CN107216346A - The method of the high-purity dimethyl cadmium of one pot process - Google Patents
The method of the high-purity dimethyl cadmium of one pot process Download PDFInfo
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- CN107216346A CN107216346A CN201710492821.5A CN201710492821A CN107216346A CN 107216346 A CN107216346 A CN 107216346A CN 201710492821 A CN201710492821 A CN 201710492821A CN 107216346 A CN107216346 A CN 107216346A
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- cadmium
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- dimethyl cadmium
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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 41
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000005580 one pot reaction Methods 0.000 title claims abstract description 28
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000012043 crude product Substances 0.000 claims abstract description 40
- 239000000047 product Substances 0.000 claims abstract description 27
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 23
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 230000026030 halogenation Effects 0.000 claims abstract description 19
- 238000005658 halogenation reaction Methods 0.000 claims abstract description 19
- -1 methyl halide Chemical class 0.000 claims abstract description 18
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- KPWJBEFBFLRCLH-UHFFFAOYSA-L cadmium bromide Chemical compound Br[Cd]Br KPWJBEFBFLRCLH-UHFFFAOYSA-L 0.000 claims description 10
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000007818 Grignard reagent Substances 0.000 claims description 7
- 150000004795 grignard reagents Chemical class 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- OKIIEJOIXGHUKX-UHFFFAOYSA-L cadmium iodide Chemical compound [Cd+2].[I-].[I-] OKIIEJOIXGHUKX-UHFFFAOYSA-L 0.000 claims description 4
- 230000006837 decompression Effects 0.000 claims description 4
- 239000000284 extract Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000010457 zeolite Substances 0.000 claims description 4
- OKJPEAGHQZHRQV-UHFFFAOYSA-N Triiodomethane Natural products IC(I)I OKJPEAGHQZHRQV-UHFFFAOYSA-N 0.000 claims description 3
- GZUXJHMPEANEGY-UHFFFAOYSA-N bromomethane Chemical compound BrC GZUXJHMPEANEGY-UHFFFAOYSA-N 0.000 claims description 3
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 3
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 229910021536 Zeolite Inorganic materials 0.000 claims description 2
- 229940075417 cadmium iodide Drugs 0.000 claims description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 2
- 150000004820 halides Chemical class 0.000 claims description 2
- 239000011343 solid material Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 238000005160 1H NMR spectroscopy Methods 0.000 abstract description 11
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 abstract description 7
- 238000010189 synthetic method Methods 0.000 abstract description 6
- 238000012360 testing method Methods 0.000 description 9
- 238000009835 boiling Methods 0.000 description 6
- 229940065285 cadmium compound Drugs 0.000 description 5
- 150000001662 cadmium compounds Chemical class 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- KVVGSXJGEUULNM-UHFFFAOYSA-N C[Cd]C Chemical compound C[Cd]C KVVGSXJGEUULNM-UHFFFAOYSA-N 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 150000001661 cadmium Chemical class 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- LGRLWUINFJPLSH-UHFFFAOYSA-N methanide Chemical compound [CH3-] LGRLWUINFJPLSH-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000007787 solid Substances 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
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- NEHMKBQYUWJMIP-OUBTZVSYSA-N chloromethane Chemical group Cl[13CH3] NEHMKBQYUWJMIP-OUBTZVSYSA-N 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 239000004611 light stabiliser 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
- 150000007524 organic acids Chemical class 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 150000003752 zinc compounds Chemical class 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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the method for the high-purity dimethyl cadmium of one pot process, prepare raw material first, raw material includes magnesium powder, halogenation cadmium, methyl halide and ether；Then the synthesis of crude product, raw material disposably puts into reactor；Then the separation of crude product；The purifying of last crude product.Directly synthesized using one kettle way, technique is easy, simple to operate, the cycle is short and product purity is high.Through1H NMR detect that the dimethyl cadmium content that the synthetic method is obtained is detected more than 99%, and by ICP OES, dimethyl cadmium high purity 99.9999%.
