Method for preparing flame-retardant polymer containing pyridine groups

Abstract

The invention discloses a method for preparing a flame-retardant polymer containing pyridine groups. The method comprises the following steps of (1) adding styrene, acrylonitrile, 2-vinyl pyridine, dibromostyrene and an emulsifier into a dispersant and stirring to obtain an emulsion; (2) adding an initiator and a chain transfer agent into the emulsion and reacting, wherein a reaction mixture is obtained after the reaction is completed; (3) adding a demulsifying agent into the reaction mixture, fully stirring and carrying out solid-liquid separation to obtain a solid product which is a crude product, and (4) sequentially washing the solid product with water and methanol, and after the washing is completed, drying to obtain the finished product. The product prepared by the method has the advantages of good flame-retardant property, good thermodynamic stability and strong surface adhesion force and has a wide range of application.

Description

technical field

[0001] The invention relates to a preparation method of a pyridine group-containing flame-retardant polymer. Background technique

[0002] Styrene acrylonitrile polymer (also known as SAN or AS), as a kind of engineering plastic with good chemical stability, is widely used in the preparation of various plastic containers, such as lighter casings, cosmetic containers, ballpoint pen holders, etc. In recent years, with the continuous improvement of people's requirements for material performance, the flame retardant performance of engineering plastics has received more and more attention. How to make conventional materials have flame retardant performance is the main research direction of researchers in the field of flame retardant material preparation. Bromine series flame retardants are currently widely used. In order to make styrene acrylonitrile polymers have flame retardant properties, a method currently used is: introduce bromine element on the phenyl group...

Examples

Embodiment 1

[0022] (1) Add 10.6g of styrene, 5.3g of acrylonitrile, 10.6g of 2-vinylpyridine, 10.6g of dibromostyrene, 1.9g of sodium dodecyl sulfate and 111.3g of water into a 500ml four-neck flask, Under the temperature condition of 70°C, stir for 30 minutes to obtain an emulsion;

[0023] (2) Add 0.8g of potassium persulfate and 0.8g of tert-dodecylmercaptan to the above emulsion, raise the temperature to 80-85°C, and react for 5 hours to prepare a reaction mixture;

[0024] (3) Add 0.8g sodium chloride to the above reaction mixture and stir for 10 minutes, then carry out suction filtration, and the solid product obtained after suction filtration is a crude product;

[0025] (4) Wash the above crude product with water first, then with methanol, put it in a vacuum drying oven after washing, and dry it for 2 hours at a pressure of -0.095mpa and a temperature of 30°C-40°C to obtain 35.8g of white particles The product is a flame-retardant polymer containing pyridine groups.

Embodiment 2

[0027] (1) Add 10.6g of styrene, 5.3g of acrylonitrile, 10.6g of 2-vinylpyridine, 13.1g of dibromostyrene, 3.1g of sodium dodecyl sulfate and 160g of water into a 500ml four-necked flask. Under the temperature condition of 70°C, stir for 30 minutes to obtain an emulsion;

[0028] (2) Add 1.1 g of potassium persulfate and 1.9 g of tert-dodecylmercaptan to the above emulsion, raise the temperature to 80-85°C, and react for 5.5 hours to prepare a reaction mixture;

[0029] (3) Add 1.5g sodium chloride to the above reaction mixture and stir for 10 minutes, then carry out suction filtration, and the solid product obtained after suction filtration is a crude product;

[0030] (4) Wash the above crude product with water first, then with methanol, put it in a vacuum drying oven after washing, and dry it for 2 hours at a pressure of -0.095mpa and a temperature of 30°C-40°C to obtain 38.6g of light yellow A granular product, the product is a pyridine group-containing flame-retardant po...

