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Preparation of Heteroatom Ligand of Sulfur and Nitrogen and Its Application

A technology of sulfur nitrogen heteroatoms, which is applied in the preparation of sulfur nitrogen heteroatom ligands and the application field of the ligands, can solve problems such as bad odor, and achieve the effect of reducing the use and simplifying the synthesis steps

Active Publication Date: 2016-08-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the synthesis process of the above two kinds of sulfur and nitrogen heteroatom ligands, it is necessary to use thiols with malodorous substances and amine hydrochlorides with high toxicity.

Method used

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  • Preparation of Heteroatom Ligand of Sulfur and Nitrogen and Its Application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The preparation of embodiment 1 sulfur nitrogen heteroatom ligand

[0039] Preparation of (di-(2-ethylthio-ethyl)-amine)

[0040] At -15°C, dissolve 8.0g (100mmol) of sodium hydroxide solution and 12.46g (100mmol) of 2-chloroethyl ethyl sulfide in 200ml of ethanol, and then add 2mol / LNH 3 25ml of methanol solution was added thereto. The solution was stirred at -15°C for 2 hours and then at room temperature for 15 hours. After the reaction was completed, filter, evaporate the filtrate to dryness, and add the residue to 50ml of diethyl ether to filter again and evaporate to dryness. After repeated several times, a light yellow oily product was obtained with a yield of 8.85g (92%). 1 H-NMR (CDCl 3 ): δ1.20 (6H, t, CH 3 ), 2.50 (1H, s, NH), 2.57 (4H, q, SCH 2 CH 3 ), 2.70 (4H,t,Sch 2 ), 2.83 (4H, t, NCH 2 ).

Embodiment 2

[0041] The preparation of the chromium complex of embodiment 2 sulfur nitrogen heteroatom ligand

[0042] Preparation of chromium trichloride (di-(2-ethylthio-ethyl)-amine)

[0043] At room temperature, a solution of 3.18 g (16.5 mmol) of di-(2-ethylthio-ethyl)-amine prepared in Example 1 in 50 ml THF was added to a solution containing 5.62 g (15 mmol) of CrCl 3 (THF) 3 150ml THF solution. After stirring was continued for 30 minutes, the solvent was removed in vacuo until a residue of 30 ml remained. Another 80 mL of ether was added, the solution was filtered and the solids were washed. A first wash with a mixture of ether and THF (100ml each) followed by a 50ml ether wash. The solid was dried under vacuum. Yield: 3.88 g (76.8%).

[0044] The elemental analysis instrument was CE-440 produced by Jialian Instrument Co., Ltd. of the United States.

[0045] The atomic absorption instrument is AA-400 produced by PerkinElmer, USA.

[0046] Elemental analysis of the product: ...

Embodiment 3

[0049] The preparation of embodiment 3 sulfur nitrogen heteroatom ligands

[0050] Preparation of (di-(2-phenylthio-ethyl)-amine)

[0051] At -5°C, dissolve 8.0g of sodium hydroxide and 17.26g (100mmol) of 2-chloroethylbenzene sulfide in 200ml of ethanol, and then add 2mol / LNH 3 25ml of methanol solution was added thereto. The solution was stirred at -5°C for 3 hours, then at room temperature for 20 hours. After filtering, the filtrate was evaporated to dryness, and the residue was added to 60ml of diethyl ether to filter again and evaporate to dryness. After repeated several times, 18.5g of bis(2-phenylthio-ethyl)-amine (yield: 64% ). 1H-NMR (CDCl 3 ): 2.05 (1H, s, NH), 7.28 (8H, d, CH), 7.24 (2H, d, CH), 2.89 (8H, t, CH 2 ).

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Abstract

The invention relates to a preparation method of a sulfur and nitrogen heteroatom ligand and application thereof in catalyst preparation and olefin polymerization. The preparation method comprises use of R1SR2X and ammonia for reaction in alkaline conditions to obtain (R1SR2)2NH, and the method provides a method for synthesizing the non-toxic or low-toxicity sulfur and nitrogen heteroatom ligand, simplifies the synthesis steps, and reduces the use of highly toxic chemicals in the testing process. In addition, the invention also relates to a preparation method of a chromium based catalyst for olefin oligomerization and application of the chromium based catalyst in ethylene trimerization, and the preparation method of the chromium based catalyst comprises the preparation method of the sulfur and nitrogen heteroatom ligand.

Description

technical field [0001] The present invention relates to a preparation method of a ligand and a catalyst system, specifically, the present invention further relates to a preparation method of a sulfur nitrogen heteroatom ligand and its application in olefin oligomerization Background technique [0002] The oligomerization of olefins, mainly α-olefins, using chromium-based catalysts has been extensively studied. More precisely, many chromium-based catalysts have been developed and used for the oligomerization of olefins to produce α-olefins. Among them, the trimerization of ethylene into 1-hexene and the tetramerization of ethylene into 1-octene are of special significance. Compared with the copolymer of 1-butene, the LLDPE resin copolymerized by 1-hexene and 1-octene has significantly better tensile strength, impact strength, tear resistance and durability, especially suitable for packaging films And greenhouses, sheds and other agricultural covering films. In terms of α-o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/20C07C323/25B01J31/22C07C2/30C07C2/22C07C11/107
CPCY02P20/52
Inventor 祁彦平隋军龙吴红飞栗同林刘珺韩春卉王霄青
Owner CHINA PETROLEUM & CHEM CORP
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