is LaCl 3 1.5THF, the organic compound is prepared by reflux reaction of lanthanum powder, trimethylchlorosilane and ethanol in THF solution, and the chemical reaction equation is as followsThe following steps:
the preparation method of the lanthanum-containing organic compound specifically comprises the following steps:
s1, weighing lanthanum powder, adding tetrahydrofuran, rapidly stirring and mixing uniformly, adding trimethylchlorosilane while stirring, and mixing uniformly to obtain a mixed solution A;
s2, slowly dripping absolute ethyl alcohol into the mixed solution A, wherein small bubbles overflow from the liquid surface, the temperature of the system slightly rises, heating, refluxing and stirring for 4-6 hours after dripping is finished, and stopping the reaction until the system gradually turns into white turbid liquid from black turbid liquid;
s3, filtering the turbid liquid after the reaction to obtain a filter cake, washing the filter cake with n-hexane for 2-4 times, and finally drying the filter cake in vacuum to obtain white powder LaCl 3 ·1.5THF。
Further preferably, the lanthanum powder has a particle size of 50 to 200 mesh.
Further preferably, the mole ratio of lanthanum powder, trimethylchlorosilane and ethanol is 1:3-4:3-4.
Further preferably, the temperature of the heated reflux in step S3 is 70 to 90 ℃.
Application of lanthanum-containing organic compound in LaCl 3 Preparation of La (R) by reaction of THF with lithium amidinate 2 -R’AMD) 3 R is one of methyl, ethyl, isopropyl, n-butyl and tert-butyl, R' is one of H, methyl, ethyl, isopropyl, n-butyl and tert-butyl, and the chemical reaction formula is as follows:
application of lanthanum-containing organic compound in LaCl 3 1.5 preparation by reaction of THF with M (RCp), lithium diisopropylacetamidinate (RCp) 2 La( i Pr 2 -MeAMD), M is Li, na,One of K, R is one of H, methyl, ethyl and isopropyl, and the chemical reaction general formula is as follows:
the invention has the beneficial effects that:
the invention prepares the lanthanum-containing organic compound LaCl through reflux reaction of lanthanum powder, trimethylchlorosilane and ethanol in THF solution 3 1.5THF, the lanthanum-containing organic compound prepared in high yield and high reactivity, and the lanthanum precursor La (R 2 -R’AMD) 3 And (RCp) 2 La( i Pr 2 -MeAMD) can greatly shorten the production time from > 5 days to within 3 days, and simultaneously improve the yield of the product from about 77% to 85% at present.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be understood that the terms "open," "upper," "lower," "thickness," "top," "middle," "length," "inner," "peripheral," and the like indicate orientation or positional relationships, merely for convenience in describing the present invention and to simplify the description, and do not indicate or imply that the components or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present invention.
An organic compound containing lanthanum, the chemical formula of the organic compound is LaCl 3 1.5THF, the organic compound is prepared by reflux reaction of lanthanum powder, trimethylchlorosilane and ethanol in THF solution, and the chemical reaction equation is as follows:
the preparation method of the lanthanum-containing organic compound specifically comprises the following steps:
s1, weighing lanthanum powder (45 g,0.3 mol), adding 1L of tetrahydrofuran, rapidly stirring and mixing uniformly, adding trimethylchlorosilane (212 g,1.9 mol) while stirring, and mixing uniformly to obtain a mixed solution A;
s2, slowly dropwise adding absolute ethyl alcohol (53 g,1.1 mol) into the mixed solution A, overflowing small bubbles on the liquid surface, slightly raising the temperature of the system, heating, refluxing and stirring for 4-6h after dropwise adding, gradually changing the system from black turbid liquid to gray until the black turbid liquid becomes white turbid liquid, and stopping reacting;
s3, filtering the turbid liquid after the reaction to obtain a filter cake, washing the filter cake with 150mL of n-hexane for 2-4 times, and finally drying the filter cake in vacuum to obtain 106g of white powder LaCl 3 1.5THF in 93% yield.
Application of lanthanum-containing organic compound, la (R) is prepared by reacting LaCl3.1.5 THF of the lanthanum-containing organic compound with amidino lithium salt 2 -R’AMD) 3 Wherein R is one of methyl, ethyl, isopropyl, n-butyl or tert-butyl, R' is one of H, methyl, ethyl, isopropyl, n-butyl and tert-butyl, and the chemical reaction general formula is as follows:
by La% i Pr 2 -MeAMD) 3 For example, the preparation method specifically comprises the following steps:
(1) In a glove box, sequentially adding N, N' -diisopropylcarbodiimide (75.7 g,0.6 mol) and 300mL of tetrahydrofuran into a 1L three-necked flask, slowly dropwise adding diethyl ether solution of methyllithium (477 mL,0.6mol, 1.6M/L) when the temperature of the system is reduced to-30 ℃, gradually returning to room temperature after dropwise adding, changing the system into a light yellow solution, and stirring overnight;
(2) Sequentially adding LaCl into a 2L three-neck flask 3 1.5THF (70 g,0.2 mol), 400mL of tetrahydrofuran, the lithium salt solution in the step (1) was rapidly added dropwise to the system, the temperature of the system was increased from 30℃to 40℃and changed from white to yellow, and the mixture was stirred overnight after the completion of the dropwise addition;
(3) The volatile components were removed under vacuum, 200mL of n-hexane was added to the residue, and filtered to give a brown filtrate, which was concentrated under vacuum until supersaturated, and placed in a-30 ℃ refrigerator overnight, whereupon a large amount of yellow solid 91g was precipitated.
