CN109369697A - A kind of production method preparing trimethyl aluminium - Google Patents
A kind of production method preparing trimethyl aluminium Download PDFInfo
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- CN109369697A CN109369697A CN201811648901.6A CN201811648901A CN109369697A CN 109369697 A CN109369697 A CN 109369697A CN 201811648901 A CN201811648901 A CN 201811648901A CN 109369697 A CN109369697 A CN 109369697A
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- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 54
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 239000002131 composite material Substances 0.000 claims abstract description 27
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 23
- 239000000725 suspension Substances 0.000 claims abstract description 19
- 150000001351 alkyl iodides Chemical class 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 10
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003999 initiator Substances 0.000 claims abstract description 8
- KMGBZBJJOKUPIA-UHFFFAOYSA-N butyl iodide Chemical compound CCCCI KMGBZBJJOKUPIA-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000002243 precursor Substances 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910019804 NbCl5 Inorganic materials 0.000 claims description 12
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 238000004821 distillation Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 7
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 claims description 6
- 230000008595 infiltration Effects 0.000 claims description 6
- 238000001764 infiltration Methods 0.000 claims description 6
- -1 alkyl iodine Chemical compound 0.000 claims description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052740 iodine Inorganic materials 0.000 claims description 4
- 239000011630 iodine Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 241000208340 Araliaceae Species 0.000 claims 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims 1
- 235000003140 Panax quinquefolius Nutrition 0.000 claims 1
- 235000008434 ginseng Nutrition 0.000 claims 1
- 230000035484 reaction time Effects 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 239000012043 crude product Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- OKJPEAGHQZHRQV-UHFFFAOYSA-N Triiodomethane Natural products IC(I)I OKJPEAGHQZHRQV-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 238000007654 immersion Methods 0.000 description 5
- 239000006193 liquid solution Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000007818 Grignard reagent Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000004795 grignard reagents Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- CPOFMOWDMVWCLF-UHFFFAOYSA-N methyl(oxo)alumane Chemical compound C[Al]=O CPOFMOWDMVWCLF-UHFFFAOYSA-N 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 230000035935 pregnancy Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000010555 transalkylation reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of production methods for preparing trimethyl aluminium, it is characterized in that, it comprises the steps of: that (1) alkyl iodide is first added into reaction vessel, then catalyst and initiator is added into alkyl iodide, stir and obtain mixture suspension；(2) triethyl aluminum is added in whipping process into mixture suspension, control reaction temperature is 60~80 DEG C, the reaction time >=10h；(3) reaction solution and catalyst are separated after reaction, rectifying purifying obtains product trimethyl aluminium；Wherein, the catalyst is Sb2O3‑SnO2‑Nb2O5Composite catalyst, the initiator are 1- iodobutane.
Description
Technical field
The invention belongs to technical field of semiconductor more particularly to a kind of production methods for preparing trimethyl aluminium.
Background technique
Trimethyl aluminium (TMA) is a kind of important organo-metallic compound, be widely used in organic catalysis, organic synthesis,
The key areas such as polymer chemistry industry and science and techniques of defence.In recent years, it is catalyzed with metallocene, late transition metal and Nonmetallocene etc.
The rapid development of agent system, TMA (produce methylaluminoxane as most important co-catalyst in above-mentioned catalyst system is synthesized
Predominant starting material), importance is shown in organic industry especially polymer chemistry industry.The factory of foreign countries production TMA
Price is greatly improved in order to limit China in the research and development in catalyzed polyolefin field, the outlet restricted T MA China in family.Institute
To reduce catalyst cost about research and development and be formed with the new method of the synthesis TMA of independent intellectual property right with very heavy
The meaning wanted.
There are many related TMA synthetic method, and classify according to differential responses mechanism mainly includes reduction method, Grignard Reagent
Method, ultrasonic irradiation and alkyl exchange process etc..Complexity from environmental protection, cost and amplification technique etc. consideration, wherein
More feasible method is that transalkylation reaction conjunction occurs under catalyst appropriate effect for halogenated alkane and trialkylaluminium
At TMA.But the yield of catalyst synthesis TMA used at present is lower, and generally less than 85%, this just gives the purifying in later period and ring
Guarantor brings very big pressure, so that purifying process is complicated, higher cost is unfavorable for the industrialization of trimethyl aluminium preparation process.
