CN115043857A - Preparation method of semiconductor grade dimethyl cadmium - Google Patents
Preparation method of semiconductor grade dimethyl cadmium Download PDFInfo
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- CN115043857A CN115043857A CN202210538362.0A CN202210538362A CN115043857A CN 115043857 A CN115043857 A CN 115043857A CN 202210538362 A CN202210538362 A CN 202210538362A CN 115043857 A CN115043857 A CN 115043857A
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- cadmium
- dimethyl cadmium
- butyl ether
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- grade dimethyl
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- VQNPSCRXHSIJTH-UHFFFAOYSA-N cadmium(2+);carbanide Chemical compound [CH3-].[CH3-].[Cd+2] VQNPSCRXHSIJTH-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000004065 semiconductor Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 47
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 30
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 22
- DVSDBMFJEQPWNO-UHFFFAOYSA-N methyllithium Chemical compound C[Li] DVSDBMFJEQPWNO-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000012298 atmosphere Substances 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000004821 distillation Methods 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- SZNYYWIUQFZLLT-UHFFFAOYSA-N 2-methyl-1-(2-methylpropoxy)propane Chemical compound CC(C)COCC(C)C SZNYYWIUQFZLLT-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- AOPDRZXCEAKHHW-UHFFFAOYSA-N 1-pentoxypentane Chemical compound CCCCCOCCCCC AOPDRZXCEAKHHW-UHFFFAOYSA-N 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000002808 molecular sieve Substances 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 26
- 238000003756 stirring Methods 0.000 description 18
- 238000009835 boiling Methods 0.000 description 16
- 239000012043 crude product Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- 238000005160 1H NMR spectroscopy Methods 0.000 description 6
- 239000007818 Grignard reagent Substances 0.000 description 6
- 150000004795 grignard reagents Chemical class 0.000 description 6
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 6
- 229940065285 cadmium compound Drugs 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 229910021536 Zeolite Inorganic materials 0.000 description 4
- 238000009529 body temperature measurement Methods 0.000 description 4
- 150000001662 cadmium compounds Chemical class 0.000 description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000011261 inert gas Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000010457 zeolite Substances 0.000 description 4
- 150000001661 cadmium Chemical class 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000011112 process operation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 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
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000007039 two-step reaction Methods 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
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses a preparation method of semiconductor grade dimethyl cadmium, which comprises the steps of adding anhydrous cadmium dichloride and an ether solvent into a reactor under the protection of inert atmosphere, wherein the molar ratio of the anhydrous cadmium dichloride to the ether solvent is 1: 3.5-5; slowly dropwise adding a methyllithium n-butyl ether solution into the system under a low-temperature condition to react to obtain dimethyl cadmium; after the reaction is finished, carrying out atmospheric distillation and rectification to obtain high-purity dimethyl cadmium; and (3) pressurizing and filtering the high-purity dimethyl cadmium by using a filter to obtain the semiconductor-grade dimethyl cadmium. Dimethyl cadmium is synthesized by a one-step method, cadmium dichloride and a solvent are added into a reaction bottle, a methyllithium n-butyl ether solution is dropwise added at a low temperature, the dimethyl cadmium is purified by rectification, particles are removed by a filter, and the high-purity semiconductor grade dimethyl cadmium is obtained.
Description
Technical Field
The invention relates to a preparation method of semiconductor grade dimethyl cadmium.
Background
Organic cadmium compounds, the alkyl and aromatic cadmium compounds of which are now used as catalysts for polymerization reactions, and the cadmium salts of organic acids, which are used as heat and light stabilizers for plastics, have found very important applications.
The mild reactivity of organic cadmium compounds to certain organic functional groups makes them uniquely useful for synthesis, and organic cadmium compounds are generally non-polar liquids or low melting solids, are soluble in most organic solvents, react violently with oxygen or water, are less sensitive to oxygen than organozinc compounds, and are less stable.