Description
Technical field
The present invention relates to the synthetic method of high-purity dimethyl cadmium of semicon industry, more particularly to one pot process are high-purity
The method of dimethyl cadmium.
Background technology
Alkyl cadmium of organic cadmium compound in very important purposes, organic cadmium compound is found to have recently and fragrant cadmium
The catalyst of polymerisation it has been used as, the cadmium salt of organic acid can be used as the light and heat stabilizer of plastics.
Organic cadmium compound makes them have the synthesis capability of uniqueness for the gentle reactivity of certain organo-functional group.Have
Machine cadmium compound is usually nonpolar liquid or low melting point solid, is dissolved in most of organic compounds, can be with oxygen or water
Vigorous reaction, the sensitiveness to oxygen is poorer than organic Zinc compounds, and stability is also low.
Representative dimethyl cadmium in organic cadmium compound is mainly used as the catalyst of the organic syntheses such as alkylation and polymerization, also uses
Semiconductor hetero-junction material is manufactured in metal organic chemical deposition method (MOCVD), or is partly led for depositing cadmium sulfide, cadmium telluride etc.
Body thin film.In addition the additive of mineral oil is also acted as to improve wearability.
For the synthetic method of dimethyl cadmium, the method for fractional steps, the i.e. first step are generally used first with magnesium powder, methyl halogenation
Thing synthesizes grignard reagent in ether；Second step is small by several times by abundant dry and fine ground halogenation cadmium under the conditions of strong agitation
Batch is added in above-mentioned grignard reagent.Ether fierceness boiling in course of reaction, cadmium salt dissolves rapidly, after having added, and controls temperature
No more than 80 DEG C, it is decompressed to 1.73KPa under nitrogen atmosphere again after boiling off most of ether with still under nitrogen flowing, steams
The receiving tank that is cooled down with liquid nitrogen of dimethyl cadmium-ether mixtures receive.Steamed again with still is careful from above-mentioned colorless fraction
Ether is removed, is removed after the first cut, target product is collected, organic purity of target product is more than 90%.Above-mentioned synthetic method
Although the dimethyl cadmium that the method for fractional steps of use can be obtained, purity is relatively low.The method of fractional steps first synthesizes grignard reagent, and reaction can not
In control, and the follow-up addition grignard reagent by halogenation cadmium, gradation small lot is needed to add, reaction time is longer.
Therefore, research and develop that a kind of technique is easy, simple to operate, the cycle is short and product purity reach more than 99% high-purity diformazan
The preparation method of base cadmium is extremely urgent.
The content of the invention
The purpose of the present invention be overcome the shortcomings of the prior art method of fractional steps synthesis dimethyl cadmium there is provided a kind of technique simplicity,
The simple to operate, cycle is short and method of the high-purity dimethyl cadmium of the high one pot process of product purity.
The purpose of the present invention is achieved through the following technical solutions：
The method of the high-purity dimethyl cadmium of one pot process, feature is：Comprise the following steps：
1) preparation of raw material, raw material includes magnesium powder, halogenation cadmium, methyl halide and ether；
2) synthesis of crude product, raw material disposably puts into reactor；
3) separation of crude product；
4) purifying of crude product.
Further, the method for the high-purity dimethyl cadmium of above-mentioned one pot process, wherein, step 1), ether is removed water to
Below 100ppm.
Further, the method for the high-purity dimethyl cadmium of above-mentioned one pot process, wherein, step 2), first put into solid former
Material, then put into liquid charging stock.
Further, the method for the high-purity dimethyl cadmium of above-mentioned one pot process, wherein, magnesium powder and methyl in course of reaction
The grignard reagent concentration of halide synthesis is in 1~3mol.L-1。
Further, the method for the high-purity dimethyl cadmium of above-mentioned one pot process, wherein, the methyl halide is chloromethane
One or more in alkane, bromomethane, iodomethane.
Further, the method for the high-purity dimethyl cadmium of above-mentioned one pot process, wherein, the halogenation cadmium be caddy,
One or more in cadmium bromide, cadmium iodide.
