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A preparation method of a compatibilizer containing multifunctional groups with controllable polarity

A multi-functional group and compatibilizer technology, applied in the production of bulk chemicals, etc., can solve the problems of weak two-phase interface adhesion, single structure, narrow application range, etc., to solve poor compatibility, reduce The effect of interfacial tension and size adjustable and controllable

Inactive Publication Date: 2018-07-31
HEBEI UNIV OF TECH
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Problems solved by technology

The compatibilizers used in the above patents all have the same disadvantages: they all use polyolefin grafted maleic anhydride as a compatibilizer, and maleic anhydride is usually directly grafted to the main chain of polyolefin in the form of a monomer In general, the grafting rate is very low, and the active functional group is only an anhydride group, so the activity is not high; in addition, due to the single structure of this type of compatibilizer, the scope of application is narrow, especially for high-performance and functional polymer materials. The improvement of requirements, so it is urgent to research and develop new compatibilizers
Although this compatibilizer has also played the role of compatibilizer, this compatibilizer still has deficiencies: (1) formaldehyde reacts with polyethylene polyamine to obtain the polar part of compatibilizer, but formaldehyde activity is low, in the reaction It only acts as a bridge, and the obtained polar part only contains a functional group of amino group, resulting in low activity of the polar part; in addition, formaldehyde is highly toxic, which is not conducive to the health of the human body and the protection of the environment; (2) the compatibilizer is It is made by the action of polar part, polyolefin grafted maleic anhydride, and nanoparticles. Due to the low activity of the polar part, there are very few polyolefin grafted maleic anhydride and nanoparticles connected to the polar part, which directly leads to The grafting rate of the prepared compatibilizer is very low
Adding a compatibilizer to an incompatible polymer blend system, due to the low grafting rate of the compatibilizer, makes the interfacial cohesion of the two phases weak and the blending effect is not very good

Method used

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  • A preparation method of a compatibilizer containing multifunctional groups with controllable polarity
  • A preparation method of a compatibilizer containing multifunctional groups with controllable polarity
  • A preparation method of a compatibilizer containing multifunctional groups with controllable polarity

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Embodiment 1

[0029] (1) Epoxypropyltrimethylammonium chloride (>96%, Dongying Yisheng Petroleum Technology Development Co., Ltd.) is added to the graphene oxide aqueous solution with a concentration of 1.00g / L until the solution becomes clear and transparent, and the room temperature React for 2 hours. The obtained flocculent precipitate was filtered, washed and dried to obtain intermediate 1. Wherein, the glycidyltrimethylammonium chloride add-on in the solution is 2.75g / L.

[0030] (2) Add 0.05mol of epichlorohydrin (analytically pure, Tianjin Bodi Chemical Co., Ltd.) dropwise to a reactor containing 0.05mol tetraethylenepentamine (analytical pure, Tianjin Fuchen Chemical Reagent Factory) , 40ml of water was used as a solvent, the temperature was maintained at 50°C, the dropwise addition was completed in 0.5h, and the reaction was carried out at 99°C for 8 hours. Rotary evaporation was carried out after cooling down. The temperature of the rotary evaporation was set at 65° C. for 2 hou...

Embodiment 2

[0039] (1) Glycidyltriethylammonium bromide was added to a graphene oxide aqueous solution with a concentration of 1.20 g / L until the solution became clear and transparent, and reacted at room temperature for 2 hours. The obtained flocculent precipitate was filtered, washed and dried to obtain intermediate 1. Wherein, the glycidyltriethylammonium bromide add-on in the solution is 2.80g / L.

[0040] (2) Add 0.06 mol of epichlorohydrin dropwise to a reactor containing 0.06 mol of diethylenetriamine, and 40 ml of water as a solvent. The temperature is maintained at 45° C. After 0.5 hours of dropping, react at 98° C. 8 hours. Rotary evaporation was carried out after cooling down. The temperature of the rotary evaporation was set at 65° C. for 2 hours, and the obtained product was dried to obtain intermediate 2.

[0041] (3) 2.5g low-density polyethylene grafted maleic anhydride and 7.0g intermediate 2 were mixed in 40ml xylene, and phase transfer catalyst tetrabutylammonium bromi...

Embodiment 3

[0044] (1) Add glycidyltriethylammonium iodide to a graphene oxide aqueous solution with a concentration of 2.00 g / L until the solution becomes clear and transparent, and react at room temperature for 2 hours. The obtained flocculent precipitate was filtered, washed and dried to obtain intermediate 1. Wherein, the epoxypropyltriethylammonium iodide add-on in the solution is 3.50g / L.

[0045] (2) Add 0.1 mol of epichlorohydrin dropwise to a reactor containing 0.05 mol of ethylenediamine, and 45 ml of water as a solvent. The temperature is maintained at 50°C, and the dropwise addition is completed in 0.5h, and the reaction is carried out at 98°C for 9 Hour. Rotary evaporation was performed after cooling down, the temperature of the rotary evaporation was set at 68° C., and the obtained product was dried for 1.5 hours to obtain intermediate 2.

[0046] (3) Mix 2.2g polypropylene grafted maleic anhydride and 7.8g intermediate 2 in 40ml xylene, add 0.05g phase transfer catalyst t...

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Abstract

The present invention is a preparation method of a compatibilizer containing a multifunctional group with controllable polarity. The method includes the following steps: (1) adding glycidyl alkyl salt compounds to the aqueous solution containing nanoparticles and reacting for 1 to 3 hours to obtain intermediate 1; (2) adding cyclic ethylene polyamine dropwise Oxychloropropane, react at 90~100℃ for 6~12 hours, rotary steam to obtain Intermediate 2; (3) Mix the non-polar polymer graft with Intermediate 2 in a solvent, add a phase transfer catalyst , react at 100~160℃ for 5~12 hours to obtain intermediate 3; (4) Mix intermediate 1 and intermediate 3 in a solvent, add a phase transfer catalyst, and react at 80~130℃ for 4~12 hours , to get the product. The compatibilizer obtained by the invention has polar parts with high activity, the grafting rate of the compatibilizer is high, and the abundant polar functional groups on the compatibilizer ensure that two phases are incompatible during the blending process Provides a large number of reactive sites and improves interfacial adhesion.

Description

technical field [0001] The invention belongs to the technical field of compatibilizers. Aiming at typical blending systems of incompatible high polymers, a compatibilizer containing multifunctional groups with controllable polarity is prepared and plays a good compatibilizing effect in the blending system. Improve the performance of blended materials. technical background [0002] The rapid development of modern science and technology and production technology has made people put forward high-performance and high-functional requirements for polymer materials. A single homopolymer and copolymer are often difficult to meet various needs. Blending two or more polymers by physical or chemical methods can significantly improve the performance of the original polymer or form a new performance polymer blends. In recent years, the most striking thing is to use the simplest method to mix the existing two polymers with large structural differences to form a polymer blend system. Ho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L51/06C08L23/06C08L77/02C08K9/04C08K3/04C08K7/24
CPCY02P20/52
Inventor 王月欣李会凡张倩
Owner HEBEI UNIV OF TECH
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