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A kind of ethylene oligomerization catalyst and method for continuous production of 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: 2022-07-12
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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  • A kind of ethylene oligomerization catalyst and method for continuous production of 1-hexene and 1-octene
  • A kind of ethylene oligomerization catalyst and method for continuous production of 1-hexene and 1-octene

Examples

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) Turn on stirring, slowly add 4 mol of n-butyllithium dropwise to the mixed solution After 10 minutes, 2 mol of methylcyclohexyl dichlorosilane and 0.22 mol of trifluoroacetic acid were added, and after 5 hours of reaction, the mixed reaction solution was placed at room temperature to react for 36 hours; (3) the insolubles in the mixed reaction solution were filtered out, cooled To -5°C, slowly add 3.5 mol of diphenylphosphine chloride dropwise to the filtrate, react for 3 hours, and 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: 1HNMR (400MHz, CDCl3): 7.28~7.45 (m, 22H...

Embodiment 2

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

[0068] Alkyl aluminum compound dilution: 130 g 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] like figure 1 As shown, the continuous production of 1-hexene and 1-octene includes the following processes:

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

Embodiment 3

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

[0077] Alkyl aluminum compound dilution: 110 g 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] like figure 1 As shown, the continuous preparation of 1-hexene and 1-octene includes the following processes:

[0080] Before the continuous reaction started, the reaction kettle and the overflow tank reactor were heated to 130°C respectively, and the whole reaction system was purged with nitrogen for 9 hours. After the temperature dropped to room temperature, it was replaced wi...

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Abstract

The invention discloses a method for continuous production of 1-hexene and 1-octene, comprising: (1) after mixing a solvent and an alkyl aluminum compound in a mixing tank, they are continuously introduced into a reaction kettle, and ethylene is introduced into the reaction kettle. Under the effect of the catalyzer that feeds, ethylene oligomerization reaction occurs, obtains the reaction solution containing 1-hexene and 1-octene; (2) the reaction solution containing 1-hexene and 1-octene enters through overflow line to the overflow tank reactor; (3) the reaction solution obtained by the overflow tank reactor enters the quenching reactor, and uses alcohols as a quenching agent to quench the reaction to obtain 1-hexene and 1-octene. Wherein, the catalyst used is a solution formed by a metal chromium compound, a PNSiNP ligand and an organic boron compound. In the invention, without changing the reaction temperature, the overflow tank adopts a higher temperature, and the polymer from the reaction kettle can be dissolved in the reaction liquid, thereby reducing the possibility of pipeline blockage and improving the continuous operation time of the device.

Description

technical field [0001] The invention belongs to the technical field of ethylene oligomerization, and relates to an ethylene oligomerization catalyst and a method for continuously producing 1-hexene and 1-octene. Background technique [0002] Linear α-olefins (linearα-Olefins, LAOs) are important organic chemical raw materials, of 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, POE and as a raw material for plasticizers, alcohols for detergents and lubricant 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 listed 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 for preparing linear α-olefins (...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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