Further, the method for the high-purity dimethyl cadmium of above-mentioned one pot process, wherein, the magnesium powder and methyl halide
Mol ratio be (1.05~1.2)：1, the mol ratio of methyl halide and halogenation cadmium is (1.05~1.2)：1.
Further, the method for the high-purity dimethyl cadmium of above-mentioned one pot process, wherein, step 2), into flask, add
Halogenation cadmium, magnesium powder, methyl halide, ether, under the condensation of coil condensation pipe, open stirring, react 8~10h, until reaction
Terminate after mixed liquor in kettle becomes viscous, mixed liquor no longer flows back, obtain crude product.
Further, the method for the high-purity dimethyl cadmium of above-mentioned one pot process, wherein, step 3), crude product is synthesized
Reactor heating normal pressure steams ether solvent, and full access vacuum decompression extracts remaining dimethyl cadmium-ether mixtures, mixture out
The receiving tank cooled down with liquid nitrogen is received, and is received gained mixture heating and is removed ether therein.
Further, the method for the high-purity dimethyl cadmium of above-mentioned one pot process, wherein, step 4), crude product is in glove box
In pour into add zeolite single port band temperature cover flask in carry out rectifying, obtain target product.
Further, the method for the high-purity dimethyl cadmium of above-mentioned one pot process, wherein, step 4), cleansing temp control
At 105~115 DEG C.
The present invention has significant advantage and beneficial effect compared with prior art, embodies in the following areas：
The present invention is directly synthesized using one kettle way, and technique is easy, simple to operate, the cycle is short and product purity is high.Through1H-
NMR detects that the dimethyl cadmium content that the synthetic method is obtained detects that dimethyl cadmium is pure more than 99%, and by ICP-OES
Degree up to 99.9999%.Realize and substitute same kind of products at abroad, response country is comprehensively domestic for presoma needed for semicon industry
The call of change.
Embodiment
In order to which technical characteristic, purpose and effect to the present invention are more clearly understood from, specific implementation is now described in detail
Scheme.
The processing step of the high-purity dimethyl cadmium of one pot process is：
1) preparation of raw material, raw material includes magnesium powder, halogenation cadmium, methyl halide and ether；Ether removes water to 100ppm
Below；Methyl halide is the one or more in chloromethanes, bromomethane, iodomethane；Halogenation cadmium is caddy, cadmium bromide, iodine
One or more in cadmium；
2) synthesis of crude product, raw material disposably puts into reactor；Solid material is first put into, then puts into liquid charging stock；Reaction
During the grignard reagent concentration that is synthesized with methyl halide of magnesium powder in 1~3mol.L-1；Mole of magnesium powder and methyl halide
Than for (1.05~1.2)：1, the mol ratio of methyl halide and halogenation cadmium is (1.05~1.2)：1；Crude yield 85% with
On；
3) separation of crude product；Separating obtained product purity is more than 90%；
4) purifying of crude product, cleansing temp is controlled at 105~115 DEG C；Products obtained therefrom purity is purified more than 99%；It is pure
The first cut proportion evaporates in 20~30%, second cut target product proportions 40~60%, the 3rd during change
Divide proportion 10~40%.
The implementation condition used in embodiment can further be adjusted according to specific requirement, and unreceipted implementation condition is usual
For normal condition.In addition, when not having specified otherwise, the consumption of component is the amount of material (mol) and percentage (%), and product refers to
Mark is obtained according to industry standard test.
Following embodiment and comparative example are under conditions of stirring, with magnesium powder, halogenation cadmium, methyl halide, ether
For raw material, synthesis, crude product separation, the obtained target product of purifying crude are sequentially passed through.Building-up process equipment therefor includes tetra- mouthfuls of 2L
Flask, 2L heating mantles, agitating device, thermometer boss, thermometer, coil condensation pipe, refrigerator etc.；Crude product separates equipment therefor
Including 2L four-hole boiling flasks, 2L heating mantles, agitating device, thermometer boss, thermometer, cold-trap receiving tank, vavuum pump etc.；Crude product
Purifying equipment therefor includes 1L single port bands temperature set flask, 1L heating mantles, rectifying column, 1L single-necked flasks, 500ml single-necked flasks, boiling
Stone etc..