Dimethyl cadmium, a representative compound in organic cadmium compounds, is mainly used as a catalyst for organic synthesis and polymerization such as alkylation and the like, is also used for manufacturing semiconductor heterojunction materials by a metal organic chemical deposition (MOCVD) method, or is used for depositing semiconductor films such as cadmium sulfide, cadmium telluride and the like, and can also be used as an additive of mineral oil to improve the wear resistance.
For the synthesis method of the dimethyl cadmium, a fractional method is generally adopted, namely, magnesium powder and methyl halide are firstly utilized to synthesize a Grignard reagent in diethyl ether in the first step; in the second step, the fully dried and ground cadmium halide is added to the grignard reagent in small batches under vigorous stirring. In the reaction process, ether is boiled violently, cadmium salt is dissolved rapidly, after the cadmium salt is added, the temperature is controlled not to exceed 80 ℃, most of ether is evaporated by a fractionating column under nitrogen flow, then the pressure is reduced to 1.73KPa under nitrogen atmosphere, and the evaporated dimethyl cadmium-ether mixture is received by a receiving tank cooled by liquid nitrogen. And then distilling off diethyl ether from the colorless fraction by using a fractionating column, removing low boiling point substances, and collecting a target product, wherein the organic purity of the target product is more than 90%. Although the dimethyl cadmium can be obtained by the step method adopted by the synthesis method, the purity is low. The Grignard reagent is synthesized by a fractional step method, the reaction is not controllable, and the cadmium halide is added into the Grignard reagent in a follow-up manner in small batches, so that the reaction period is longer.
Therefore, it is necessary to develop a preparation method of high-purity dimethyl cadmium, which has a simple process, a short period and a product purity of more than 99.9%.
Disclosure of Invention
The invention aims to overcome the defects of the existing fractional method for synthesizing the dimethyl cadmium and provide the method for preparing the high-purity dimethyl cadmium, which has the advantages of simple steps, convenient operation and short period.
The purpose of the invention is realized by the following technical scheme:
the preparation method of the semiconductor grade dimethyl cadmium is characterized in that: the method comprises the following steps:
1) under the protection of inert atmosphere, adding anhydrous cadmium dichloride and an ether solvent into a reactor, wherein the molar ratio of the anhydrous cadmium dichloride to the ether solvent is 1: 3.5-5;
2) slowly dropwise adding a methyllithium n-butyl ether solution into the system under a low-temperature condition to react to obtain dimethyl cadmium;
3) after the reaction is finished, carrying out atmospheric distillation and rectification to obtain high-purity dimethyl cadmium;
4) and (4) pressurizing and filtering the high-purity dimethyl cadmium by using a filter to obtain the semiconductor-grade dimethyl cadmium.
Further, in the preparation method of the semiconductor grade dimethyl cadmium, the ether solvent is n-butyl ether, isobutyl ether or n-pentyl ether.
Further, in the preparation method of the semiconductor grade dimethyl cadmium, in the step 1), firstly, drying and dehydrating the n-butyl ether dissolved with the cadmium dichloride, drying 500g of the n-butyl ether by using 100g of a 4A molecular sieve for 48 hours, and sampling to analyze that the water content of the n-butyl ether is less than 50 ppm; and filtering and distilling the dried n-butyl ether to obtain the usable n-butyl ether solvent.
Further, in the preparation method of the semiconductor grade dimethyl cadmium, the system temperature is between 10 ℃ below zero and 15 ℃ below zero, and the reaction is returned to room temperature and stirred for 3 hours after the reaction is finished.
Further, the preparation method of the semiconductor grade dimethyl cadmium comprises the step 2), wherein the concentration of the methyl lithium n-butyl ether solution dropwise added into the system is 1.5mol/L, and the molar ratio of the cadmium dichloride to the methyl lithium is 1-1.5: 2
Further, in the preparation method of the semiconductor grade dimethyl cadmium, step 3), atmospheric distillation and rectification are carried out under inert atmosphere.