Summary of the invention
In order to solve the above technical problems, including following step the present invention provides a kind of production method for preparing trimethyl aluminium
It is rapid:
(1) alkyl iodide is first added into reaction vessel, then catalyst and initiator is added into alkyl iodide, stir
Obtain mixture suspension；
(2) it is added triethyl aluminum in whipping process into mixture suspension, control reaction temperature is 60~80 DEG C, when reaction
Between >=10h；
(3) reaction solution and catalyst are separated after reaction, rectifying purifying obtains product trimethyl aluminium；
Wherein, the catalyst is Sb2O3-SnO2-Nb2O5Composite catalyst, the initiator are 1- iodobutane.
Further, the addition quality of the catalyst is the 1/8~1/7 of alkyl iodine quality；The addition quality of initiator
It is the 1/10 of alkyl iodine quality.
Further, the Sb2O3-SnO2-Nb2O5Composite catalyst the preparation method comprises the following steps:
1) precursor solution is configured, the precursor solution is SbCl3、NbCl5With the ethanol solution of 1,2-PD, forerunner
The mass percent of each component is respectively as follows: SbCl in liquid solution3 10%、NbCl55%~6%, the volume fraction of 1,2-PD is
100~150mL/L；
2) by SnO2Powder is immersed in the precursor solution, is sufficiently taken out after infiltration, is dried, be subsequently placed in 450~480
1~2h is calcined in DEG C environment, that is, obtains the Sb2O3-SnO2-Nb2O5Composite catalyst.
Further, the SnO2The immersion quality and precursor solution volume ratio of powder are 50~100g/L.
Further, the Sb2O3-SnO2-Nb2O5The surface-modified processing of composite catalyst, method of modifying are as follows: will
Sb2O3-SnO2-Nb2O5Composite catalyst is placed in closed container, uses N2Air in closed container is driven away, then by pregnancy
Base disilazane introduces in closed container, and the mixture in container is heated to 180~200 DEG C of 2~4h of heat preservation by sealing container,
Then container cooled to room temperature is separated by solid-liquid separation, drying obtains modified Sb2O3-SnO2-Nb2O5Composite catalyst.
Further, the rectification parameters are 120~130 DEG C of air-distillations.
As can be seen from the above technical solutions, the invention has the advantages that
Present invention improves over the methods for synthesizing trimethyl aluminium in the prior art, Experimental Comparison discovery, and what is prepared through the invention urges
Agent, so that the yield of trimethyl aluminium significantly improves, impurity content is reduced, and is conducive to subsequent purification technological design, is saved life
Cost is produced, subsequent processing and environmental protection pressure are reduced.
Specific embodiment
It is described in detail below with reference to embodiment:
Embodiment 1
A kind of production method preparing trimethyl aluminium comprising the steps of:
(1) it first is passed through nitrogen removal air to sealed reaction vessel, iodomethane 200g is added into container, then into alkyl iodide
26g Sb is added2O3-SnO2-Nb2O5Composite catalyst and 20g1- iodobutane stir and obtain mixture suspension；
(2) triethyl aluminum 100g is added in whipping process into mixture suspension, control reaction temperature is 60~80 DEG C, instead
It is 10h between seasonable；
(3) reaction solution and catalyst are separated after reaction, reaction solution rectifying purifying, rectification parameters are 120~130 DEG C normal
Pressure distillation, it is final to obtain product trimethyl aluminium crude product.
Sb described in the present embodiment2O3-SnO2-Nb2O5Composite catalyst the preparation method comprises the following steps:
1) precursor solution is configured, the precursor solution is SbCl3、NbCl5With the ethanol solution of 1,2-PD, forerunner
The mass percent of each component is respectively as follows: SbCl in liquid solution3 10%、NbCl55%, the volume fraction of 1,2-PD is
100mL/L；
2) by SnO2Powder is immersed in the precursor solution, SnO2The immersion quality and precursor solution volume ratio of powder
For 50g/L, is sufficiently taken out after infiltration, dry, be subsequently placed in 450 DEG C of environment and calcine 1h, that is, obtain the Sb2O3-SnO2-
Nb2O5Composite catalyst.
