CN113264955A - Preparation method of triisobutyl aluminum - Google Patents
Preparation method of triisobutyl aluminum Download PDFInfo
- Publication number
- CN113264955A CN113264955A CN202110669798.9A CN202110669798A CN113264955A CN 113264955 A CN113264955 A CN 113264955A CN 202110669798 A CN202110669798 A CN 202110669798A CN 113264955 A CN113264955 A CN 113264955A
- Authority
- CN
- China
- Prior art keywords
- aluminum
- reaction
- isobutene
- triisobutyl aluminum
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- MCULRUJILOGHCJ-UHFFFAOYSA-N triisobutylaluminium Chemical compound CC(C)C[Al](CC(C)C)CC(C)C MCULRUJILOGHCJ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 230000035484 reaction time Effects 0.000 claims abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 7
- 239000003999 initiator Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims 6
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000004904 shortening Methods 0.000 abstract 1
- SPRIOUNJHPCKPV-UHFFFAOYSA-N hydridoaluminium Chemical compound [AlH] SPRIOUNJHPCKPV-UHFFFAOYSA-N 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- SIPUZPBQZHNSDW-UHFFFAOYSA-N bis(2-methylpropyl)aluminum Chemical compound CC(C)C[Al]CC(C)C SIPUZPBQZHNSDW-UHFFFAOYSA-N 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000005062 Polybutadiene Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/06—Aluminium compounds
- C07F5/061—Aluminium compounds with C-aluminium linkage
- C07F5/062—Al linked exclusively to C
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses a preparation method of triisobutyl aluminum, belonging to the technical field of triisobutyl aluminum production; the preparation method of triisobutyl aluminum comprises the following steps: (1) adding an initiator, active aluminum paste and isobutene into a reaction kettle, hydrogenating, pressurizing and heating to prepare aluminum hydride; (2) cooling and depressurizing the reaction kettle, adding isobutene, pressurizing and heating for reaction to generate triisobutyl aluminum. The invention has the advantages of stable product amount after reaction, raw material saving of isobutene, reduction of reaction time and shortening of settlement time after reaction.
Description
Technical Field
The invention relates to the technical field of triisobutyl aluminum production, in particular to a preparation method of triisobutyl aluminum.
Background
Triisobutylaluminum is an important chemical used as a polymerization catalyst for butadiene rubber, synthetic resin, synthetic fiber and olefin polymer, and also as an intermediate of organometallic compounds and a high-energy raw material and a reducing agent for a jet engine ignition system, etc.
The existing preparation method of triisobutyl aluminum comprises the steps of adding an initiator, active aluminum paste and isobutene into a reaction kettle at one time, introducing hydrogen into heat-conducting oil, and heating for reaction, and has the following defects:
1. the quality of the product after reaction is unstable, and the fluctuation of the content of the aluminum hydride is large (different from 15 to 70 percent);
2. the consumption of isobutene is higher, and the average consumption per ton is about 1200L;
3. the reaction time is too long, and the average reaction time per kettle is more than or equal to 20 hours;
4. the settling time after the reaction is too long, and the flash evaporation condition can be met in 30-40 days.
Disclosure of Invention
The invention aims to provide a preparation method of triisobutyl aluminum, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of triisobutyl aluminum comprises the following steps:
(1) adding an initiator, active aluminum paste and isobutene into a reaction kettle, hydrogenating, pressurizing and heating to prepare aluminum hydride;
(2) cooling and depressurizing the reaction kettle, adding isobutene, pressurizing and heating for reaction to generate triisobutyl aluminum.
As a further scheme of the invention: the activated aluminum paste in the step (1) comprises aluminum powder and n-hexane, wherein the weight of the n-hexane is 2-4 times that of the aluminum powder.
As a further scheme of the invention: the weight of the n-hexane is 3 times of that of the aluminum powder.
As a further scheme of the invention: the pressure in the step (1) is increased to 5.0-6.0MPa, the reaction is heated to 110 ℃ and 140 ℃, and the reaction time is 3 h.
As a further scheme of the invention: and (2) reducing the temperature to 70 ℃ and reducing the pressure to 0.1 MPa.
As a further scheme of the invention: the adding amount of the isobutene in the step (2) is two thirds of the adding amount of the isobutene in the step (1).
As a further scheme of the invention: pressurizing to 0.3-0.8MPa in the step (2), heating to 80-85 ℃, and reacting for 2-4 h.
Compared with the prior art, the invention has the beneficial effects that:
1. the product amount is stable after reaction, and the content of aluminum hydride is less than or equal to 10 percent;
2. the consumption of isobutene is reduced to 840L/t, and 30 percent of isobutene is saved per ton;
3. the reaction time is reduced, the average single kettle reaction operation time is reduced to 16h and reduced by 25 percent;
4. the settling time after the reaction is shortened to about 15 to 20 days, which is reduced by 30 to 50 percent.
