CN102443019A - Process for producing diisobutyl aluminium hydride - Google Patents
Process for producing diisobutyl aluminium hydride Download PDFInfo
- Publication number
- CN102443019A CN102443019A CN201110423993XA CN201110423993A CN102443019A CN 102443019 A CN102443019 A CN 102443019A CN 201110423993X A CN201110423993X A CN 201110423993XA CN 201110423993 A CN201110423993 A CN 201110423993A CN 102443019 A CN102443019 A CN 102443019A
- Authority
- CN
- China
- Prior art keywords
- aluminium
- diisobutyl
- raw material
- content
- hydride
- 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.)
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- SIPUZPBQZHNSDW-UHFFFAOYSA-N diisobutylaluminium hydride Substances CC(C)C[Al]CC(C)C SIPUZPBQZHNSDW-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 51
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 47
- 239000002994 raw material Substances 0.000 claims abstract description 21
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 11
- 239000001257 hydrogen Substances 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 239000003999 initiator Substances 0.000 claims abstract description 3
- 239000004411 aluminium Substances 0.000 claims description 41
- 239000000843 powder Substances 0.000 claims description 16
- MCULRUJILOGHCJ-UHFFFAOYSA-N triisobutylaluminium Chemical compound CC(C)C[Al](CC(C)C)CC(C)C MCULRUJILOGHCJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 4
- 239000003973 paint Substances 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000001311 chemical methods and process Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a new process for producing diisobutyl aluminum hydride, which belongs to the field of chemical processes and is characterized in that: the raw materials of the active aluminum paste, isobutene and hydrogen are subjected to a synthesis reaction in a reaction kettle at a temperature of 110-140 ℃ under a pressure of 5.5-6.0 MPa by taking an aluminum agent as an initiator to generate the aluminum agent with the required diisobutylaluminum hydride content. Under the condition that the adding amount of the raw material aluminum paste is not changed, the content of diisobutyl aluminum hydride in the product is changed by properly increasing and decreasing the adding amount of the raw material isobutene and changing the constant temperature time after the reaction; the invention realizes the content of diisobutyl aluminum hydride by changing the adding amount of the raw material isobutene and the constant temperature time after the reaction, has strong operability, stabilizes the product quality and the product content, reduces the material consumption and the energy consumption in the production process, and has low risk, less investment and obvious effect.
Description
Technical field
The present invention relates to a kind of novel process of producing diisobutyl aluminium hydride, belong to the chemical technique field.
Background technology
It is the old technology of continuing to use the seventies that at present domestic aluminium agent is produced always.Content to quality product and key ingredient never has the rational and effective control device in process of production; Cause the unstable product quality of producing; Content is inhomogeneous, and just product performance are unstable, will cause product percent of pass lower like this; Cause the product power consumption bigger like this, spent material is bigger.This technology is based on the former technology of aluminium agent and novel process newly developed.
Summary of the invention
Deficiency according to prior art; The technical problem that the present invention will solve is: a kind of novel process of producing diisobutyl aluminium hydride is provided; Rationally effectively control the content of diisobutyl aluminium hydride in the total aluminium of aluminium agent; Stabilized product quality and product content reduce in process of production supplies consumption and energy consumption.
The technical solution adopted for the present invention to solve the technical problems is: a kind of novel process of producing diisobutyl aluminium hydride is provided; It is characterized in that: the active aluminium paste of raw material, iso-butylene and hydrogen are made initiator with the aluminium agent in reaction kettle; Under 5.5～6.0Mpa pressure, carry out building-up reactions under 110～140 ℃ the temperature, generate the aluminium agent of required diisobutyl aluminium hydride content.
Described aluminium agent staple comprises: solvent oil, triisobutyl aluminium, diisobutyl aluminum and pure aluminum.
The active aluminium paste of described raw material is prepared by following steps:
(1), will paint with aluminium powder brokenly through sand barreling abrasive dust under the protection of solvent oil, remove the sull on aluminium powder surface, the macrobead aluminium powder is pulverized, to increase the specific surface area of aluminium powder, obtain the activated aluminum powder of enough unsalted surfaces;
(2), iso-butylene is got into drying tower, remove minor amount of water, as raw material;
(3), raw hydrogen is boosted to 6.5-9.0Mpa supply autoclave with the hydrogen pressure machine, as the raw material of synthetic triisobutyl aluminium.
In the described diisobutyl aluminium hydride mixture, can control: total aluminium content >=65g/l; The total mole number of triisobutyl aluminium accounts for 40～80% of total aluminium mole number; The total mole number of diisobutyl aluminium hydride accounts for 10～60% of triisobutyl aluminium mole number.