Embodiment 3

[0032] (1) Add 10.6g styrene, 5.3g acrylonitrile, 10.6g 2-vinylpyridine, 13.1g dibromostyrene, 3.1g sodium dodecylbenzenesulfonate, 160g water and 20g methanol into a 500ml four-necked flask , under the temperature condition of 65-70°C, stirring for 30 minutes to obtain an emulsion;

[0033] (2) Add 1.1 g of potassium persulfate and 1.9 g of tert-dodecylmercaptan to the above emulsion, raise the temperature to 80-85°C, and react for 5.5 hours to prepare a reaction mixture;

[0034] (3) Add 1.2g sodium chloride to the above reaction mixture and stir for 10 minutes, then carry out suction filtration, and the solid product obtained after suction filtration is a crude product;

[0035] (4) Wash the above crude product first with water and then with methanol, put it in a vacuum drying oven after washing, and dry it for 2 hours at a pressure of -0.095mpa and a temperature of 30°C-40°C to obtain 38.9g of light yellow A granular product, the product is a pyridine group-containing fla...

technical field

[0001] The invention relates to a preparation method of a pyridine group-containing flame-retardant polymer. Background technique

[0002] Styrene acrylonitrile polymer (also known as SAN or AS), as a kind of engineering plastic with good chemical stability, is widely used in the preparation of various plastic containers, such as lighter casings, cosmetic containers, ballpoint pen holders, etc. In recent years, with the continuous improvement of people's requirements for material performance, the flame retardant performance of engineering plastics has received more and more attention. How to make conventional materials have flame retardant performance is the main research direction of researchers in the field of flame retardant material preparation. Bromine series flame retardants are currently widely used. In order to make styrene acrylonitrile polymers have flame retardant properties, a method currently used is: introduce bromine element on the phenyl group...

Examples

Embodiment 1

[0022] (1) Add 10.6g of styrene, 5.3g of acrylonitrile, 10.6g of 2-vinylpyridine, 10.6g of dibromostyrene, 1.9g of sodium dodecyl sulfate and 111.3g of water into a 500ml four-neck flask, Under the temperature condition of 70°C, stir for 30 minutes to obtain an emulsion;

[0023] (2) Add 0.8g of potassium persulfate and 0.8g of tert-dodecylmercaptan to the above emulsion, raise the temperature to 80-85°C, and react for 5 hours to prepare a reaction mixture;

[0024] (3) Add 0.8g sodium chloride to the above reaction mixture and stir for 10 minutes, then carry out suction filtration, and the solid product obtained after suction filtration is a crude product;

[0025] (4) Wash the above crude product with water first, then with methanol, put it in a vacuum drying oven after washing, and dry it for 2 hours at a pressure of -0.095mpa and a temperature of 30°C-40°C to obtain 35.8g of white particles The product is a flame-retardant polymer containing pyridine groups.

Embodiment 2

[0027] (1) Add 10.6g of styrene, 5.3g of acrylonitrile, 10.6g of 2-vinylpyridine, 13.1g of dibromostyrene, 3.1g of sodium dodecyl sulfate and 160g of water into a 500ml four-necked flask. Under the temperature condition of 70°C, stir for 30 minutes to obtain an emulsion;

[0028] (2) Add 1.1 g of potassium persulfate and 1.9 g of tert-dodecylmercaptan to the above emulsion, raise the temperature to 80-85°C, and react for 5.5 hours to prepare a reaction mixture;

[0029] (3) Add 1.5g sodium chloride to the above reaction mixture and stir for 10 minutes, then carry out suction filtration, and the solid product obtained after suction filtration is a crude product;

[0030] (4) Wash the above crude product with water first, then with methanol, put it in a vacuum drying oven after washing, and dry it for 2 hours at a pressure of -0.095mpa and a temperature of 30°C-40°C to obtain 38.6g of light yellow A granular product, the product is a pyridine group-containing flame-retardant po...

Embodiment 3

[0032] (1) Add 10.6g styrene, 5.3g acrylonitrile, 10.6g 2-vinylpyridine, 13.1g dibromostyrene, 3.1g sodium dodecylbenzenesulfonate, 160g water and 20g methanol into a 500ml four-necked flask , under the temperature condition of 65-70°C, stirring for 30 minutes to obtain an emulsion;

[0033] (2) Add 1.1 g of potassium persulfate and 1.9 g of tert-dodecylmercaptan to the above emulsion, raise the temperature to 80-85°C, and react for 5.5 hours to prepare a reaction mixture;

[0034] (3) Add 1.2g sodium chloride to the above reaction mixture and stir for 10 minutes, then carry out suction filtration, and the solid product obtained after suction filtration is a crude product;

[0035] (4) Wash the above crude product first with water and then with methanol, put it in a vacuum drying oven after washing, and dry it for 2 hours at a pressure of -0.095mpa and a temperature of 30°C-40°C to obtain 38.9g of light yellow A granular product, the product is a pyridine group-containing fla...

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