CN103772423A - Synthesis technology for triethyl aluminum - Google Patents
Synthesis technology for triethyl aluminum Download PDFInfo
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- CN103772423A CN103772423A CN201310676078.0A CN201310676078A CN103772423A CN 103772423 A CN103772423 A CN 103772423A CN 201310676078 A CN201310676078 A CN 201310676078A CN 103772423 A CN103772423 A CN 103772423A
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- Prior art keywords
- triethyl aluminum
- reaction
- under
- aluminum
- synthesis technology
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- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 13
- 238000005516 engineering process Methods 0.000 title abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000000047 product Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- 239000005977 Ethylene Substances 0.000 claims abstract description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000746 purification Methods 0.000 claims abstract description 7
- 238000004821 distillation Methods 0.000 claims abstract description 6
- 239000004411 aluminium Substances 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 239000012043 crude product Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000012467 final product Substances 0.000 abstract 1
- 239000011261 inert gas Substances 0.000 abstract 1
- 235000010210 aluminium Nutrition 0.000 description 10
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000007259 addition reaction Methods 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- UOFGSWVZMUXXIY-UHFFFAOYSA-N 1,5-Diphenyl-3-thiocarbazone Chemical compound C=1C=CC=CC=1N=NC(=S)NNC1=CC=CC=C1 UOFGSWVZMUXXIY-UHFFFAOYSA-N 0.000 description 1
- QSJXEFYPDANLFS-UHFFFAOYSA-N Diacetyl Chemical compound CC(=O)C(C)=O QSJXEFYPDANLFS-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 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
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000004845 hydriding Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical compound C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012545 processing Methods 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
- 239000002760 rocket fuel Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N sec-butylidene Natural products CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a synthesis technology for triethyl aluminum. The synthesis technology comprises the following steps of mixing aluminum powder and titanium powder in percentage by mass, under the protection of inert gas, adding the aluminum and titanium powder into a reaction kettle with triethyl aluminum serving as seeds, performing hydrogenation for 6-7 hours under reaction conditions that the temperature is 120-130 DEG C and the pressure is 8-12MPa, continuously feeding ethylene into the reaction kettle under the pressure of 0.2-0.3MPa, terminating the reaction within 5-6 hours to obtain rough triethyl aluminum, performing distillation and ethylene purification on the product to obtain the final product. The synthesis technology for the triethyl aluminum adopts a body catalysis reaction method in which the triethyl aluminum seeds are used as a dispersing medium, so that the reaction temperature and the reaction pressure are low, and the yield of the product is up to over 90 percent.
Description
Technical field
The present invention relates to a kind of synthetic process of organic synthesis technique, particularly a kind of triethyl aluminum.
Background technology
Triethyl aluminum (Aluminumtriethyl, TEA), chemical formula is C
6h
15al, Al(C
2h
5)
3, molecular weight is 114.16.Be mainly used in organic synthesis, the particularly important composition of catalyzer in ethene, propylene polymerization, also as rocket fuel.The problem that the synthesis technique of existing triethyl aluminum exists is that High Temperature High Pressure generated time is long, is unfavorable for production control, and hydrogen feed consumes high simultaneously.
Summary of the invention
The synthesis technique that the object of the present invention is to provide a kind of triethyl aluminum, comprises the steps:
1) titanium valve and aluminium powder are mixed in white oil, under the protection of rare gas element, join and be equipped with in the reactor that triethyl aluminum is seed, at 120-130 ℃, under 8-10MPa, pass into hydrogen, reaction 6-7 hour;
2) at 120-130 ℃, under 0.2-0.3MPa, pass into continuously ethene, react and within 5-6 hour, make triethyl aluminum crude product;
3) by the distillation of triethyl aluminum crude product process, ethylene purification obtains the finished product.
Described rare gas element is nitrogen.
Described titanium valve and the mass ratio of aluminium powder are 0.1%-0.3%:99.9%-99.7%.
Described distillation is to carry out at-0.1MPa, 90～100 ℃.
Described ethylene purification is to carry out under 60～65 ℃, 0.1～0.2MPa.
In above-mentioned processing method, in reactor, can retain the seed of a part of triethyl aluminum crude product as next building-up reactions.