The invention has the beneficial effects as follows: under the constant situation of raw material aluminium paste add-on, through suitable increase with reduce the add-on of raw material iso-butylene and through changing the content that reacted constant temperature time changes diisobutyl aluminium hydride in the product; The content that the present invention realizes diisobutyl aluminium hydride through the add-on and the reacted constant temperature time of change raw material iso-butylene, workable, stabilized product quality and product content; Reduce in process of production supplies consumption and energy consumption; Risk is low, less investment, and effect is obvious.
Embodiment
Below in conjunction with embodiment the present invention is done and to further describe.
Instance 1
Aluminium paste preparation: (1), will paint with aluminium powder brokenly through sand barreling abrasive dust under the protection of solvent oil, remove the sull on aluminium powder surface, make the pulverizing of macrobead aluminium powder, with the specific surface area of increase aluminium powder, obtain the activated aluminum powder of enough unsalted surfaces;
(2), iso-butylene is got into drying tower, remove minor amount of water, as raw material;
(3), raw hydrogen is boosted to 6.5-7.0Mpa supply autoclave with the hydrogen pressure machine, as the raw material of synthetic triisobutyl aluminium.
The raw material add-on is respectively: aluminium paste 250Kg, and iso-butylene 420Kg, reaction pressure 6.0MPa, 120～135 ℃ of temperature of reaction, constant temperature time is 7h, obtaining the content in total aluminium of diisobutyl aluminium hydride in the product is 12～25%.
Instance 2
Aluminium paste preparation: (1), will paint with aluminium powder brokenly through sand barreling abrasive dust under the protection of solvent oil, remove the sull on aluminium powder surface, make the pulverizing of macrobead aluminium powder, with the specific surface area of increase aluminium powder, obtain the activated aluminum powder of enough unsalted surfaces;
(2), iso-butylene is got into drying tower, remove minor amount of water, as raw material;
(3), raw hydrogen is boosted to 8.5-9.0Mpa supply autoclave with the hydrogen pressure machine, as the raw material of synthetic triisobutyl aluminium.
The raw material add-on is respectively: aluminium paste 250Kg, and iso-butylene 300Kg, permanent reaction pressure 6.0MPa, 120～135 ℃ of temperature of reaction, temperature is 3h the time, obtains that the content of diisobutyl aluminium hydride in total aluminium is 40～60% in the product.
Claims (4)
1. novel process of producing diisobutyl aluminium hydride; It is characterized in that: the active aluminium paste of raw material, iso-butylene and hydrogen are made initiator with the aluminium agent in reaction kettle; Under 5.5～6.0Mpa pressure, carry out building-up reactions under 110～140 ℃ the temperature, generate the aluminium agent of required diisobutyl aluminium hydride content.
2. the novel process of production diisobutyl aluminium hydride according to claim 1 is characterized in that described aluminium agent staple comprises: solvent oil, triisobutyl aluminium, diisobutyl aluminum and pure aluminum.
3. the novel process of production diisobutyl aluminium hydride according to claim 1 is characterized in that the active aluminium paste of described raw material is prepared by following steps:
(1), will paint with aluminium powder brokenly through sand barreling abrasive dust under the protection of solvent oil, remove the sull on aluminium powder surface, the macrobead aluminium powder is pulverized, to increase the specific surface area of aluminium powder, obtain the activated aluminum powder of enough unsalted surfaces;
(2), iso-butylene is got into drying tower, remove minor amount of water, as raw material;
(3), raw hydrogen is boosted to 6.5-9.0Mpa supply autoclave with the hydrogen pressure machine, as the raw material of synthetic triisobutyl aluminium.
4. the novel process of production diisobutyl aluminium hydride according to claim 1 is characterized in that can controlling in the described diisobutyl aluminium hydride mixture: total aluminium content >=65g/l; The total mole number of triisobutyl aluminium accounts for 40～80% of total aluminium mole number; The total mole number of diisobutyl aluminium hydride accounts for 10～60% of triisobutyl aluminium mole number.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110423993XA CN102443019A (en) | 2011-12-16 | 2011-12-16 | Process for producing diisobutyl aluminium hydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110423993XA CN102443019A (en) | 2011-12-16 | 2011-12-16 | Process for producing diisobutyl aluminium hydride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102443019A true CN102443019A (en) | 2012-05-09 |
Family
ID=46005995
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110423993XA Pending CN102443019A (en) | 2011-12-16 | 2011-12-16 | Process for producing diisobutyl aluminium hydride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102443019A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113264955A (en) * | 2021-06-17 | 2021-08-17 | 山东东方宏业化工有限公司 | Preparation method of triisobutyl aluminum |
-
2011
- 2011-12-16 CN CN201110423993XA patent/CN102443019A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113264955A (en) * | 2021-06-17 | 2021-08-17 | 山东东方宏业化工有限公司 | Preparation method of triisobutyl aluminum |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C05 | Deemed withdrawal (patent law before 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120509 |