Further, in the above method for preparing semiconductor grade dimethyl cadmium, in step 3), the filter is a 0.01um teflon filter manufactured by kobaite corporation, and the pressurized gas is nitrogen.
Further, in the above method for preparing semiconductor grade dimethyl cadmium, the inert atmosphere is nitrogen or argon.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and is embodied in the following aspects:
the traditional Grignard reagent method uses ether with low boiling point as solvent, the ether is flammable and explosive, and the reaction is not controllable; the invention adopts high boiling point ether solvent such as n-butyl ether, the reaction process is safe, and the initiation of the reaction is controllable;
secondly, the traditional reaction is a two-step reaction, the Grignard reagent is firstly synthesized, and then the cadmium dichloride is added in batches, so the operation steps are complicated and are not easy to implement in the amplification process; the method synthesizes the dimethyl cadmium by a one-step method, the cadmium dichloride and the solvent are added into a reaction bottle, the methyl lithium n-butyl ether solution is dripped at low temperature, the dimethyl cadmium is purified by rectification, the particles are removed by a filter, the high-purity semiconductor grade dimethyl cadmium is obtained, any raw material does not need to be added in batches in the reaction process, the process operation steps are simplified, and the safety in the reaction process is greatly improved;
③ the high-boiling point ethers in the subsequent rectification process of the dimethyl cadmium are easier to purify the high-purity dimethyl cadmium without solvent than the ether.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments will now be described in detail.
The preparation process of the semiconductor grade dimethyl cadmium comprises the following steps:
1) under the protection of inert atmosphere, adding anhydrous cadmium dichloride and an ether solvent into a reactor under the inert atmosphere of nitrogen or argon, wherein the molar ratio of the anhydrous cadmium dichloride to the ether solvent is 1: 3.5-5; the ether solvent is high boiling point and good dissolubility, such as n-butyl ether or isobutyl ether, n-amyl ether, etc.;
firstly, drying and dehydrating n-butyl ether in which cadmium dichloride is dissolved, drying 500g of the n-butyl ether by using a 100g of 4A molecular sieve for 48 hours, and sampling to analyze that the water content of the n-butyl ether is less than 50 ppm; filtering and distilling the dried n-butyl ether to obtain a usable n-butyl ether solvent;
2) slowly dropwise adding a methyllithium n-butyl ether solution into the system at the temperature of between 10 ℃ below zero and 15 ℃ below zero to react to obtain dimethyl cadmium, and after the reaction is finished, recovering the room temperature and stirring for 3 hours; the concentration of the methyl lithium n-butyl ether solution dripped into the system is 1.5mol/L, and the molar ratio of the cadmium dichloride to the methyl lithium is 1-1.5: 2;
3) after the reaction is finished, carrying out normal pressure distillation and rectification in an inert atmosphere, wherein the inert atmosphere is nitrogen or argon, and obtaining high-purity dimethyl cadmium;
4) and (3) pressurizing and filtering the high-purity dimethyl cadmium by using a filter to obtain semiconductor-grade dimethyl cadmium, wherein the filter is a 0.01um polytetrafluoroethylene filter of Corbert company, and the pressurized gas is nitrogen.
Example 1
In an inert gas glove box, 1mol of anhydrous cadmium dichloride and 400ml of n-butyl ether are added into a 2L reaction bottle, and 2mol of methyl lithium n-butyl ether solution is dripped into the reaction bottle under the condition of fast stirring at the temperature of 15 ℃ below zero; the temperature of the system is kept at about minus 10 ℃ in the dripping process, the dripping is carried out while stirring, and after the dripping is finished, the stirring is maintained for 3 hours after the temperature is raised to the room temperature. After the reaction is finished, crude dimethyl cadmium is distilled out under normal pressure under the condition of stirring to obtain 125g of product, the yield is 85 percent, and the product passes the identification of nuclear magnetic hydrogen spectrum.