Embodiment 2
A kind of production method preparing trimethyl aluminium comprising the steps of:
(1) it first is passed through nitrogen removal air to sealed reaction vessel, iodomethane 200g is added into container, then into alkyl iodide
26g Sb is added2O3-SnO2-Nb2O5Composite catalyst and 20g1- iodobutane stir and obtain mixture suspension；
(2) triethyl aluminum 100g is added in whipping process into mixture suspension, control reaction temperature is 60~80 DEG C, instead
It is 10h between seasonable；
(3) reaction solution and catalyst being separated after reaction, rectifying purifying, rectification parameters are 120~130 DEG C of air-distillations,
It is final to obtain product trimethyl aluminium crude product.
Sb described in the present embodiment2O3-SnO2-Nb2O5Composite catalyst the preparation method comprises the following steps:
1) precursor solution is configured, the precursor solution is SbCl3、NbCl5With the ethanol solution of 1,2-PD, forerunner
The mass percent of each component is respectively as follows: SbCl in liquid solution3 10%、NbCl56%, the volume fraction of 1,2-PD is
120mL/L；
2) by SnO2Powder is immersed in the precursor solution, SnO2The immersion quality and precursor solution volume ratio of powder
For 70g/L, is sufficiently taken out after infiltration, dry, be subsequently placed in 460 DEG C of environment and calcine 1h, that is, obtain the Sb2O3-SnO2-
Nb2O5Composite catalyst.
Embodiment 3
A kind of production method preparing trimethyl aluminium comprising the steps of:
(1) it first is passed through nitrogen removal air to sealed reaction vessel, iodomethane 200g is added into container, then into alkyl iodide
26g Sb is added2O3-SnO2-Nb2O5Composite catalyst and 20g1- iodobutane stir and obtain mixture suspension；
(2) triethyl aluminum 100g is added in whipping process into mixture suspension, control reaction temperature is 60~80 DEG C, instead
It is 10h between seasonable；
(3) reaction solution and catalyst being separated after reaction, rectifying purifying, rectification parameters are 120~130 DEG C of air-distillations,
It is final to obtain product trimethyl aluminium crude product.
Sb described in the present embodiment2O3-SnO2-Nb2O5Composite catalyst the preparation method comprises the following steps:
1) precursor solution is configured, the precursor solution is SbCl3、NbCl5With the ethanol solution of 1,2-PD, forerunner
The mass percent of each component is respectively as follows: SbCl in liquid solution3 10%、NbCl56%, the volume fraction of 1,2-PD is
150mL/L；
2) by SnO2Powder is immersed in the precursor solution, SnO2The immersion quality and precursor solution volume ratio of powder
For 100g/L, is sufficiently taken out after infiltration, dry, be subsequently placed in 480 DEG C of environment and calcine 1h, that is, obtain the Sb2O3-SnO2-
Nb2O5Composite catalyst.
Embodiment 4
A kind of production method preparing trimethyl aluminium comprising the steps of:
(1) it first is passed through nitrogen removal air to sealed reaction vessel, iodomethane 200g is added into container, then into alkyl iodide
26g Sb is added2O3-SnO2-Nb2O5It is suspended to stir acquisition mixture for modified composite catalyst and 20g1- iodobutane
Liquid；
(2) triethyl aluminum 100g is added in whipping process into mixture suspension, control reaction temperature is 60~80 DEG C, instead
It is 10h between seasonable；
(3) reaction solution and catalyst being separated after reaction, rectifying purifying, rectification parameters are 120~130 DEG C of air-distillations,
It is final to obtain product trimethyl aluminium crude product.
Sb described in the present embodiment2O3-SnO2-Nb2O5Modified composite catalyst the preparation method comprises the following steps:
1) precursor solution is configured, the precursor solution is SbCl3、NbCl5With the ethanol solution of 1,2-PD, forerunner
The mass percent of each component is respectively as follows: SbCl in liquid solution3 10%、NbCl56%, the volume fraction of 1,2-PD is
150mL/L；
2) by SnO2Powder is immersed in the precursor solution, SnO2The immersion quality and precursor solution volume ratio of powder
It for 100g/L, is sufficiently taken out after infiltration, dries, be subsequently placed in 480 DEG C of environment and calcine 1h, is i.e. acquisition Sb2O3-SnO2-Nb2O5It is multiple
Close catalyst；
3) by Sb2O3-SnO2-Nb2O5Composite catalyst is placed in closed container, uses N2Air in closed container is driven away, so
Hexamethyldisilazane is introduced in closed container afterwards, sealing container, the mixture in container is heated to 180~200 DEG C of guarantors
Warm 2h, then container cooled to room temperature, is separated by solid-liquid separation, drying obtains modified Sb2O3-SnO2-Nb2O5Composite catalyzing
Agent.