The nuclear magnetic resonance hydrogen spectrum of the yellow solid product is: 1 HNMR(C 6 D 6 1.18 (d, 12H), 1.66 (s, 3H), 3.42 (m, 2H), the yellow solid product was La # i Pr 2 -MeAMD) 3 The yield thereof was found to be 80%.
Application of lanthanum-containing organic compound in LaCl 3 1.5 preparation by reaction of THF with M (RCp), lithium diisopropylacetamidinate (RCp) 2 La( i Pr 2 -MeAMD), M is one of Li, na and K, R is one of H, methyl, ethyl and isopropyl, and the chemical reaction general formula is as follows:
in order (EtCp) 2 La( i Pr 2 -MeAMD), the preparation process comprises in particular the following steps:
(1) NaH (8.0 g,0.2 mol) and 100mL tetrahydrofuran are sequentially added into a 250mL three-neck flask, under stirring, a tetrahydrofuran solution of EtOP (0.2 mol,18.8 g) is slowly added dropwise, the temperature of the system is kept at about 15 ℃, in the dropping process, bubbles overflow from the liquid surface, the system gradually changes into a red solution, and the system is stirred overnight at room temperature;
(2) N, N' -diisopropylcarbodiimide (12.6 g,0.1 mol) and 100mL of tetrahydrofuran are sequentially added into a 250mL three-neck flask, the temperature of the system is reduced to-30 ℃, an ether solution of methyllithium (62.5 mL,0.1mol, 1.6M/L) is slowly added dropwise, and after the dropwise addition is completed, the mixture is stirred at room temperature overnight to obtain a light yellow lithium salt solution;
(3) Sequentially adding LaCl into a 1L three-neck flask 3 1.5THF (35.3 g,0.1 mol), 250mL of tetrahydrofuran, was slowly added dropwise with stirring to the sodium salt solution of (1), and the temperature of the system was increased from 25℃to 31 ℃. Stirring overnight at room temperature;
(4) And (3) dropwise adding the lithium salt solution obtained in the step (2) into the mixed solution, heating the mixed solution at reflux overnight after the system temperature is increased to 30 ℃ from 25 ℃, stopping heating, filtering after the system is restored to room temperature, and pumping out volatile components in vacuum to obtain brown sticky matters, and carrying out reduced pressure distillation (150 ℃/0.50 mbar) to obtain 37.6g yellow oily liquid.
The nuclear magnetic resonance hydrogen spectrum of the yellow oily liquid product was obtained: 1 HNMR(C 6 D 6 25 c). 0.89 (d, 12H), 1.19 (t, 6H), 1.48 (s, 3H), 2.53 (m, 4H), 3.15 (s, 2H), 6.06 (s, 3H), 6.18 (s, 3H), the yellow oily liquid product being (EtOP) 2 La( i Pr 2 -mead), with a yield of 80%.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims.
Claims (3)
1. Lanthanum-containing materialA process for producing an organic compound, characterized in that the organic compound has the chemical formula LaCl 3 1.5THF, wherein the organic compound is prepared by reflux reaction of lanthanum powder, trimethylchlorosilane and ethanol in THF solution, and the chemical reaction equation is as follows;
the preparation method of the lanthanum-containing organic compound specifically comprises the following steps:
s1, weighing lanthanum powder, adding tetrahydrofuran, rapidly stirring and mixing uniformly, adding trimethylchlorosilane while stirring, and mixing uniformly to obtain a mixed solution A;
s2, slowly dripping absolute ethyl alcohol into the mixed solution A, wherein small bubbles overflow from the liquid surface, the temperature of the system slightly rises, heating, refluxing and stirring for 4-6 hours after dripping is finished, and stopping the reaction until the system gradually turns into white turbid liquid from black turbid liquid;
s3, filtering the turbid liquid after the reaction to obtain a filter cake, washing the filter cake with n-hexane for 2-4 times, and finally drying the filter cake in vacuum to obtain white powder LaCl 3 ·1.5THF；
The mole ratio of the lanthanum powder, the trimethylchlorosilane and the ethanol is 1:3-4:3-4.
2. The method for producing a lanthanum containing organic compound according to claim 1, wherein the lanthanum powder has a particle size of 50 to 200 mesh.
3. The method for producing a lanthanum containing organic compound according to claim 1, wherein the temperature of the heating reflux in step S3 is 70 to 90 ℃.
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| CN1471494A (en) * | 2000-10-03 | 2004-01-28 | �ǵ�˹ | Rare earth or gallium additive composition, methods for preparing same and use thereof as catalyst |
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|---|---|---|---|---|
| CN1471494A (en) * | 2000-10-03 | 2004-01-28 | �ǵ�˹ | Rare earth or gallium additive composition, methods for preparing same and use thereof as catalyst |
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| Title |
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