In above-mentioned processing method, waste liquid carries out burning disposal after can adopting white oil dilution to distill residual night.
The invention has the beneficial effects as follows, adopt the body catalysis method that is dispersed in aluminium powder with triethyl aluminum seed, technical process is terse, hydrogenation is close with logical alkene reaction condition, can in same reactor, carry out, reaction time is short, to equipment require little, pollution-free, cost is low, quality product is high, and the temperature and pressure of reaction is lower, and the yield that obtains product can reach more than 90%.
Embodiment
By following embodiment, the present invention is described in further detail, makes those skilled in the art can comprehensively understand the present invention, but do not limit the present invention in any way.
the synthesis technique of 1 one kinds of triethyl aluminums of embodiment
1) preparation of catalyzer
200 kg aluminium powders and 0.5 kg titanium valve join in mixing kettle, add white oil, and the quality of controlling white oil is 2 times of titanium aluminium powder; still temperature control is at 60-65 ℃; after being fully uniformly mixed, under nitrogen protection, join in hydriding reactor, now stir always in opened condition.
2) hydrogenation
Under the pressure of nitrogen protection and 0.15MPa; by the above-mentioned catalyzer preparing; add and be equipped with in the high pressure synthesis reaction vessel that 4.5 tons of triethyl aluminums are seed; temperature rises to 130 ℃; start to pass into hydrogen by Hydrogen distribution pipe and carry out building-up reactions; building-up reactions pressure-controlling under 8-10MP, sustained reaction 6 hours.
3) logical alkene reaction
Temperature of reaction kettle is down to 100 ℃, then passes into continuously ethene and carries out addition reaction, and reaction pressure is controlled at 0.2-0.3MPa, 5 hours reaction times; Ethene injects pipeline and is incorporated into reactor hydrogenation pipeline and is injected ethene by Hydrogen distribution pipe by gas distributor.It is thick triethyl aluminum that reaction finishes reaction product, and by spacing overflow spout, the thick triethyl aluminum that addition reaction is generated is removed solid residue through middle vessel and transferred to retort.In reactor, retain the triethyl aluminum of 4.5 tons, as the seed material of next building-up reactions.
4) distillation is refining
Thick triethyl aluminum in retort, refining and distilling at-0.1MPa, 95 ℃, finished product triethyl aluminum enters into product receiving tank through condenser, then transfers to purifying products still and carries out ethylene purification reaction.
5) purifying products reaction
For improving triethyl aluminum product purity, make the content of three aluminum hydride in product be less than 0.1%, also need to carry out the purification reaction of product, purifying products still temperature of reaction is controlled at 62 ℃, ethylene pressure 0.2MPa, finished product imports canned station by canned-motor pump and carries out product packing.
After the said products pre-treatment, through detecting, the purity of product is more than 95%, and index is as shown in table 1.
Detection method is as follows:
1. total aluminium content
Quantitatively hydrolysis triethyl aluminum sample, with excessive EDTA complexing aluminium, take dithizone as indicator, with the excessive EDA of zinc sulfate back titration, and then calculates the total aluminium content in triethyl aluminum sample.
2. the mensuration of other composition in triethyl aluminum
Triethyl aluminum sample can be hydrolyzed into the gas of definite composition and amount, comprises hydrogen and all kinds of hydro carbons, and qualitative with absolute retention time, external standard method is quantitative, then calculates the content of triethyl aluminum, three n-butylaluminum and three aluminum hydride.Chromatogram testing conditions is as follows:
Gas-chromatography: Shimadzu GC-8A.JS-3070 chromatographic working station
The stainless steel column of chromatographic column: 3mm*2000mm
Stationary phase: apiczon M/ activated alumina
Detected temperatures: 150 ℃
Standard mixture: hydrogen 0.5% ethane 60% normal butane 2%, all the other are nitrogen
6) raffinate processing
Raffinate, with after white oil dilution, is burned.