Comparative example 1
A kind of production method preparing trimethyl aluminium comprising the steps of:
(1) it first is passed through nitrogen removal air to sealed reaction vessel, iodomethane 200g is added into container, then into alkyl iodide
26g Sb is added2O3As catalyst and 20g1- iodobutane, stirs and obtain mixture suspension；
(2) triethyl aluminum 100g is added in whipping process into mixture suspension, control reaction temperature is 60~80 DEG C, instead
It is 10h between seasonable；
(3) reaction solution and catalyst being separated after reaction, rectifying purifying, rectification parameters are 120~130 DEG C of air-distillations,
It is final to obtain product trimethyl aluminium crude product.
Comparative example 2
A kind of production method preparing trimethyl aluminium comprising the steps of:
(1) it first is passed through nitrogen removal air to sealed reaction vessel, iodomethane 200g is added into container, then into alkyl iodide
26g SnO is added2As catalyst and 20g1- iodobutane, stirs and obtain mixture suspension；
(2) triethyl aluminum 100g is added in whipping process into mixture suspension, control reaction temperature is 60~80 DEG C, instead
It is 10h between seasonable；
(3) reaction solution and catalyst being separated after reaction, rectifying purifying, rectification parameters are 120~130 DEG C of air-distillations,
It is final to obtain product trimethyl aluminium crude product.
Comparative example 3
A kind of production method preparing trimethyl aluminium comprising the steps of:
(1) it first is passed through nitrogen removal air to sealed reaction vessel, iodomethane 200g is added into container, then into alkyl iodide
26g Nb is added2O5As catalyst and 20g1- iodobutane, stirs and obtain mixture suspension；
(2) triethyl aluminum 100g is added in whipping process into mixture suspension, control reaction temperature is 60~80 DEG C, instead
It is 10h between seasonable；
(3) reaction solution and catalyst being separated after reaction, rectifying purifying, rectification parameters are 120~130 DEG C of air-distillations,
It is final to obtain product trimethyl aluminium crude product.
Embodiment 5
The content of trimethyl aluminium in difference testing example 1~4 and 1~3 gained trimethyl aluminium crude product of comparative example, and calculate corresponding
Trimethyl aluminium yield, the results are shown in Table 1.
Table 1
| Test group | The yield of trimethyl aluminium |
| Embodiment 1 | 90.6% |
| Embodiment 2 | 91.3% |
| Embodiment 3 | 90.8% |
| Embodiment 4 | 93.2% |
| Comparative example 1 | 71.7% |
| Comparative example 2 | 57.4% |
| Comparative example 3 | 68.4% |
As shown in Table 1, catalyst prepared by the present invention, compared with the prior art used in bismuth, vfanadium compound catalyst so that
The yield of trimethyl aluminium significantly improves, and impurity content is reduced, and is conducive to subsequent purification technological design, saves production cost.It is right
Than embodiment 4 and embodiment 2 it is found that modifying process of the present invention can further increase the catalytic activity of composite catalyst,
Yield is macroscopically shown as to further increase.
Technical solution provided by the present invention is described in detail above, for those of ordinary skill in the art,
Thought according to an embodiment of the present invention, there will be changes in the specific implementation manner and application range, in conclusion this theory
Bright book content should not be construed as limiting the invention.
Claims (6)
1. a kind of production method for preparing trimethyl aluminium, which is characterized in that comprise the steps of:
(1) alkyl iodide is first added into reaction vessel, then catalyst and initiator is added into alkyl iodide, stir
Obtain mixture suspension；
(2) it is added triethyl aluminum in whipping process into mixture suspension, control reaction temperature is 60~80 DEG C, when reaction
Between >=10h；
(3) reaction solution and catalyst are separated after reaction, rectifying purifying obtains product trimethyl aluminium；
Wherein, the catalyst is Sb2O3-SnO2-Nb2O5Composite catalyst, the initiator are 1- iodobutane.
