Method for synthesizing short-chain olefin by ethylene oligomerization
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A technology of ethylene oligomerization and oligomerization, which is applied in the field of olefin oligomerization, can solve the problems of difficult separation of catalyst and product, difficult synthesis of catalyst, poor stability, etc., and achieve the effects of improved catalytic activity, good thermal stability, and high activity
Inactive Publication Date: 2008-06-18
SUN YAT SEN UNIV
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[0006] The purpose of the present invention is to overcome the problems of difficult catalyst synthesis, poor stability, and difficult separation of catalyst and product in the existing olefin oligomerization technology, and provide a method for ethylene oligomerization into short-chain olefins. and catalysts with good stability, and realize the easy separation of catalysts and products, and a catalytic system that can be recycled and reused
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Embodiment 1
[0017] Embodiment 1: the synthesis of aluminate imidazolium ionic liquid
[0018] Under anhydrous and oxygen-free conditions, at 0°C, take 30.5g of anhydrous AlCl 3 (0.229mol) was added to 33.3g of 1-butyl-3-methylimidazole chloride (0.191mol), then the temperature was raised to 40°C, and stirred overnight to obtain an imidazolium-aluminate ionic liquid with a molar ratio of 1.2.
[0019]
Embodiment 2
[0020] Embodiment 2: the synthesis of double salicylaldamine nickel compound 1
[0021] 1ml of salicylaldehyde (12.9mmol) was added to the solution containing 6.85g (38.7mmol) of 2,6-diisopropylaniline, 1.60g of Ni(OAc) 2 4H 2 O (6.45mmol) in 100ml ethanol solution, heated to reflux for 4h, cooled to room temperature, a large amount of green crystals were generated, filtered, and recrystallized in n-heptane to obtain fine granular green crystals, weighing 2.62g, yield 65.6 %. Elemental analysis (by C 38 h 44 N 2 NiO 2 Calculated, %), theoretical value: C, 73.68, H, 7.16, N, 4.52; found value: C, 73.66, H, 7.31, N, 4.43.
Embodiment 3
[0022] Embodiment 3: the synthesis of double salicylaldamine nickel compound 2
[0023] 1ml of salicylaldehyde (12.9mmol) was added to the solution containing 2.28g (38.7mmol) n-propylamine, 1.60gNi(OAc) 2 4·H 2 In 100ml ethanol solution of O (6.45mmol), heat and reflux for 4h, cool to room temperature, generate a large amount of green crystals, filter, recrystallize in n-heptane to obtain granular green crystals, weighing 1.55g, yield 62.8% . Elemental analysis (by C 20 h 24 N 2 NiO 2 Calculated, %), theoretical value: C, 62.70, H, 6.31, N, 7.31; found value: C, 62.68, H, 6.41, N, 7.29.
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Abstract
The invention discloses a method for a short chain olefin hydrocarbon through an ethylene oligomeric. The invention is characterized in that: the dual salicylaldehyde imine nickel catalyst is loaded in imidazole Al-ionic ionic liquid; under the assistant catalysis of AlEt2Cl, the ethylene oligosaccharide can be catalyzed in two phase in a mild reaction condition. Comparing with a homogeneous system, the activity of the catalyst system in the ionic liquid can be improved greatly; all generative products are ethylene oligomeric, and the production can be separated through a simple settlement. The ionic liquid of the catalyst can be recycled by being dissolved. The reaction condition has no great impact to the distribution of the oligomeric production. The test result of gas chromatography mass spectrum that the ethylene oligomeric production mainly is a short chain olefin hydrocarbon with the carbon atom of less than 10. Compared with the tradition of salicylaldehyde imine nickel catalyst 1 and 2, the catalyst 3 and 4 after the ion function has a higher activity and a better thermal stability. The test for atomic emission spectroscopy of the plasma shows that the recovery rate of catalyst 1 and 2 can be more than 98 percent, while that of the catalyst 3 and 4 after the ion function can reach 99.9 percent.
Description
technical field [0001] The invention relates to the field of olefin oligomerization, in particular to a method for preparing short-chain olefins by using a catalyst to catalyze ethylene oligomerization. Background technique [0002] Ethylene oligomerization is an important petrochemical industry. Short-chain olefins synthesized through ethylene oligomerization are an important class of chemical raw materials. According to different chain lengths, they are widely used in detergents, plasticizers, lubricating oils, surfactants, etc. There are a wide range of uses. Alternatively, linear alpha-olefins (LAO) can be used as comonomers (such as 1-butene, 1-hexene, and 1-octene) to be copolymerized with ethylene to produce various commercial brands of branched polyethylene (LLDPE) or elastomeric body material. [0003] At present, the ethylene oligomerization catalysts in the industry are mainly the alkylaluminum catalysts of BP Amoco, the nickel catalysts of Shell's SHOP process,...
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