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Preparation method and application of complex

A complex and compound technology, applied in 1 field, can solve the problems of poor solubility, affecting the conversion rate of raw materials, catalyst utilization, etc., and achieve the effects of increased solubility, broad industrialization prospects, and stable ethylene oligomerization reaction

Active Publication Date: 2015-03-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the solubility of the catalyst in the solvent is very poor, causing the catalyst to settle in the pipeline before reaching the reactor in the continuous reaction of ethylene oligomerization, which affects the conversion rate of raw materials and the utilization rate of the catalyst

Method used

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  • Preparation method and application of complex
  • Preparation method and application of complex
  • Preparation method and application of complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] This example is the synthesis of catalyst 2-acetyl-1,10-phenanthroline 2,6-diethylaniline ferrocene(II) complex and its catalytic ethylene oligomerization reaction. The specific steps are as follows:

[0030] a) Synthesis of 2-acetyl-1,10-phenanthroline

[0031]

[0032]Put 5.1 g (28.3 mmol) of 1,10-phenanthroline into a 250 ml three-necked flask, and dissolve it with 100 ml of toluene under nitrogen protection and magnetic stirring. Slowly add 10ml of triethylaluminum (70.8mmol) dropwise to the three-necked flask under stirring at -60°C, the dropwise addition is completed in about 15 minutes, continue stirring at this temperature for 18h, then raise the temperature to about 30°C, and continue stirring 10h. Then the reaction mixture was cooled to about -30°C, 50ml of distilled water was slowly added thereto, and then heated to 30°C and stirred for 10h. Then separate the liquids, take out the organic phase, and extract the inorganic phase three times with dichlorome...

Embodiment 2

[0048] This embodiment is a solubility contrast experiment. Taking 2-acetyl-1,10-phenanthroline chloride as a comparative example, it is slightly soluble or insoluble in ethylene oligomerization catalyst solvents, such as toluene , after the action of ultrasound is still granular. However, the 2-acetyl-1,10-phenanthroline 2,6-diethylaniline ferrocene(II) in the present invention is soluble in toluene.

Embodiment 3

[0050] Repeat step 1 of Example 1, except that the 2,6-diethylaniline in step b of Example 1 is replaced by the following substituted anilines in turn: 2-methylaniline, 3-methylaniline, 4- Methylaniline, 2,3-dimethylaniline, 2,4-dimethylaniline, 2,5-dimethylaniline, 2,6-dimethylaniline, 3,4-dimethylaniline, 3 ,5-Dimethylaniline, 2,4,6-trimethylaniline, 4-bromo-2,6-dimethylaniline, 2-ethylaniline, 2-ethyl-6-methylaniline, 2 -isopropylaniline, 2,6-diisopropylaniline, 2-fluoroaniline, 2-fluoro-4-methylaniline, 2-fluoro-5-methylaniline, 2,4-difluoroaniline, 2 ,5-difluoroaniline, 2,6-difluoroaniline, 3,4-difluoroaniline, 2,3,4-trifluoroaniline, 2,4,5-trifluoroaniline, 2,4,6-trifluoroaniline Fluoroaniline, 2,3,4,5,6-pentafluoroaniline, 3-chloroaniline, 2,6-dichloroaniline, 2,3,4-trichloroaniline, 2,4,5-trichloroaniline, 2,4,6-Trichloroaniline, 2-bromoaniline, 2-bromo-4-methylaniline, 2-bromo-4-fluoroaniline, 4-bromo-2-fluoroaniline, 2,6-dibromoaniline , 2,6-dibromo-4-methylanilin...

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Abstract

The invention provides a 2-acetyl-1,10-phenanthroline amine ferrocene (II) complex represented by general formula I. The invention also provides a preparation method of the complex, and an application of the complex in ethylene oligomerization. The complex provided by the invention has a larger solubility in an organic solvent than present phenanthroline amine iron (II) complexes. The synthesis method provided by the invention has the advantages of simple technology and reduction of the catalyst preparation cost; and the generated complex has an increased conversion rate in the catalysis of an ethylene oligomerization reaction, has accepted reactive activity, and has wide industrial prospect.

Description

technical field [0001] The invention relates to a complex, its preparation method and the application of the complex, more specifically the complex relates to an acetyl-substituted 1,10-phenanthroline amide iron (II) complex. Background technique [0002] Ethylene oligomerization is one of the most important reactions in the olefin polymerization industry. Through oligomerization, cheap small molecule olefins can be transformed into products with high added value. Ethylene oligomerization product linear α-olefin (LAO) is an important organic chemical raw material. For example LAOC 4 -C 30 It can be used to prepare daily cleaning agents, flotation agents, emulsifiers, lubricating components of refrigerators and drilling fluids, plasticizers, various additives, low-viscosity synthetic oils, polymers and copolymers, petroleum And petroleum product additives, higher alkylamines, higher organoaluminum compounds, higher alkaryl hydrocarbons, higher fatty alcohols and fatty aci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/02B01J31/22C07C2/32
CPCB01J31/2295B01J2231/20B01J2531/842C07C2/32C07F17/02C07C11/02
Inventor 张海英王怀杰刘珺郑明芳栗同林李维真
Owner CHINA PETROLEUM & CHEM CORP
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