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Preparation method of phosphorus and nitrogen contained acrylate and copolymer core-shell particles of phosphorus and nitrogen contained acrylate

A technology of acrylate and butyl acrylate, which is applied in the preparation of phosphorus-nitrogen-containing acrylate and its copolymer core-shell particles, in the field of polymer chemistry and polymers, can solve the problems of high synthesis cost and unsuitability for industrialization, and achieve composition adjustable effect

Active Publication Date: 2017-02-22
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are two main methods for the preparation of phosphorus-containing acrylates: one is obtained by reacting acryloyl chloride with epoxy or hydroxyl groups. This method is expensive to synthesize and is not suitable for industrialization, such as US Patent US5399733A and Chinese Patents ZL201410096997.5 and ZL201410096979 .7; the other is the reaction of monohydroxy acrylic acid with phosphorus (phosphine) chloride, because phosphorus (phosphine) chloride is cheap and widely available, it is more suitable for industrialization, such as Chinese patent ZL200910116317.0

Method used

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  • Preparation method of phosphorus and nitrogen contained acrylate and copolymer core-shell particles of phosphorus and nitrogen contained acrylate
  • Preparation method of phosphorus and nitrogen contained acrylate and copolymer core-shell particles of phosphorus and nitrogen contained acrylate
  • Preparation method of phosphorus and nitrogen contained acrylate and copolymer core-shell particles of phosphorus and nitrogen contained acrylate

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Embodiment 1

[0023] Add 19.5g (0.1mol) of phenylphosphoryl dichloride (PDCP), 25.3g (0.25mol) of triethylamine (TEA) and 80mL of solvent tetrahydrofuran (THF) into a three-necked flask equipped with a stirrer and cool down to -5 -0°C, add 11.6g (0.1mol) of hydroxyethyl acrylate (HEA) dropwise, react at 0-5°C for 3 hours, add 7.3g (0.1mol) of diethylamine (DEA) dropwise, After reacting at ℃ for 2 hours, raise the temperature to room temperature and react for 4 hours. The reaction mixture is filtered to remove triethylamine hydrochloride, and the obtained filtrate removes the solvent and unreacted triethylamine to obtain a crude product; the product is mobile with ethyl acetate. The phase was purified by neutral silica gel column chromatography, and the light yellow viscous liquid was obtained after removing ethyl acetate, which was phosphorus-nitrogen-containing acrylate.

Embodiment 2

[0025] First add 80ml of distilled water to a 250ml four-neck flask equipped with an electric stirrer, a thermometer, and a reflux condenser, then turn on the stirring device, add 0.4gNaHCO3, 2.5gSDS and 1.5gOP-10 to make it stir slowly. After it dissolves, add 0.1g KPS and start to heat up. After the temperature rises to about 60°C, add 20g of inner core monomer (a mixture of 15g of phosphorus nitrogen-containing acrylate and 10g of butyl acrylate), raise the temperature to 70-75°C, initiate polymerization, and then add dropwise The remaining 36g of inner core monomer (a mixture of 10g of phosphorus nitrogen-containing acrylate and 26g of butyl acrylate) was reacted for 2 hours, and 0.1g of KPS was added, and 21g of methyl methacrylate, a shell monomer, was added dropwise, and the reaction was continued for 3 hours. After the emulsion is demulsified, copolymer core-shell particles with particle diameters ranging from 0.05 to 0.16 microns are obtained.

Embodiment 3

[0027] First add 80ml of distilled water to a 250ml four-neck flask equipped with an electric stirrer, a thermometer, and a reflux condenser, then turn on the stirring device, add 0.4gNaHCO3, 2.5gSDS and 1.5gOP-10 to make it stir slowly. After it dissolves, add 0.1g KPS and start to heat up. After the temperature rises to about 60°C, add 20g of inner core monomer (a mixture of 16g ​​of phosphorus-nitrogen acrylate and 4g of butyl acrylate), raise the temperature to 70-75°C, initiate polymerization, and then add dropwise The remaining 30g of inner core monomer (a mixture of 24g of phosphorus-nitrogen acrylate and 6g of butyl acrylate) was reacted for 2 hours, and 0.1g of KPS was added, and 25g of methyl methacrylate, a shell monomer, was added dropwise, and the reaction was continued for 3 hours. After the emulsion is demulsified, copolymer core-shell particles with a particle size of 0.05-0.23 microns are obtained.

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Abstract

The invention discloses a preparation method of phosphorus and nitrogen contained acrylate and copolymer core-shell particles of the phosphorus and nitrogen contained acrylate. Phenylphosphonic dichloride, hydroxyethyl acrylate and diethylamine which are taken as raw materials react with trimethylamine as an acid binding agent in tetrahydrofuran at 0-5 DEG C, and phosphorus and nitrogen contained acrylate is prepared. The synthesis method is simple, and the cost is low. The phosphorus and nitrogen contained acrylate can be subjected to free-radical copolymerization with other acrylate monomers. The core-shell particles of the phosphorus and nitrogen contained acrylate are prepared with a core-shell emulsion polymerization method, the core-shell particles have the advantages of adjustable structure and composition, have certain flame retardancy on the premise that the structure of a core-shell impact modifier is not changed and are expected to be used for toughening flame retardant materials.

Description

technical field [0001] The invention relates to a preparation method of phosphorus nitrogen-containing acrylate and its copolymer core-shell particles, belonging to the technical field of polymer chemistry and polymer technology. Background technique [0002] In recent years, with the continuous improvement of awareness of environmental protection and safety protection, halogen-free flame retardants have become a hot spot in the field of flame retardant development. However, halogen-free flame retardants have disadvantages such as low flame retardant efficiency and poor mechanical properties of materials after flame retardancy. Solving the contradiction between "improving flame retardancy and maintaining mechanical properties" has become an important issue. Combining "structural modification with functional modification" is a new way to solve this problem. Acrylate copolymer particles with a core-shell structure are impact modifiers for many polymer materials, but there is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/44C08F265/04C08F275/00
CPCC07F9/4419C07F9/4438C08F265/04C08F275/00
Inventor 闫莉李青芳桑晓明刘娟
Owner NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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