CN104710446B - Production method of triethyl aluminum - Google Patents
Production method of triethyl aluminum Download PDFInfo
- Publication number
- CN104710446B CN104710446B CN201310676689.5A CN201310676689A CN104710446B CN 104710446 B CN104710446 B CN 104710446B CN 201310676689 A CN201310676689 A CN 201310676689A CN 104710446 B CN104710446 B CN 104710446B
- Authority
- CN
- China
- Prior art keywords
- kettle
- temperature
- reaction
- triethyl aluminum
- ethene
- 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.)
- Active
Links
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012043 crude product Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 239000005977 Ethylene Substances 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- 150000001336 alkenes Chemical class 0.000 claims description 7
- 239000004411 aluminium Substances 0.000 claims description 7
- 238000006200 ethylation reaction Methods 0.000 claims description 7
- 239000002826 coolant Substances 0.000 claims description 6
- 238000005984 hydrogenation reaction Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 3
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 abstract description 2
- 238000006886 vinylation reaction Methods 0.000 abstract 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- 239000006227 byproduct Substances 0.000 abstract 1
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- SQBBHCOIQXKPHL-UHFFFAOYSA-N tributylalumane Chemical compound CCCC[Al](CCCC)CCCC SQBBHCOIQXKPHL-UHFFFAOYSA-N 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241001122767 Theaceae Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- VPCAAUUIFCAFRZ-UHFFFAOYSA-N butylalumane Chemical compound CCCC[AlH2] VPCAAUUIFCAFRZ-UHFFFAOYSA-N 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical compound C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000002760 rocket fuel 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a production method of triethyl aluminum. The method comprises the following steps: adding titanium-containing aluminum powder into a reaction kettle provided with triethyl aluminum as a seed under the protection of an inert gas, introducing hydrogen at 135-138DEG C under 6.0-8.0MPa, and reacting for 5-6h; carrying out an ethylating reaction to obtain a crude product, guiding the crude product into a rectifying tower, and controlling the tower bottom temperature at 100-135DEG C and the tower top temperature at 65-80DEG C; and adding rectifying tower top distillate into an advanced vinylation kettle, controlling the temperature in the advanced vinylation kettle at 45-55DEG C, and introducing a quantitative amount of ethylene into the advanced vinylation kettle in order to obtain the finished product triethyl aluminum. The method reduces the initial ethylene introduction temperature and the vinylation reaction temperature, greatly reduces the generation of a byproduct tri-n-butylaluminum in the vinylation reaction process, allows remaining aluminum trihydride to be converted into triethyl aluminum in the advanced reaction, improves the indexes of the finished product triethyl aluminum, and allows the product yield to reach above 90%.
Description
Technical field
The present invention relates to organic synthesis technique, particularly a kind of synthetic process of triethyl aluminum.
Background technology
Triethyl aluminum (aluminumtriethyl, tea), chemical formula is c6h15Al, al(c2h5)3, molecular weight is
114.16.Be mainly used in organic synthesis, particularly ethene, in propylene polymerization catalyst important composition, also serve as rocket fuel.
The synthesis technique of existing triethyl aluminum, there is problems that HTHP generated time is long, is unfavorable for producing control, hydrogen simultaneously
Consumption of raw materials is high.
Content of the invention
It is an object of the invention to provide a kind of synthesis technique of triethyl aluminum, comprise the steps:
1) hydrogenation: titaniferous aluminium powder (Ti content is 0.2-1%) is added to equipped with three second under the protection of inert gas
Base aluminium is in the reactor of seed, at 135-138 DEG C, is passed through hydrogen under 6.0-8.0mpa, reacts 5-6 hour；
2) ethylation reaction: after hydrogenation terminates, temperature of reaction kettle is down to 50-60 DEG C, starts to be passed through quantitative ethene,
Control the intake of cooling medium and ethene, in 0.4-1.0mpa, reactor temperature is in one hour to make Stress control in kettle
Rise to 70 DEG C, control 70-80 DEG C of temperature of reaction kettle, when extremely remaining ethene is the 15-20% of added in a single lot total ethylene volume, close
Cooling medium valve, reaction institute liberated heat participated in by remaining ethene makes temperature of reaction kettle rise to 110-120 DEG C, and ethene is passed through
After finishing, now in kettle, pressure can be gradually lowered, and as pressure≤0.3mpa in kettle, ethylation reaction terminates, and obtains crude product.
3) rectification under vacuum: crude product is imported in rectifying column, controls column bottom temperature at 100-135 DEG C, tower top temperature 65-80
℃.