Embodiment 1
Crude product is synthesized：Into above-mentioned 2L four-hole boiling flasks, 1.0mol caddies, 1.21mol magnesium powders, 1.1mol iodine first are added
Alkane, 7.1mol ether, under the condensation of coil condensation pipe, open stirring, stir speed (S.S.) is set as 600R/min, reacts 8-10h,
Until terminating after the mixed liquor in reactor becomes viscous, mixed liquor no longer flows back, gained crude product warp1H-NMR tests confirm as two
Cadmium methide, crude product is used for later separation.
Crude product is separated：2L reactors during above-mentioned crude product is synthesized are heated to 50 DEG C of normal pressures and steam most of ether solvent
Afterwards, full access vacuum decompression extracts remaining dimethyl cadmium-ether mixtures out, and the receiving tank that the mixture is cooled down with liquid nitrogen connects
Receive, receive the heating of gained mixture until 90 DEG C remove ether therein, the test of gained crude product1H-NMR, the organic purity of product
93%, dimethyl cadmium content is 0.89mol, crude yield 96%, for subsequent purification in crude product.
Purifying crude：Essence is carried out in the single port band temperature set flask that above-mentioned crude product is poured into 1L addition zeolites in glove box
Evaporate, obtain target product 0.53mol, the test of gained target product1H-NMR, organic purity is 99.5%；Test ICP-OES, nothing
Machine purity is 99.99996%.
Embodiment 2
Crude product is synthesized：Into above-mentioned 2L four-hole boiling flasks, 1.0mol caddies, 1.21mol magnesium powders, 1.1mol bromine first are added
Alkane, 7.1mol ether, under the condensation of coil condensation pipe, open stirring, stir speed (S.S.) is set as 600R/min, reacts 8-10h,
Until terminating after the mixed liquor in reactor becomes viscous, mixed liquor no longer flows back, gained crude product warp1H-NMR tests confirm as two
Cadmium methide, crude product is used for later separation.
Crude product is separated：2L reactors during above-mentioned crude product is synthesized are heated to 50 DEG C of normal pressures and steam most of ether solvent
Afterwards, full access vacuum decompression extracts remaining dimethyl cadmium-ether mixtures out, and the receiving tank that the mixture is cooled down with liquid nitrogen connects
Receive, receive the heating of gained mixture until 90 DEG C remove ether therein, the test of gained crude product1H-NMR, the organic purity of product
94%, dimethyl cadmium content is 0.91mol, crude yield 91%, for subsequent purification in crude product.
Purifying crude：Essence is carried out in the single port band temperature set flask that above-mentioned crude product is poured into 1L addition zeolites in glove box
Evaporate, obtain target product 0.46mol, the test of gained target product1H-NMR, organic purity is 99.6%；Test ICP-OES, nothing
Machine purity is 99.99994%.
Comparative example 1
The basic be the same as Example 1 of this example, unlike, halogenation cadmium used is cadmium bromide in this example, and consumption is also 1mol.
Crude product is tested1Dimethyl cadmium content is 0.91mol, crude yield in H-NMR, the organic purity 94% of product, crude product
91%；Gained target product is tested1H-NMR, organic purity is 99.7%；ICP-OES is tested, inorganic purity is
99.99998%.
Comparative example 2
The basic be the same as Example 2 of this example, unlike, halogenation cadmium used is cadmium bromide in this example, and consumption is also 1mol.
Crude product is tested1Dimethyl cadmium content is 0.89mol, crude yield in H-NMR, the organic purity 92% of product, crude product
89%；Gained target product is tested1H-NMR, organic purity is 99.4%；ICP-OES is tested, inorganic purity is
99.99993%.
