Preparation method of high-purity 1-butene

A high-purity butene technology, applied in the field of olefin polymerization, can solve problems such as reduced catalytic activity and unbalanced mixing ratio, and achieve the effects of reduced processing costs, high selectivity, and strong controllability

Active Publication Date: 2021-04-16
PETROCHINA CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] China Taiwan patent TW201609612 discloses a catalytic system comprising an alkoxy or aryloxy compound, an ether compound, and an alkylaluminum compound for selective ethylene dimerization. By adjusting the ether compound and the The molar ratio between the alkoxyl or aryloxytitanium compounds, and the alkyl substituents on the alkylaluminum, can be 1-butene selectivity greater than or equal to 90%, but the mixing ratio imbalance between multi-component catalysts is easy to cause Reduced catalytic activity and formation of by-product polymers

Method used

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preparation example Construction

[0027] The invention provides a kind of preparation method of high-purity 1-butene product, comprises the following steps:

[0028] Under anhydrous and oxygen-free conditions, the titanium source with a Ti-O bicyclic structure and the alkylaluminum are separately prepared in a fixed ratio, dissolved in a solvent, and the molar ratio of the catalyst titanium source to the alkylaluminum co-catalyst is 1:0.5 In the range of ~10, the reaction solvent needs to be dehydrated in advance to ensure that the water content is lower than 10ppm.

[0029] After replacing the heat of the ethylene polymerization reactor, add the solvent, raise it to a certain temperature and pressure, then add the prepared binary catalyst, control the reaction temperature during the reaction, and continuously replenish ethylene to ensure a stable reaction temperature and pressure. The preferred reaction pressure is 1MPa, 1.5MPa, 2.0MPa, 2.5MPa, 3.0MPa, 3.5MPa; the preferred reaction temperature is 30°C, 35°C,...

Embodiment 1

[0035] Heat the alkane solvent to 130°C to clean the high-pressure reactor, and then vacuumize at 110°C after discharging to ensure that the reactor is completely dry, then cool the reactor to 60°C, and replace the gas in the reactor with high-purity nitrogen for 3 Then use ethylene gas to evacuate several times, add 200ml of heptane solvent into the reactor, maintain the system temperature to 50°C, and select tetrakis(2-ethyl-1,3-hexanediol)titanium as catalyst titanium source (Ti[OCH 2 CHCH 2 CH 3 CHCH 2 CH 2 CH 3 O] 2 ), cocatalyst triisobutylaluminum, titanium / aluminum ratio of 1:5, after reacting for 5 hours at 2.5MPa and 55°C, the products in the reactor were collected and analyzed by gas chromatography. The results are shown in Table 1.

Embodiment 2

[0037] Heat the alkane solvent to 130°C to clean the high-pressure reactor, and then vacuumize at 110°C after discharging to ensure that the reactor is completely dry, then cool the reactor to 60°C, and replace the gas in the reactor with high-purity nitrogen for 3 Then use ethylene gas to evacuate several times, add 200ml of hexane solvent into the reactor, maintain the system temperature to 45°C, select tetrakis(2-ethyl-1,3-hexanediol)titanium as catalyst titanium source (Ti[OCH 2 CHCH 2 CH 3 CHCH 2 CH 2 CH 3 O] 2 ), cocatalyst triethylaluminum, titanium / aluminum ratio of 1:5, reacted at 2.5MPa, 50°C for 4 hours, collected the products in the reactor, and analyzed the composition by gas chromatography, the results are shown in Table 1.

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Abstract

The invention discloses a preparation method of high-purity 1-butene, which comprises the following steps of carrying out dimerization reaction with higher activity on ethylene in a binary catalyst system with a Ti-O bicyclic structure by controlling the reaction pressure, temperature, catalyst ratio and retention time to generate an intermediate product with the 1-butene content of 90% or above, and carrying out pressurized rectification, and separating a 1-butene product with the purity of more than or equal to 99.47% from the tower top. The product can be directly used for polyethylene comonomers.

Description

technical field [0001] The invention relates to the field of olefin polymerization, in particular to a method for preparing a high-purity 1-butene product. Background technique [0002] 1-butene is the main comonomer of low-density polyethylene (LLDPE) and high-density polyethylene (HDPE) in the production line. The consumption of 1-butene comonomer is huge in my country, mainly from the separation of mixed carbon four from ethylene crackers However, the production of polymer grade 1-butene by this route has the defects of high separation difficulty and high impurity content. In recent years, great changes have taken place in my country's C4 industry, and the scarcity of mixed C4 raw materials has seriously affected the production of 1-butene by cracking C4 separation. [0003] The technology of producing 1-butene with ethylene as raw material has the advantages of high product purity and low processing cost. In the past, due to the cost of ethylene raw material, its industr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C11/08C07C2/26C07C2/30C07C7/04C08F210/16C08F210/08
Inventor 蒋岩王斯晗褚洪岭徐显明王力搏霍宏亮牟玉强于部伟马立莉黄付玲
Owner PETROCHINA CO LTD
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