And (3) crude product purification: pouring the crude product into 500ml of single-neck flask with temperature measurement and added with zeolite in a glove box for rectification, heating to 106 ℃, removing impurities with low boiling point and high boiling point, receiving 60% of target product to obtain 70g of target product, and testing the target product 1 H-NMR, organic purity 99.9%; ICP-OES was tested and the inorganic purity was 99.9999%.
Example 2
In an inert gas glove box, 1.1mol of anhydrous cadmium dichloride and 400ml of n-butyl ether are added into a 2L reaction bottle, and 2mol of methyllithium n-butyl ether solution is dripped into the reaction bottle under the condition of rapid stirring at the temperature of 15 ℃ below zero; the temperature of the system is kept at about minus 10 ℃ in the dripping process, the dripping is carried out while stirring, and after the dripping is finished, the stirring is maintained for 3 hours after the temperature is raised to the room temperature. After the reaction is finished, the crude dimethyl cadmium is distilled out under normal pressure under the stirring condition to obtain 130g of product with the yield of 88 percent, and the product passes the identification of nuclear magnetic hydrogen spectrum.
And (3) crude product purification: pouring the crude product into 500ml of single-neck flask with temperature measurement and added with zeolite in a glove box for rectification, heating to 106 ℃, removing impurities with low boiling point and high boiling point, receiving 60% of target product to obtain 70g of target product, and testing the target product 1 H-NMR, organic purity 99.9%; ICP-OES was tested and the inorganic purity was 99.9999%.
Example 3
In an inert gas glove box, 1.3mol of anhydrous cadmium dichloride and 400ml of n-butyl ether are added into a 2L reaction bottle, and 2mol of methyllithium n-butyl ether solution is dripped into the reaction bottle under the condition of rapid stirring at the temperature of 15 ℃ below zero; the temperature of the system is kept at about minus 10 ℃ in the dripping process, the dripping is carried out while stirring, and after the dripping is finished, the stirring is maintained for 3 hours after the temperature is raised to the room temperature. After the reaction is finished, the crude dimethyl cadmium is distilled out under normal pressure under the stirring condition to obtain 140g of product, the yield is 95%, and the product passes the identification of nuclear magnetic hydrogen spectrum.
And (3) crude product purification: pouring the crude product into 500ml of a single-neck flask with a temperature measurement and added with zeolite in a glove box for rectification, heating to 106 ℃, removing impurities with low boiling point and impurities with high boiling point, receiving 60% of a target product to obtain 70g of the target product, and testing the target product 1 H-NMR, organic purity 99.9%; ICP-OES was tested and the inorganic purity was 99.9999%.
Example 4
In an inert gas glove box, 1.5mol of anhydrous cadmium dichloride and 400ml of n-butyl ether are added into a 2L reaction bottle, and 2mol of methyllithium n-butyl ether solution is dripped into the reaction bottle under the condition of fast stirring at the temperature of 15 ℃ below zero; the temperature of the system is kept at about minus 10 ℃ in the dripping process, the dripping is carried out while stirring, and after the dripping is finished, the stirring is maintained for 3 hours after the temperature is raised to the room temperature. After the reaction is finished, the crude dimethyl cadmium is distilled out under normal pressure under the stirring condition to obtain 138g of product with the yield of 94 percent, and the product passes the identification of nuclear magnetic hydrogen spectrum.
And (3) crude product purification: pouring the crude product into 500ml of single-neck flask with temperature measurement and added with zeolite in a glove box for rectification, heating to 106 ℃, removing impurities with low boiling point and high boiling point, receiving 60% of target product to obtain 70g of target product, and testing the target product 1 H-NMR, organic purity 99.9%; ICP-OES is tested, and the inorganic purity is 99.9999 percent
Rectifying in a flask, heating to 106 deg.C, removing low boiling point impurities and high boiling point impurities, receiving target product 60%, to obtain target product 160g, and testing the target product 1 H-NMR, organic purity 99.9%; ICP-OES was tested and the inorganic purity was 99.9999%.
