Catalytic composition and process for the dimerisation of ethylene to 1-butene

一种组合物、化合物的技术，应用在碳氢化合物、碳氢化合物、化学仪器和方法等方向，能够解决催化剂失活可操作性难度等问题

Active Publication Date: 2016-01-13
INST FR DU PETROLE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The main disadvantage of titanium-based catalytic systems leading to the selective formation of 1-butene is the formation of non-negligible amounts of polymers, namely polyethylene
The formation of this polyethylene may be responsible for the rapid deactivation of the catalyst and the increased difficulty of operability

Method used

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  • Catalytic composition and process for the dimerisation of ethylene to 1-butene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1: Adduct "THF.AlEt 3 "Synthesis

[0043] Dissolved 0.832 g (7.3 mmol) of AlEt in an inert atmosphere 3 Introduce 25 mL of n-heptane into the Schlenk flask. Next, 0.54 g (7.5 mmol) of THF were added in a controlled manner. The solution was stirred at ambient temperature for about 1 hour. The n-heptane was then removed under dynamic vacuum at ambient temperature. Adduct "THF.AlEt 3 ” was isolated as a colorless liquid in near quantitative yield (95%). 1 HNMR analysis confirmed THF / AlEt 3 The molar ratio is 1.03 / 1.

[0044] 1 HNMR: (300MHz, CD 2 Cl 2 ); δ (ppm): 4.12 (m, 4H); 2.11 (m, 4H); 1.04 (t, 9H); -0.18 (q, 6H).

Embodiment 2-10

[0046] The ethylene dimerization experiments given in Table 1 below were carried out in a stainless steel autoclave with an effective volume of 500 ml, equipped with a jacket for temperature regulation by oil circulation. Agitation is provided using a Rushton impeller with mechanical drive. 40 ml of n-heptane and 5 ml of a 0.085 mol / l solution of a titanium compound in n-heptane were introduced into the reactor under an ethylene atmosphere at ambient temperature. Once the temperature of the reactor reached 53°C, the required amount of aluminum-based cocatalyst (diluted in n-heptane) was introduced under ethylene pressure. For Examples 2-4 (comparative examples), the aluminum-based cocatalyst is AlEt 3 . For Examples 5-10 (according to the invention), the aluminum-based cocatalyst is the adduct THF-AlEt synthesized in Example 1 3 . The ethylene pressure was maintained at 23 MPa, and the temperature was maintained at 53°C. After a reaction time "t" (see Table 1), the introd...

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Abstract

The invention describes a catalytic composition obtained by interaction of an alkyl titanate on the one hand with a preformed mixture of an alkylaluminium and a Lewis base on the other hand. The invention also describes the use of said composition in a process for the selective dimerization of ethylene to 1-butene.

Description

technical field [0001] The present invention relates to a catalytic composition and a method for selectively dimerizing ethylene to 1-butene using the catalytic composition. Background technique [0002] Among catalytic systems capable of selectively dimerizing ethylene to 1-butene, vanadium-based catalytic systems can be identified in the literature (S. Zhang et al., Organometallics 2009, 28, 5925; K. Nomura et al., Inorg. Chem. 2013, 52, 2607), catalytic systems based on iron or cobalt (S.Song et al., J. Organomet. Chem. , 2011, 696, 2594; V.Appukuttan et al., Organometallics 2011, 30, 2285), tungsten-based catalytic systems (H.Olivier et al., J. Moore. Catal. A: Chem. 1999, 148, 43; R.Tooze et al., SasolTechnology WO2005089940A2, 2005), tantalum-based catalytic systems (S.McLain et al., J.Am.Chem.Soc. , 1978, 100(4), 1315; R. Schrock et al., Pure & App. Chem. , 1980,52,729), nickel-based catalytic systems (S.Mukherjee et al., Organometallics 2009, 28, 3074; K. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/14C07C11/08C07C2/26C07C2/30
CPCB01J31/0212B01J31/128B01J2231/20C07C2/30C07C2531/12C07C2531/14Y02P20/52B01J31/143C07C11/08B01J37/00
Inventor L.马尼亚H.奥利维耶-布尔比古
Owner INST FR DU PETROLE
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