4) depth adds alkene reaction: rectifying column tower top is slipped out thing is then added to depth and add in alkene kettle, control temperature in the kettle 45-
55 DEG C, into kettle, it is passed through quantitative ethene, finally give finished product triethyl aluminum.
The invention has the beneficial effects as follows: reduce and initially lead to alkene temperature and ethylation reaction temperature, substantially reduce ethyl
Change the generation of accessory substance three n-butylaluminum in course of reaction, remaining three aluminum hydride transform into triethyl group in deep reaction
Aluminium, makes the finished product index of triethyl aluminum be improved, the yield of product is up to more than 90%.
Specific embodiment
The production method of embodiment 1 triethyl aluminum
Step is as follows:
1) hydrogenation: by 280kg titaniferous aluminium powder (Ti content be 0.5%) add under inert gas shielding equipped with
5000kg triethyl aluminum is that in the reactor of seed, reaction temperature controls at 135-138 DEG C, and now aluminium powder more activates, pressure
Control in 6.0-8.0mpa, be passed through hydrogen, so that hydrogen, aluminium powder and triethyl aluminum is sufficiently mixed, reaction time 5-6 hour.
2) ethylation reaction: after hydrogenation terminates, temperature of reaction kettle is down to 50-60 DEG C, starts to be passed through ethene, ethene
Consumption be 900kg, control the intake of cooling medium and ethene, make reactor temperature rise to 70 DEG C in one hour, control
Kettle temperature 70-80 DEG C processed, in kettle, Stress control is in 0.4-1.0mpa.When ethene adds to remaining 180kg, close cooling medium valve
Door, making remaining ethene participate in reaction institute liberated heat makes kettle temperature rise to 110-120 DEG C.Ethene is passed through after finishing, now kettle
Interior pressure can be gradually lowered, and as pressure≤0.3mpa in kettle, ethylation reaction terminates, and obtains crude product.
3) rectification under vacuum: crude product is imported in rectifying column, controls column bottom temperature at 100-135 DEG C, tower top temperature 65-80
℃.
4) depth adds alkene reaction: rectifying column tower top is slipped out thing is then added to depth and add in alkene kettle, control temperature in the kettle 45-
55 DEG C, it is passed through 20kg ethene into kettle, finally give finished product triethyl aluminum.Yield is pressed ethylene volume for 91.3%(and is calculated), result is such as
Table 1.
Claims (1)
1. the production method of triethyl aluminum is it is characterised in that method is as follows:
1) hydrogenation: titaniferous aluminium powder is added under inert gas shielding equipped with triethyl aluminum as in the reactor of seed,
At 135-138 DEG C, under 6.0-8.0mpa, it is passed through hydrogen, react 5-6 hour；
2) ethylation reaction: after hydrogenation terminates, temperature of reaction kettle is down to 50-60 DEG C, starts to be passed through quantitative ethene, control
Cooling medium and the intake of ethene, in 0.4-1.0mpa, reactor temperature rose in one hour to make Stress control in kettle
70 DEG C, control 70-80 DEG C of temperature of reaction kettle, when extremely remaining ethene is the 15-20% of added in a single lot total ethylene volume, close cooling
Medium valve, reaction institute liberated heat participated in by remaining ethene makes temperature of reaction kettle rise to 110-120 DEG C, and ethene is passed through and finishes
Afterwards, now in kettle, pressure can be gradually lowered, and as pressure≤0.3mpa in kettle, ethylation reaction terminates, and obtains crude product；
3) rectification under vacuum: crude product is imported in rectifying column, controls column bottom temperature at 100-135 DEG C, tower top temperature 65-80 DEG C；
4) depth adds alkene reaction: rectifying column tower top distillate is then added to depth and adds in alkene kettle, control temperature in the kettle 45-55
DEG C, it is passed through quantitative ethene into kettle, finally give finished product triethyl aluminum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310676689.5A CN104710446B (en) | 2013-12-13 | 2013-12-13 | Production method of triethyl aluminum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310676689.5A CN104710446B (en) | 2013-12-13 | 2013-12-13 | Production method of triethyl aluminum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104710446A CN104710446A (en) | 2015-06-17 |
| CN104710446B true CN104710446B (en) | 2017-01-18 |