Claims (5)
1. a synthesis technique for triethyl aluminum, is characterized in that method is as follows:
1) titanium valve and aluminium powder are mixed in white oil, under the protection of rare gas element, join and be equipped with in the reactor that triethyl aluminum is seed, at 120-130 ℃, under 8-10MPa, pass into hydrogen, reaction 6-7 hour;
2) be cooled to 100-120 ℃, under 0.2-0.3MPa, pass into continuously ethene, react and within 5-6 hour, make triethyl aluminum crude product;
3) by the distillation of triethyl aluminum crude product process, ethylene purification obtains the finished product.
2. the synthesis technique of a kind of triethyl aluminum according to claim 1, is characterized in that: described rare gas element is nitrogen.
3. the synthesis technique of a kind of triethyl aluminum according to claim 1, is characterized in that: described titanium valve and the mass ratio of aluminium powder are 0.1%-0.3%:99.9%-99.7%.
4. the synthesis technique of a kind of triethyl aluminum according to claim 1, is characterized in that: described distillation is to carry out at-0.1MPa, 90～100 ℃.
5. the synthesis technique of a kind of triethyl aluminum according to claim 1, is characterized in that: described ethylene purification is to carry out under 60～65 ℃, 0.1～0.2MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310676078.0A CN103772423B (en) | 2013-12-13 | 2013-12-13 | A kind of synthesis technique of triethyl aluminum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310676078.0A CN103772423B (en) | 2013-12-13 | 2013-12-13 | A kind of synthesis technique of triethyl aluminum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103772423A true CN103772423A (en) | 2014-05-07 |
| CN103772423B CN103772423B (en) | 2015-11-11 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310676078.0A Active CN103772423B (en) | 2013-12-13 | 2013-12-13 | A kind of synthesis technique of triethyl aluminum |
Country Status (1)
| Country | Link |
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| CN (1) | CN103772423B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106749374A (en) * | 2017-03-16 | 2017-05-31 | 山东东方宏业化工有限公司 | Slag recovering after triisobutyl aluminium production utilizes system and process |
| 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 |
| RU2773423C1 (en) * | 2021-04-23 | 2022-06-03 | Акционерное общество "Государственный Ордена Трудового Красного Знамени научно-исследовательский институт химии и технологии элементоорганических соединений" (АО "ГНИИХТЭОС") | Method for producing triethylaluminium |
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 |
| CN101805363A (en) * | 2010-04-22 | 2010-08-18 | 浙江福瑞德化工有限公司 | Continuous producing method of triethyl aluminium |
-
2013
- 2013-12-13 CN CN201310676078.0A patent/CN103772423B/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 |
| CN101805363A (en) * | 2010-04-22 | 2010-08-18 | 浙江福瑞德化工有限公司 | Continuous producing method of triethyl aluminium |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106831844B (en) * | 2017-02-10 | 2019-07-02 | 安徽博泰电子材料有限公司 | A kind of preparation method of trimethyl aluminium |
| CN106749374A (en) * | 2017-03-16 | 2017-05-31 | 山东东方宏业化工有限公司 | Slag recovering after triisobutyl aluminium production utilizes system and process |
| RU2773423C1 (en) * | 2021-04-23 | 2022-06-03 | Акционерное общество "Государственный Ордена Трудового Красного Знамени научно-исследовательский институт химии и технологии элементоорганических соединений" (АО "ГНИИХТЭОС") | Method for producing triethylaluminium |
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| Publication number | Publication date |
|---|---|
| CN103772423B (en) | 2015-11-11 |
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Inventor after: Wang Lei Inventor after: Li Huayi Inventor after: Yu Yanmei Inventor after: Wang Zhenguo Inventor after: Chen Xue Inventor after: Zhang Yang Inventor before: Wang Lei Inventor before: Li Huayi Inventor before: Yu Yanmin Inventor before: Wang Zhenguo Inventor before: Chen Xue Inventor before: Zhang Yang |
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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. |
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Inventor after: Wang Lei Inventor after: Yu Yanmei Inventor after: Wang Zhenguo Inventor after: Chen Xue Inventor after: Zhang Yang Inventor before: Wang Lei Inventor before: Li Huayi Inventor before: Yu Yanmei Inventor before: Wang Zhenguo Inventor before: Chen Xue Inventor before: Zhang Yang |
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