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Ethylene oligomerization catalyst and method for continuously producing 1-hexene and 1-octene

An ethylene oligomerization and catalyst technology, which is applied in chemical instruments and methods, catalysts, and bulk chemical production, etc., can solve problems such as affecting the heat transfer of the reactor, clogging the pipeline, affecting the continuous operation time of the device, etc. The effect of reducing pipeline blockage and improving plant running time

Active Publication Date: 2021-09-28
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the biggest difficulty affecting the industrial application of ethylene oligomerization is the accumulation of high polymers, which affects the continuous operation time of the device
A small amount of PE generated by the oligomerization reaction will remain in the reactor and the pipeline, affecting the heat transfer of the reactor, or blocking the pipeline

Method used

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  • Ethylene oligomerization catalyst and method for continuously producing 1-hexene and 1-octene
  • Ethylene oligomerization catalyst and method for continuously producing 1-hexene and 1-octene
  • Ethylene oligomerization catalyst and method for continuously producing 1-hexene and 1-octene

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Ligand preparation: (1) Dissolve 4.5 mol of pyrrole in 400 ml of dichloromethane, and cool the mixed solution to -70°C; (2) Start stirring, and slowly add 4 mol of n-butyl lithium dropwise to the mixed solution successively After 10 minutes, add 2mol methylcyclohexyldichlorosilane and 0.22mol trifluoroacetic acid, react for 5 hours and place the mixed reaction solution at room temperature for 36 hours; (3) filter the insoluble matter in the mixed reaction solution, cool Slowly add 3.5 mol of diphenylphosphine chloride dropwise to the filtrate at -5°C, react for 3 hours and then place the reaction solution at room temperature for 6 hours; (4) Purify the reaction solution by column chromatography and rinse with tetrahydrofuran , the white solid powder obtained by evaporating the solvent is the PNSiNP ligand of the present invention, and the nuclear magnetic data of the above-mentioned ligand is as follows: 1H NMR (400MHz, CDCl ): 7.28~7.45 (m, 22H), 6.27~6.33 (m , 4H), 1....

Embodiment 2

[0067] Catalyst preparation: weigh 10mmol of CrCl 3 (THF) 3 , 20mmol of PNSiNP ligand and 18mmol of trityl tetrakis (pentafluorophenyl) borate, according to the method of Example 1, configure the methylcyclohexane of 0.5umolCr / mL into 20L with methylcyclohexane The solution was stored in a 30L catalyst storage tank under nitrogen protection.

[0068] Alkylaluminum compound dilution: 130g of triisobutylaluminum (20wt% Al) was diluted 200 times (mass ratio) with methylcyclohexane and stored in a 30L booster tank under high-purity nitrogen protection.

[0069] Continuous response:

[0070] Such as figure 1 As shown, the continuous preparation of 1-hexene and 1-octene includes the following process:

[0071] Before the continuous reaction starts, the reaction kettle and the overflow tank reactor were heated to 130°C respectively, and the whole reaction system was purged with nitrogen for 7 hours. After the temperature dropped to room temperature, it was replaced with ethylene ...

Embodiment 3

[0076] Catalyst preparation: weigh 10mmol of CrCl 3 (THF) 3 , 18mmol of PNSiNP ligand and 40mmol of N,N-dimethylanilinium tetrakis (pentafluorophenyl) borate, according to the method of Example 1, configure 20L of 0.5umolCr / mL with methylcyclohexane Methylcyclohexane solution, stored in a 30L catalyst storage tank protected by nitrogen.

[0077] Alkylaluminum compound dilution: 110g of triisobutylaluminum (20wt% Al) was diluted 200 times (mass ratio) with methylcyclohexane and stored in a 30L booster tank under high-purity nitrogen protection.

[0078] Continuous response:

[0079] Such as figure 1 As shown, the continuous preparation of 1-hexene and 1-octene includes the following process:

[0080] Before the start of the continuous reaction, the reactor and overflow tank reactor were heated to 130°C respectively, and the entire reaction system was purged with nitrogen for 9 hours. After the temperature dropped to room temperature, it was replaced with ethylene for three ...

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Abstract

The invention discloses a method for continuously producing 1-hexene and 1-octene, the method comprises the following steps: (1) mixing a solvent and an aluminum alkyl compound through a mixing tank, continuously introducing the mixture into a reaction kettle, introducing ethylene, and carrying out ethylene oligomerization reaction under the action of a continuously introduced catalyst to obtain a reaction solution containing 1-hexene and 1-octene; (2) a reaction solution containing 1-hexene and 1-octene enters an overflow tank reactor through an overflow pipeline; and (3) enabling the reaction liquid obtained in the overflow tank reactor to enter a quenching reactor, and quenching the reaction by using an alcohol substance as a quenching agent to obtain 1-hexene and 1-octene. The used catalyst is a solution formed by a metal chromium compound, a PNSiNP ligand and an organic boron compound. Under the condition that the reaction temperature is not changed, the overflow tank adopts a higher temperature, and a polymer from the reaction kettle can be dissolved in a reaction solution, so that the possibility of pipeline blockage is reduced, and the continuous operation time of the device is prolonged.

Description

technical field [0001] The invention belongs to the field of ethylene oligomerization technology, and relates to an ethylene oligomerization catalyst and a method for continuously producing 1-hexene and 1-octene. Background technique [0002] Linear α-Olefins (linear α-Olefins, LAOs) are important organic chemical raw materials, among which 1-octene and 1-hexene are the most widely used. As an important organic raw material and chemical intermediate, 1-octene is mainly used in the production of high-end PE and POE, as well as raw materials for the production of plasticizers, detergent alcohols and lubricating oil additives. 1-Hexene is mainly used in the production of linear low density polyethylene (LLDPE) and high density polyethylene (HDPE). 1-hexene and 1-octene products are also included in the National Petroleum and Chemical Industry Development Guidelines to encourage key development of chemical products. Ethylene oligomerization is currently one of the main methods...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C2/22C07C2/32C07C11/02C07C11/107B01J31/14
CPCB01J31/188B01J31/2247C07C2/32C07C2/22B01J31/146B01J2231/20B01J2531/62C07C2531/22C07C11/02C07C11/107Y02P20/52
Inventor 刘帮明陈冠良张彦雨郭华黄传兵黄玲燕王金强刘万弼陈海波
Owner WANHUA CHEM GRP CO LTD
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