The present invention is directly synthesized using one kettle way, and technique is easy, simple to operate, the cycle is short and product purity is high.Through1H-
NMR detects that the dimethyl cadmium content that the synthetic method is obtained detects that dimethyl cadmium is pure more than 99%, and by ICP-OES
Degree up to 99.9999%.Realize and substitute same kind of products at abroad, response country is comprehensively domestic for presoma needed for semicon industry
The call of change.
It should be noted that：The preferred embodiment of the present invention is the foregoing is only, the power of the present invention is not limited to
Sharp scope；Simultaneously more than description, should can understand and implement for the special personage of correlative technology field, thus it is other without departing from
The equivalent change or modification completed under disclosed spirit, should be included in claim.
Claims (11)
1. the method for the high-purity dimethyl cadmium of one pot process, it is characterised in that：Comprise the following steps：
1) preparation of raw material, raw material includes magnesium powder, halogenation cadmium, methyl halide and ether；
2) synthesis of crude product, raw material disposably puts into reactor；
3) separation of crude product；
4) purifying of crude product.
2. the method for the high-purity dimethyl cadmium of one pot process according to claim 1, it is characterised in that：Step 1), ether
Remove water to below 100ppm.
3. the method for the high-purity dimethyl cadmium of one pot process according to claim 1, it is characterised in that：Step 2), first throw
Enter solid material, then put into liquid charging stock.
4. the method for the high-purity dimethyl cadmium of one pot process according to claim 1, it is characterised in that：Magnesium in course of reaction
The grignard reagent concentration that powder is synthesized with methyl halide is in 1~3mol.L-1。
5. the method for the high-purity dimethyl cadmium of one pot process according to claim 1, it is characterised in that：The methyl halogenation
Thing is the one or more in chloromethanes, bromomethane, iodomethane.
6. the method for the high-purity dimethyl cadmium of one pot process according to claim 1, it is characterised in that：The halogenation cadmium is
One or more in caddy, cadmium bromide, cadmium iodide.
7. the method for the high-purity dimethyl cadmium of one pot process according to claim 1, it is characterised in that：The magnesium powder and first
The mol ratio of base halide is (1.05~1.2)：1, the mol ratio of methyl halide and halogenation cadmium is (1.05~1.2)：1.
8. the method for the high-purity dimethyl cadmium of one pot process according to claim 1, it is characterised in that：Step 2), to burning
In bottle, halogenation cadmium, magnesium powder, methyl halide, ether are added, under the condensation of coil condensation pipe, opens and stirs, reaction 8~
10h, until terminating after the mixed liquor in reactor becomes viscous, mixed liquor no longer flows back, obtains crude product.
9. the method for the high-purity dimethyl cadmium of one pot process according to claim 1, it is characterised in that：Step 3), will be thick
The reactor heating normal pressure of product synthesis steams ether solvent, and full access vacuum decompression extracts remaining dimethyl cadmium-ether mixing out
Thing, the receiving tank that mixture is cooled down with liquid nitrogen is received, and is received gained mixture heating and is removed ether therein.
10. the method for the high-purity dimethyl cadmium of one pot process according to claim 1, it is characterised in that：Step 4), crude product
Poured into glove box in the single port band temperature set flask for add zeolite and carry out rectifying, obtain target product.
11. the method for the high-purity dimethyl cadmium of one pot process according to claim 1, it is characterised in that：Step 4), purifying
Temperature control is at 105~115 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115043857A (en) * | 2022-05-17 | 2022-09-13 | 江苏南大光电材料股份有限公司 | Preparation method of semiconductor grade dimethyl cadmium |
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|---|---|---|---|---|
| US5245065A (en) * | 1991-11-19 | 1993-09-14 | Shell Research Limited | Process for the preparation of di-alkyl compounds of group 2b metals |
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|---|
| 韩长日 等主编: "《电子与信息化学助剂生产与应用技术》", 30 June 2009, 北京：中国石化出版社 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115043857A (en) * | 2022-05-17 | 2022-09-13 | 江苏南大光电材料股份有限公司 | Preparation method of semiconductor grade dimethyl cadmium |
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