Family
ID=53410225
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310676689.5A Active CN104710446B (en) | 2013-12-13 | 2013-12-13 | Production method of triethyl aluminum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104710446B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111534033A (en) * | 2020-06-15 | 2020-08-14 | 扬州爱非科鞋业有限公司 | Preparation method of anti-slip sole |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3038922A (en) * | 1960-02-15 | 1962-06-12 | Hercules Powder Co Ltd | Process for preparation of triethylaluminum |
| CN101220049A (en) * | 2007-12-24 | 2008-07-16 | 王学力 | Technique for synthesizing triethylaluminum |
| CN102584879A (en) * | 2012-01-19 | 2012-07-18 | 营口市向阳催化剂有限责任公司 | Preparation method of aluminium triethyl |
-
2013
- 2013-12-13 CN CN201310676689.5A patent/CN104710446B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3038922A (en) * | 1960-02-15 | 1962-06-12 | Hercules Powder Co Ltd | Process for preparation of triethylaluminum |
| CN101220049A (en) * | 2007-12-24 | 2008-07-16 | 王学力 | Technique for synthesizing triethylaluminum |
| CN102584879A (en) * | 2012-01-19 | 2012-07-18 | 营口市向阳催化剂有限责任公司 | Preparation method of aluminium triethyl |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104710446A (en) | 2015-06-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108250041B (en) | Preparation method of fully deuterated methanol | |
| CN105481726A (en) | Preparation method of metformin hydrochloride | |
| WO2014175495A1 (en) | Method for producing catalyst for polyolefin polymerization and method for preparing polyolefin | |
| CN104710446B (en) | Production method of triethyl aluminum | |
| CN106188116A (en) | A kind of method of synthesizing pyrazole 4 boric acid pinacol ester | |
| CN101391979B (en) | Unsymmetrical bis(imino)pyridines iron and cobalt complexes containing halogen, preparation method and use | |
| Sun et al. | Cp 2 TiCl 2-catalyzed cis-hydroalumination of propargylic amines with Red-Al: stereoselective synthesis of Z-configured allylic amines | |
| CN101220049A (en) | Technique for synthesizing triethylaluminum | |
| CN107011151B (en) | Method for improving benzaldehyde selectivity in toluene liquid-phase catalytic oxidation process | |
| CN109096127A (en) | Using silane coupling agent production by-product as the hydramine of raw material and preparation method and application | |
| CN103254101B (en) | Prepare the method and apparatus of Urethylane | |
| CN109232478B (en) | Preparation method of epoxy resin key intermediate | |
| CN103449954B (en) | Preparation method of high-purity longifolene | |
| CN110183481A (en) | The technique of catalytic pyrolysis organosilicon high-boiling product | |
| CN106986890B (en) | A kind of environment-friendly preparation method of 2- vinyl -2,4,4,6,6- pentamethyl cyclotrisiloxane | |
| CN113402554B (en) | PNSiNP ligand and preparation method thereof, ethylene oligomerization catalyst and application thereof | |
| CN103772423B (en) | A kind of synthesis technique of triethyl aluminum | |
| CN103193828B (en) | Double-imidazole imide nickel hydroxide coordination complex as well as preparation method and application thereof | |
| CN108117536A (en) | A kind of method of 1,2-PD and carbon dioxide synthesizing acrylic ester | |
| CN107162920A (en) | A kind of preparation method of R-1- amino -2- propyl alcohol | |
| CN101775029A (en) | Convenient synthesis method for alkyl substitution phenyloboricacid | |
| CN109796317A (en) | A kind of preparation method of 1- Phenyl 2 butanone | |
| CN110498818A (en) | A kind of preparation method of ethylene oligomerisation catalyst | |
| CN104447168B (en) | A kind of method for producing 1 hexene coproduction heptene and octene | |
| CN1331602C (en) | Oxygen-containing metallocene catalyst, preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 115005, Yingkou, Liaoning Province, the old border road south Zhenjiang home Patentee after: YINGKOU FENGGUANG ADVANCED MATERIAL CO.,LTD. Address before: 115005, 519, Jiang Jia village, old border area, Liaoning, Yingkou Patentee before: YINGKOU FENGGUANG CHEMICAL CO.,LTD. |
|
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wang Lei Inventor after: Wang Zhenguo Inventor after: Yu Yanmin Inventor after: Chen Xue Inventor after: Zhang Yang Inventor after: Yang Sen Inventor before: Wang Lei Inventor before: Li Huayi Inventor before: Wang Zhenguo Inventor before: Yu Yanmin Inventor before: Chen Xue Inventor before: Zhang Yang Inventor before: Yang Sen |