2. a kind of production method for preparing trimethyl aluminium according to claim 1, which is characterized in that the catalyst adds
Enter 1/8~1/7 that quality is alkyl iodine quality；The addition quality of initiator is the 1/10 of alkyl iodine quality.
3. a kind of production method for preparing trimethyl aluminium according to claim 1 or 2, which is characterized in that the Sb2O3-
SnO2-Nb2O5Composite catalyst the preparation method comprises the following steps:
1) precursor solution is configured, the precursor solution is SbCl3、NbCl5With the ethanol solution of 1,2-PD, presoma
The mass percent of each component is respectively as follows: SbCl in solution3 10%、NbCl55%~6%, the volume fraction of 1,2-PD is
100~150mL/L；
2) by SnO2Powder is immersed in the precursor solution, is sufficiently taken out after infiltration, is dried, be subsequently placed in 450~480 DEG C
1~2h is calcined in environment, that is, obtains the Sb2O3-SnO2-Nb2O5Composite catalyst.
4. a kind of production method for preparing trimethyl aluminium according to claim 3, which is characterized in that the SnO2Powder
It impregnates quality and precursor solution volume ratio is 50~100g/L.
5. a kind of production method for preparing trimethyl aluminium according to claim 3, which is characterized in that the Sb2O3-SnO2-
Nb2O5The surface-modified processing of composite catalyst, method of modifying are as follows: by Sb2O3-SnO2-Nb2O5Composite catalyst is placed in closed appearance
In device, N is used2Air in closed container is driven away, is then introduced hexamethyldisilazane in closed container, sealing container,
Mixture in container is heated to 180~200 DEG C of 2~4h of heat preservation, then container cooled to room temperature, is separated by solid-liquid separation, dries
It is dry to obtain modified Sb2O3-SnO2-Nb2O5Composite catalyst.
6. a kind of production method for preparing trimethyl aluminium according to claim 1 or 2, which is characterized in that the rectifying ginseng
Number is 125~130 DEG C of atmospheric distillations.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4364873A (en) * | 1981-07-13 | 1982-12-21 | Ethyl Corporation | Method of making aluminum alkyls |
| US4364874A (en) * | 1981-07-13 | 1982-12-21 | Ethyl Corporation | Method of making aluminum alkyls |
| US4948906A (en) * | 1990-02-16 | 1990-08-14 | Ethyl Corporation | Trimethylaluminum process |
| CN1229797A (en) * | 1998-03-25 | 1999-09-29 | 中国石油化工总公司 | Synthetic process for alkyl aluminium |
| TW201506030A (en) * | 2013-08-12 | 2015-02-16 | Pentapro Chemical Inc | Producing method of organometallic compound |
| CN106831844A (en) * | 2017-02-10 | 2017-06-13 | 安徽博泰电子材料有限公司 | A kind of preparation method of trimethyl aluminium |
-
2018
- 2018-12-30 CN CN201811648901.6A patent/CN109369697A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4364873A (en) * | 1981-07-13 | 1982-12-21 | Ethyl Corporation | Method of making aluminum alkyls |
| US4364874A (en) * | 1981-07-13 | 1982-12-21 | Ethyl Corporation | Method of making aluminum alkyls |
| US4948906A (en) * | 1990-02-16 | 1990-08-14 | Ethyl Corporation | Trimethylaluminum process |
| CN1229797A (en) * | 1998-03-25 | 1999-09-29 | 中国石油化工总公司 | Synthetic process for alkyl aluminium |
| TW201506030A (en) * | 2013-08-12 | 2015-02-16 | Pentapro Chemical Inc | Producing method of organometallic compound |
| CN106831844A (en) * | 2017-02-10 | 2017-06-13 | 安徽博泰电子材料有限公司 | A kind of preparation method of trimethyl aluminium |
Non-Patent Citations (1)
| Title |
|---|
| 贾军纪等: "三甲基铝的合成", 《石油化工》 * |
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