Detailed Description
The technical solution of the present patent will be described in further detail with reference to the following embodiments.
Example 1
The preparation method of triisobutyl aluminum is characterized by comprising the following steps of:
at 2.5m3Taking a reaction kettle as an example, the first step is as follows: adding 300 kg of triisobutyl aluminum initiator, 320 kg of active aluminum paste (wherein 80 kg of aluminum powder and 240 kg of normal hexane) and 400L of isobutene into a reaction kettle, introducing hydrogen, controlling the pressure at 5.0MPa and the temperature at 110 ℃ to react, and generating diisobutyl aluminum hydride for 5 hours, wherein the reaction equation is as follows:
Al+H2+C4H8→AlH（C4H9）2
the second step is that: cooling to 70 ℃, reducing the pressure to 0.1MPa, adding 300L of isobutene, controlling the temperature at 80 ℃ and the pressure at 0.3MPa, reacting for 2h to generate triisobutyl aluminum, wherein the reaction equation is as follows:
AlH（C4H9）2+C4H8→AlH（C4H9）3
example 2
The preparation method of triisobutyl aluminum is characterized by comprising the following steps of:
at 2.5m3Taking a reaction kettle as an example, the first step is as follows: adding 300 kg of triisobutylaluminum initiator, 320 kg of active aluminum paste (80 kg of aluminum powder and 240 kg of normal hexane) and 425L of isobutene into a reaction kettle, introducing hydrogen, controlling the pressure at 5.5MPa and the temperature at 125 ℃ for reaction, and generating diisobutylaluminum hydride in 4 hours, wherein the reaction equation is as follows:
Al+H2+C4H8→AlH（C4H9）2
the second step is that: cooling to 70 ℃, reducing the pressure to 0.1MPa, adding 300L of isobutene, controlling the temperature at 83 ℃ and the pressure at 0.5MPa, reacting for 2h to generate triisobutyl aluminum, wherein the reaction equation is as follows:
AlH（C4H9）2+C4H8→AlH（C4H9）3
example 3
The preparation method of triisobutyl aluminum is characterized by comprising the following steps of:
at 2.5m3Taking a reaction kettle as an example, the first step is as follows: adding 300 kg of triisobutyl aluminum initiator, 320 kg of active aluminum paste (wherein 80 kg of aluminum powder and 240 kg of normal hexane) and 450L of isobutene into a reaction kettle, introducing hydrogen, controlling the pressure at 6.0MPa and the temperature at 110 ℃ to react, and generating diisobutyl aluminum hydride for 3 hours, wherein the reaction equation is as follows:
Al+H2+C4H8→AlH（C4H9）2
the second step is that: cooling to 70 ℃, reducing the pressure to 0.1MPa, adding 300L of isobutene, controlling the temperature at 85 ℃ and the pressure at 0.8MPa, reacting for 2h to generate triisobutyl aluminum, wherein the reaction equation is as follows:
AlH（C4H9）2+C4H8→AlH（C4H9）3
the raw materials and products involved in the above examples were tested and developed in this way, and the following data were collected:
as can be seen from the above table, the weight of the product aluminum hydride does not exceed 10% of the total product weight; and the single-pot reaction time is about 16 h.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. The preparation method of triisobutyl aluminum is characterized by comprising the following steps of:
adding an initiator, active aluminum paste and isobutene into a reaction kettle, hydrogenating, pressurizing and heating to prepare aluminum hydride;
cooling and depressurizing the reaction kettle, adding isobutene, pressurizing and heating for reaction to generate triisobutyl aluminum.
2. The method for preparing triisobutyl aluminum as claimed in claim 1, wherein the activated aluminum paste in (1) comprises aluminum powder and n-hexane, and the weight of the n-hexane is 2-4 times that of the aluminum powder.
3. The method of claim 2, wherein the weight of the n-hexane is 3 times the weight of the aluminum powder.
4. The method as claimed in claim 1, wherein the pressure in (1) is 5.0-6.0MPa, the temperature is 110-140 ℃, and the reaction time is 3-5 h.
5. The method of claim 1, wherein the temperature in (2) is reduced to 70 ℃ and the pressure in (2) is reduced to 0.1 MPa.
6. The method of claim 1, wherein the amount of isobutylene added in (2) is two-thirds of the amount of isobutylene added in (1).