In conclusion, the mixture ratio in example 3 is the optimum ratio.
The high-purity dimethyl cadmium is pressurized and filtered by a 0.01um filter into a steel cylinder, and then the steel cylinder can be sent to customers for use.
In conclusion, the invention synthesizes the dimethyl cadmium by a one-step method, the cadmium dichloride and the solvent are added into the reaction bottle, the methyl lithium n-butyl ether solution is dripped at low temperature, the dimethyl cadmium is purified by rectification, the particles are removed by the filter, the high-purity semiconductor grade dimethyl cadmium is obtained, any raw material is not required to be added in batches in the reaction process, the process operation steps are simplified, and the safety in the reaction process is greatly improved.
The high-boiling-point ether solvent such as n-butyl ether is adopted, the reaction process is safe, and the initiation of the reaction is controllable; compared with ether, the high boiling point ether in the subsequent rectification process of dimethyl cadmium can purify the high-purity dimethyl cadmium without solvent more easily.
Warp beam 1 H-NMR detection shows that the organic content of the dimethyl cadmium obtained by the preparation method is more than 99.9 percent, and ICP-OES detection shows that the inorganic purity of the obtained dimethyl cadmium is as high as 99.9999 percent.
It should be noted that: the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention; while the foregoing description will be apparent to those skilled in the relevant art and it is intended to cover in the appended claims all such modifications and changes as fall within the true spirit of the invention.
Claims (8)
1. The preparation method of the semiconductor grade dimethyl cadmium is characterized by comprising the following steps: the method comprises the following steps:
1) under the protection of inert atmosphere, adding anhydrous cadmium dichloride and an ether solvent into a reactor, wherein the molar ratio of the anhydrous cadmium dichloride to the ether solvent is 1: 3.5-5;
2) slowly dropwise adding a methyllithium n-butyl ether solution into the system under a low-temperature condition to react to obtain dimethyl cadmium;
3) after the reaction is finished, carrying out atmospheric distillation and rectification to obtain high-purity dimethyl cadmium;
4) and (4) pressurizing and filtering the high-purity dimethyl cadmium by using a filter to obtain the semiconductor-grade dimethyl cadmium.
2. The method of claim 1, wherein the step of preparing semiconductor grade dimethyl cadmium comprises: the ether solvent is n-butyl ether, isobutyl ether or n-pentyl ether.
3. The method of claim 1 or 2, wherein the semiconductor grade dimethyl cadmium comprises: step 1), firstly, drying and dehydrating the n-butyl ether dissolved with the cadmium dichloride, drying 500g of the n-butyl ether by using 100g of a 4A molecular sieve for 48 hours, and sampling and analyzing the water content of the n-butyl ether to be less than 50 ppm; and filtering and distilling the dried n-butyl ether to obtain the usable n-butyl ether solvent.
4. The method of claim 1, wherein the step of preparing semiconductor grade dimethyl cadmium comprises: the temperature of the system is between 10 ℃ below zero and 15 ℃ below zero, and the reaction is returned to room temperature and stirred for 3 hours.
5. The method of claim 1, wherein the step of preparing semiconductor grade dimethyl cadmium comprises: and step 2), the concentration of the methyllithium n-butyl ether solution dropwise added into the system is 1.5mol/L, and the molar ratio of the cadmium dichloride to the methyllithium is 1-1.5: 2.
6. The method of claim 1, wherein the step of preparing semiconductor grade dimethyl cadmium comprises: and 3) distilling and rectifying under normal pressure in an inert atmosphere.
7. The method of claim 1, wherein the step of preparing semiconductor grade dimethyl cadmium comprises: and 4) the filter is a 0.01um polytetrafluoroethylene filter, and the pressurized gas is nitrogen.
8. The method of claim 1, wherein the step of preparing semiconductor grade dimethyl cadmium comprises: the inert atmosphere is nitrogen or argon.
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