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Catalyst composition for preparing polyketone compound, palladium mixed catalyst system, method for preparing polyketone compound using same, and polyketone polymer

A technology for catalysts and compounds, applied in catalyst activation/preparation, organic compound/hydride/coordination complex catalysts, catalyst supports, etc., can solve the problems of difficulty in mass production process, low apparent density, scaling, etc. Achieve good stability and activity, high apparent density, and prevent scaling

Active Publication Date: 2019-02-05
AJOU UNIV IND ACADEMIC COOP FOUND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, existing polyketones made in the form of amorphous slurries cannot adjust their particle shape, so there are problems of low apparent density and low productivity per unit volume of the reactor
This amorphous slurry polyketone particle sticks to reactor surfaces, agitators, transfer pipes, etc., causing fouling problems during batch production
[0005] Moreover, in the existing polyketone preparation methods, it is difficult to increase the activity to a level with industrial applicability without directly using additives such as sulfonic acid (sulfonic acid), but when strong acidic additives are used, there is a tendency to cause condensation. The problem of scale, so it is difficult to apply to the mass production process

Method used

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  • Catalyst composition for preparing polyketone compound, palladium mixed catalyst system, method for preparing polyketone compound using same, and polyketone polymer
  • Catalyst composition for preparing polyketone compound, palladium mixed catalyst system, method for preparing polyketone compound using same, and polyketone polymer
  • Catalyst composition for preparing polyketone compound, palladium mixed catalyst system, method for preparing polyketone compound using same, and polyketone polymer

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preparation example Construction

[0168] Preparation method of polyketone

[0169] Yet another embodiment of the present invention relates to a method for preparing polyketones, which is characterized in that it comprises: the step of dispersing a catalyst composition for preparing polyketides in a solvent; and adding olefin and carbon monoxide to carry out the polymerization step.

[0170] The preparation method of polyketone according to a specific embodiment has the above-mentioned carrier modified with sulfonic acid groups as a heterogeneous material mixed with a palladium-based catalyst, for example, it has the difference from the palladium-based catalyst loaded in the surface modified with sulfonic acid groups The state of the catalyst in the form of a permanent carrier, thereby, when applied to the polyketone polymerization process, etc., uniformly controls the shape and size of the finally prepared polyketone, thereby improving the apparent density of the polyketone and preventing The fouling phenom...

preparation example 1

[0199] Preparation example 1: preparation carries out the carrier of surface modification with sulfonic acid group

[0200] (Prepare carrier)

[0201] 500mL of methanol (Methanol), 90mL of H 2 0. 32 mL of ammonium hydroxide solution (Ammonium hydroxide solution) and 1.2 g of hexadecyltrimethyl ammonium bromide (CTAB) were sequentially added to a 1 L beaker and stirred at 300 RPM for 30 minutes. While stirring at 300 RPM, Tetraethyl orthosilicate (TEOS) was added. While stirring at 300 RPM, react at room temperature for 24 hours. The synthesized silica (Silica) was separated with a centrifuge, washed with methanol and dried in an oven. The dried silica was then calcined at 550 °C for 5 hours. The prepared calcined silica was finely ground in a mortar and heated at 850° C. for 12 hours in an Ar furnace to prepare a support.

[0202] benzyl magnesium chloride was added to the silica carrier prepared above, and stirred at room temperature in a nitrogen atmosphere to generate ...

preparation example 2

[0205] Preparation example 2: preparation carries out the carrier of surface modification with sulfonic acid group

[0206] (Prepare carrier)

[0207] Zinc nitrate hexahydrate (Zinc nitrate hexahydrate, 1eq, 0.1mol, 297.49g / mol, 29.75g) was dissolved in 500mL of methanol to prepare zinc nitrate solution (Zinc nitrate solution), hexadecyltrimethyl bromide Ammonium bromide (Hexadecyltrimethyl ammonium bromide; CTAB, 99+%, 0.25 eq, 0.025 mol, 364.45 g / mol, 9.1 g) was dissolved in 125 mL of methanol to prepare a solution (CTAB solution). And, 2-methylimidazole (4eq, 0.4mol, 82.10g / mol, 32.84g) was dissolved in 500 mL of methanol to prepare a solution (2-methylimidazole solution).

[0208] Add 100mL of zinc nitrate solution prepared above into 250mL of RB (5 pieces), add 20mL of CTAB solution and 100mL of 2-methylimidazole solution sequentially while stirring at 1100rpm, and stir for 5 minutes. Thereafter, stirring was stopped, and the mixture was allowed to stand (room temperatu...

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Abstract

The present invention relates to a catalyst composition for preparing a polyketone compound, the catalyst composition comprising: an onium salt compound having 5 to 40 carbon atoms and comprising a carboxylic acid group or a carrier surface-modified with a sulfonic acid group; and a palladium-based catalyst. Through the catalyst composition, the present invention can provide: a palladium mixed catalyst system capable of showing high activity and preventing fouling in the preparation of polyketone; a method for preparing a polyketone compound, the method being capable of preventing fouling, skipping the feeding of seeds, and attaining excellent stability and activity in a polymerization reaction, by using the palladium mixed catalyst system; and a polyketone polymer with a high apparent density prepared from the method.

Description

technical field [0001] The present invention relates to a palladium mixed catalyst system capable of exhibiting high activity and preventing fouling in the preparation of polyketones, a method for preparing polyketide compounds using the above mixed catalyst system, and a polyketone polymer prepared thereby. Background technique [0002] Polyketones are a type of polymer known as carbon monoxide / olefin copolymers. Recently, polyketones have been actively used as raw materials for high-strength fibers and engineering plastics, and thus their demand is also increasing. The synthesis of such polyketones has good industrial applicability in terms of converting carbon monoxide into useful substances and in being able to provide polymer compounds excellent in physical properties. [0003] In the existing polyketone production method, a catalyst is dissolved in methanol and then added to a reactor to polymerize carbon monoxide and ethylene into polyketone under pressure. In this ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/02B01J31/12B01J23/44B01J32/00B01J37/04C07C309/32C08G67/02
CPCB01J23/44B01J31/12C07C309/32C08G67/02C08L67/02B01J37/0207B01J35/30B01J37/04
Inventor 张慧暎李泍烈林有娜孙性旭朴鲁镇姜信宁卢炯完郑然州
Owner AJOU UNIV IND ACADEMIC COOP FOUND
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