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Synthesis method of polyketone

A kind of synthesis method, the technology of polyketone

Active Publication Date: 2020-01-14
CHAMBROAD CHEM IND RES INST CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In terms of preparation process, since the volume of polyketone that can be accommodated in a batch-type reactor is constant and the bulk density is low, the amount of polyketone produced by a single reactor is low, and the catalytic activity of the catalyst is relatively reduced; and polyketone The bulk density of the product is low, which will easily cause the solvent in the kettle to be absorbed by the fluffy polyketone product, resulting in that the polyketone product cannot be released from the bottom of the kettle; secondly, the low bulk density will cause the product to hang on the wall, and it will be difficult to clean the high-pressure reactor, which will affect the process Fluency of the process

Method used

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  • Synthesis method of polyketone
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  • Synthesis method of polyketone

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preparation example Construction

[0023] The invention provides a kind of synthetic method of polyketone, comprises the following steps:

[0024] Carbon monoxide and olefins are polymerized in a solvent containing mineral powder, polyketone powder, catalyst and ligand to obtain polyketone;

[0025] The mineral powder includes one or more of talcum powder, mica powder, montmorillonite and apatite.

[0026] In the synthesis method provided by the invention, firstly, mineral powder, polyketone powder, catalyst and ligand are added to the solvent. Wherein, the mineral powder includes one or more of talcum powder, mica powder, montmorillonite and apatite; the particle size of the mineral powder is preferably 1 nm to 100 μm, specifically 1 nm, 10 nm, 20 nm, 50nm, 70nm, 100nm, 150nm, 200nm, 500nm, 700nm, 800nm, 1μm, 5μm, 10μm, 15μm, 20μm, 50μm, 70μm, 100μm; the amount ratio of the mineral powder to the solvent is preferably (0.01-0.1) g: 100mL, specifically 0.01g: 100mL, 0.015g: 100mL, 0.02g: 100mL, 0.025g: 100mL, ...

Embodiment 1

[0041] Preparation of CO / ethylene / propylene terpolymer

[0042] Add 250mL of methanol, 9.7mg of p-benzoquinone, 14.8mg of magnesium trifluoromethanesulfonate, 2mL of trifluoromethanesulfonic acid solution (7.5mmol / L), 0.08g of mica powder (particle size 100-150nm) into a 500mL autoclave , 2g polyketone powder (particle size 100~200μm, bulk density 0.21g / mL), and catalyst solution: 10mL acetone, 1.7mg palladium acetate, 6mg 3,3-bis-[bis-(2-methoxybenzene yl)phosphinomethyl]-1,5-dioxa-spiro[5,5]undecane. Wherein, the polyketone powder is a terpolymer obtained by polymerization reaction using CO, ethylene and propylene as reactants.

[0043] After adding the above-mentioned substances, the autoclave was filled with nitrogen for pressure maintenance and replacement, then filled with 15g of propylene, and filled with CO:C 2 h 4 = When the mixed gas of 47:53 reaches 5MPa, start to heat up, set the temperature at 85°C, and stir at a speed of 400r / min. When the temperature rises to...

Embodiment 2

[0048] Preparation of CO / ethylene binary polymer

[0049] Add 300mL of methanol, 15.2mg of p-benzoquinone, 25.6mg of magnesium trifluoromethanesulfonate, 1.5mL of p-toluenesulfonic acid solution (7.5mmol / L), 0.06g of talcum powder (particle size 10-50μm) into a 1L autoclave , 4g polyketone powder (particle size 80-160μm, bulk density 0.22g / mL), and catalyst solution: 15mL acetone, 2.42mg palladium acetate, 3.75mg 2,2-dimethoxy-1,3-bis[ Bis(2-methoxyphenyl)phosphino]propane. Wherein, the polyketone powder is a binary polymer obtained by polymerizing CO and ethylene as reactants.

[0050] After adding the above substances, the autoclave is filled with nitrogen to keep the pressure, replaced, and filled with CO:C 2 h 4 = When the mixed gas of 40:60 reaches 5.2MPa, start to heat up, set the temperature at 95°C, and stir at a speed of 300r / min. When the temperature rises to 95°C, continue to add CO:C 2 h 4 =40:60 mixed gas, maintain the reaction pressure at 5.2MPa, and the rea...

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Abstract

The invention belongs to the technical field of chemical engineering, and particularly relates to a synthesis method of polyketone. The synthesis method comprises a step of subjecting carbon monoxideand olefin to a polymerization reaction in a solvent containing mineral powder, polyketone powder, a catalyst and a ligand so as to obtain polyketone, wherein the mineral powder comprises one or moreselected from the group consisting of talcum powder, mica powder, montmorillonite and apatite. According to the synthesis method provided by the invention, polyketone powder and specific mineral powder are used as seed crystals and are added into a polymerization reaction system at the beginning of the reaction, so the bulk density of the synthesized polyketone product is effectively improved. Experimental results show that the bulk density of the polyketone product obtained by using the synthesis method provided by the invention can be increased from 0.09 g / mL to 0.32 g / mL compared with traditional synthesis processes.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a synthesis method of polyketone. Background technique [0002] Since the 1980s, the alternate copolymerization of CO and ethylenically unsaturated hydrocarbons into polyketones has been favored by academia and industrial applications. Polyketone is a green polymer material with excellent comprehensive properties, which can be used as general-purpose plastics, engineering plastics, special engineering plastics, fibers and films. The ketone group on the main chain of polyketone endows it with excellent photodegradability and chemical modification performance. The main raw materials of polyketone come from a wide range of sources, and CO can be obtained from coal gas production, and can also be obtained from CO-containing industries. It can be obtained through purification of exhaust gas, which makes the synthesis and application of polyketone truly a green s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G67/02C08K3/34C08K3/32
CPCC08G67/02C08K3/32C08K3/34C08K3/346C08K2003/325
Inventor 曹丽艳裴立军刘英贤杨鹏飞王朋朋王旭亮刘文超郭龙龙
Owner CHAMBROAD CHEM IND RES INST CO LTD
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