7. The method for preparing triisobutyl aluminum according to claim 1, wherein the pressure in the step (2) is increased to 0.3-0.8MPa, the temperature is increased to 80-85 ℃, and the reaction time is 2-4 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110669798.9A CN113264955A (en) | 2021-06-17 | 2021-06-17 | Preparation method of triisobutyl aluminum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110669798.9A CN113264955A (en) | 2021-06-17 | 2021-06-17 | Preparation method of triisobutyl aluminum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113264955A true CN113264955A (en) | 2021-08-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110669798.9A Pending CN113264955A (en) | 2021-06-17 | 2021-06-17 | Preparation method of triisobutyl aluminum |
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Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1000818B (en) * | 1954-02-01 | 1957-01-17 | Dr Dr E H Karl Ziegler | Process for the preparation of aluminum triisobutyl |
| US2900402A (en) * | 1955-03-17 | 1959-08-18 | Monsanto Chemicals | Preparation of aluminum alkyls |
| GB848103A (en) * | 1956-09-26 | 1960-09-14 | Goodrich Gulf Chem Inc | Preparation of aluminium hydrocarbyls |
| GB894089A (en) * | 1959-02-24 | 1962-04-18 | Ethyl Corp | Process for the manufacture of alkyl aluminum compounds and dialkyl aluminum hydrides |
| JPH06128270A (en) * | 1992-10-15 | 1994-05-10 | Mitsui Toatsu Chem Inc | Production of triisobutyl aluminum |
| JPH06247982A (en) * | 1993-02-25 | 1994-09-06 | Mitsui Toatsu Chem Inc | Production of triisobutylaluminum |
| CN1374251A (en) * | 2002-04-08 | 2002-10-16 | 常耀辉 | Prepn of superpurity nano level alumina powder |
| RU2295532C1 (en) * | 2005-08-12 | 2007-03-20 | Открытое акционерное общество "Нижнекамскнефтехим" | Method for preparing aluminum alkyls |
| CN102443019A (en) * | 2011-12-16 | 2012-05-09 | 淄博齐翔腾达化工股份有限公司 | Novel process for producing diisobutylaluminium hydride |
| CN105148796A (en) * | 2015-09-07 | 2015-12-16 | 中国兵器科学研究院宁波分院 | Spray granulation method of active nano aluminum powder |
| CN111454287A (en) * | 2020-05-12 | 2020-07-28 | 南通艾德旺化工有限公司 | One-step production process of tri-n-butyl aluminum for preparing tetrabutyltin by alkyl aluminum method |
| CN111574314A (en) * | 2020-05-21 | 2020-08-25 | 中国科学院兰州化学物理研究所 | Method for improving stability and combustion performance by modifying aluminum powder with fluoroalkyl compound |
| CN211799163U (en) * | 2020-03-12 | 2020-10-30 | 山东东方宏业化工有限公司 | Tri-isobutyl aluminum filtration system |
-
2021
- 2021-06-17 CN CN202110669798.9A patent/CN113264955A/en active Pending
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1000818B (en) * | 1954-02-01 | 1957-01-17 | Dr Dr E H Karl Ziegler | Process for the preparation of aluminum triisobutyl |
| US2900402A (en) * | 1955-03-17 | 1959-08-18 | Monsanto Chemicals | Preparation of aluminum alkyls |
| GB848103A (en) * | 1956-09-26 | 1960-09-14 | Goodrich Gulf Chem Inc | Preparation of aluminium hydrocarbyls |
| GB894089A (en) * | 1959-02-24 | 1962-04-18 | Ethyl Corp | Process for the manufacture of alkyl aluminum compounds and dialkyl aluminum hydrides |
| JPH06128270A (en) * | 1992-10-15 | 1994-05-10 | Mitsui Toatsu Chem Inc | Production of triisobutyl aluminum |
| JPH06247982A (en) * | 1993-02-25 | 1994-09-06 | Mitsui Toatsu Chem Inc | Production of triisobutylaluminum |
| CN1374251A (en) * | 2002-04-08 | 2002-10-16 | 常耀辉 | Prepn of superpurity nano level alumina powder |
| RU2295532C1 (en) * | 2005-08-12 | 2007-03-20 | Открытое акционерное общество "Нижнекамскнефтехим" | Method for preparing aluminum alkyls |
| CN102443019A (en) * | 2011-12-16 | 2012-05-09 | 淄博齐翔腾达化工股份有限公司 | Novel process for producing diisobutylaluminium hydride |
| CN105148796A (en) * | 2015-09-07 | 2015-12-16 | 中国兵器科学研究院宁波分院 | Spray granulation method of active nano aluminum powder |
| CN211799163U (en) * | 2020-03-12 | 2020-10-30 | 山东东方宏业化工有限公司 | Tri-isobutyl aluminum filtration system |
| CN111454287A (en) * | 2020-05-12 | 2020-07-28 | 南通艾德旺化工有限公司 | One-step production process of tri-n-butyl aluminum for preparing tetrabutyltin by alkyl aluminum method |
| CN111574314A (en) * | 2020-05-21 | 2020-08-25 | 中国科学院兰州化学物理研究所 | Method for improving stability and combustion performance by modifying aluminum powder with fluoroalkyl compound |
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| M. ROHA等: "Low Pressure Polyethylene Catalysts", 《JOURNAL OF POLYMER SCIENCE》, 31 December 1959 (1959-12-31), pages 51 - 61 * |
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Application publication date: 20210817 |
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