Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of unsymmetrical benzhydryl α-diimine nickel complex and its preparation and application

A technology of diphenylmethyl and diimide nickel, which is applied in the direction of nickel organic compounds, can solve problems such as few reports, and achieve the effects of wide molecular weight distribution, high degree of branching, and good catalytic activity

Active Publication Date: 2017-02-15
PETROCHINA CO LTD
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, most of the above-mentioned studies are based on the identical structure of α-diimine and the nitrogen-linked benzene ring (Ar=Ar'), and reports on asymmetric α-diimine (Ar, Ar' are different) rarely reported

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of unsymmetrical benzhydryl α-diimine nickel complex and its preparation and application
  • A kind of unsymmetrical benzhydryl α-diimine nickel complex and its preparation and application
  • A kind of unsymmetrical benzhydryl α-diimine nickel complex and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Embodiment 1, the synthetic method of preparing 2-(2,6-benzhydryl-4-methylaniline) butanone.

[0064] Add catalyst amount (0.88g) to 2,6-dibenzhydryl-4-methylaniline (8.80g, 20mmol) and 2,3-butanedione (2.06g, 24mmol) in toluene (200mL) solution The p-toluenesulfonic acid, reflux reaction 8h. The solvent was removed, and the residue was subjected to silica gel column chromatography with a mixed solvent of petroleum ether and ethyl acetate at a volume ratio of 50:1, and the eluted fraction was detected through a thin-layer silica gel plate, and the developing solvent was the volume of petroleum ether and ethyl acetate. Mixed solvents at a ratio of 8:1, the second fraction was collected, and a yellow solid was obtained after removal of the solvent. Yield 29.5%. Melting point: 158°C. The structure confirmation data are as follows: FT-IR(KBr,cm -1 ):3026(m), 2168(w), 1703(s), 1653(m), 1600(m), 1495(s), 1448(s), 1419(m), 1353(s), 1251(m ),1118(s),1078(m),1031(m),922(m),...

Embodiment 2

[0065] Example 2, preparation of 2-(2,6-dibenzhydryl-4-methylaniline)-3-(2,6-dimethylaniline) butane [L1]

[0066] 2-(2,6-Dibenzhydryl-4-methylaniline) butanone (1.00g, 1.97mmol) and 2,6-dimethylaniline (0.24g, 2.00mmol) in toluene (50mL) Add a catalytic amount of p-toluenesulfonic acid, and heat to reflux for 8h. The solvent toluene was removed, and the residue was subjected to silica gel column chromatography with a mixed solvent of petroleum ether and ethyl acetate at a volume ratio of 50:1. The eluted fractions were examined through a thin-layer silica gel plate, the first fraction was collected, and the solvent was removed to give a yellow solid. Yield: 30.3%. Melting point: 141°C. The structure confirmation data are as follows: FT-IR(KBr,cm -1 ):3025(m), 2918(w), 1977(w), 1648(s), 1599(m), 1494(s), 1448(s), 1420(m), 1354(s), 1253(m ),1199(w),1118(s),1078(m),1030(m),857(m),802(w),767(m),746(w),697(s). 1 H NMR (400MHz, CDCl 3 ,TMS):δ7.19-7.17(m,5H,Aryl-H),7.09-7.06(...

Embodiment 3

[0067] Example 3, preparation of 2-(2,6-dibenzhydryl-4-methylaniline)-3-(2,6-diethylaniline) butane [L2]

[0068] 2-(2,6-Dibenzhydryl-4-methylaniline) butanone (1.00g, 1.97mmol) and 2,6-diethylaniline (0.30g, 2.00mmol) in toluene (50mL) Add a catalytic amount of p-toluenesulfonic acid, and heat to reflux for 6h. The solvent toluene was removed, and the residue was subjected to silica gel column chromatography with a mixed solvent of petroleum ether and ethyl acetate at a volume ratio of 50:1. The eluted fractions were examined through a thin-layer silica gel plate, the first fraction was collected, and the solvent was removed to give a yellow solid. Yield: 42.3%. Melting point: 162°C. The structure confirmation data are as follows: FT-IR(KBr,cm -1 ):3060(w),3025(m),2962(w),2168(w),1977(w),1649(s),1599(m),1494(s),1448(s),1420(w ),1355(m),1251(m),1118(s),1077(m),1030(m),918(w),858(w),768(m),746(m),697(s ). 1 H NMR (400MHz, CDCl 3 ,TMS):7.20-7.16(m,8H,Aryl-H),7.10-7.09(m,...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
melting pointaaaaaaaaaa
melting pointaaaaaaaaaa
melting pointaaaaaaaaaa
Login to View More

Abstract

The invention relates to an asymmetric benzhydryl alpha-diimine nickel complex, a preparation and an application thereof; a structural formula is shown as a formula I, R1 is selected from benzhydryl or fluoro benzhydryl; R2 is selected from methyl or chlorine; R3 is selected from methyl, ethyl or isopropyl; R4 is selected from methyl or hydrogen, X is selected from bromine or chlorine; under room temperature condition, and a compound in a formula V is reacted with NiBr2 or NiCl26H2O to obtain a formula I. Under effect of a cocatalyst methylaluminoxane or modified methylaluminoxane, the complex has catalysis ethene polymerization with higher activity (as high as 107g.mol<-1> (Ni).h<-1>), the obtained polymer has high molecular weight, and the molecular weight distribution has obvious bimodal distribution characteristic, so that the bimodal distribution is the polyethylene material with good processing property.

Description

technical field [0001] The invention relates to an unsymmetrical alpha-diimine nickel complex and its preparation and application in catalyzing olefin polymerization. Background technique [0002] Polyethylene is the world's fastest growing synthetic resin with the largest output and a wide range of uses. It is widely used in many fields such as industry, agriculture, military, medical and health care, and daily life. The improvement of the world's polyethylene production capacity has also promoted the development of polyethylene product performance and production technology. The progress of process and catalyst technology has further improved the performance of polyethylene. Compared with ordinary polyethylene products, the products produced by bimodal polyethylene technology have more excellent performance, so they are attracting more and more attention. The advantage of polyethylene with a bimodal molecular mass distribution is that it contains a very short polymer molec...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/04C08F4/70C08F10/02
Inventor 毛静朱柏青张文娟义建军张明革李红明李荣波贾德东王仪森谭魁龙孙天旭孙文华
Owner PETROCHINA CO LTD