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Preparation method of oligomeric phosphonate flame retardant

The technology of polyphosphonate and flame retardant is applied in the field of preparation of oligomeric phosphonate flame retardant, which can solve the problems of containing alkali metal ions and high organic tin acid value, and achieve excellent thermal stability and flame retardant performance. Excellent, avoid core burning effect

Inactive Publication Date: 2020-07-03
青岛长荣化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The purpose of the present invention is to overcome the problems that existing oligophosphonate products contain alkali metal ions, organic tin and high acid value, and provide a method for preparing oligophosphonate

Method used

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  • Preparation method of oligomeric phosphonate flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Add 114g of tetraethyl titanate and 106g of diethylene glycol into a reactor equipped with a thermometer, a magnetic stirrer and a distillation device, start stirring, heat in an oil bath, and gradually increase the temperature, at 70-96°C, 0.03-0.08MPa vacuum Under the condition of 3h, 90g of ethanol was evaporated while reacting, and the residue was cooled to obtain 130g of bis(diethylene glycol) titanate. The appearance was a colorless transparent viscous liquid, and 130g of dimethyl methylphosphonate Dilute and mix to obtain 260 g of 50% bis(diethylene glycol) titanate solution, code-named TDEG, for use in the following experiments.

[0044] In a 500mL reactor equipped with a thermometer, a stirrer and a vacuum distillation device, add 372g of dimethyl methylphosphonate, 106g of diethylene glycol and 10g of TDEG, stir, heat, and under nitrogen protection, gradually increase the temperature and gradually reduce the vacuum Control the reaction temperature at 120-180°C...

Embodiment 2

[0046] In a 500mL reactor equipped with a thermometer, a stirrer and a vacuum distillation device, add 372g of dimethyl methylphosphonate, 106g of diethylene glycol and 10g of TDEG, stir, heat, and under nitrogen protection, gradually increase the temperature and gradually reduce the vacuum Control the reaction temperature at 120-180°C, vacuum degree 0-0.06MPa, and distill the by-product methanol while reacting within 6 hours. After the exchange reaction was completed, 57.6 g of methanol was recovered. Keep the temperature at 180°C, gradually increase the degree of vacuum to above 0.095MPa, and distill off excess dimethyl methylphosphonate under reduced pressure. When the rate of distillate is obviously slow, stop vacuuming, continue to pass nitrogen to restore normal pressure, and recover 126.6 g of dimethyl methylphosphonate were used to obtain 303.8 g of a crude product with an acid value of 12.6 mgKOH / g. Cool the crude product to 115°C, add 15g of 1,4-butanediol diglycidy...

Embodiment 3

[0048] In a 500mL reactor equipped with a thermometer, a stirrer and a vacuum distillation device, add 372g of dimethyl methylphosphonate, 106g of diethylene glycol and 14.3g of TDEG, stir, heat, and gradually raise the temperature and gradually lower the temperature under the protection of nitrogen. Vacuum degree, control the reaction temperature at 120-180°C, vacuum degree 0-0.06MPa, and distill the by-product methanol within 5h while reacting. After the transesterification reaction was completed, 60.8 g of methanol was recovered. Keep the temperature at 180°C, gradually increase the degree of vacuum to above 0.095MPa, and distill off excess dimethyl methylphosphonate under reduced pressure. When the rate of distillate is obviously slow, stop vacuuming, continue to pass nitrogen to restore normal pressure, and recover 133.6 g of dimethyl methylphosphonate were used to obtain 298.6 g of a crude product with an acid value of 8.6 mgKOH / g. Cool the crude product to 115°C, add 7...

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Abstract

The invention discloses a preparation method of an oligomeric phosphonate flame retardant, and relates to the technical field of preparation of organophosphorus flame retardants. According to the method, excessive phosphonate and a polyhydric alcohol are used as raw materials, the feeding molar ratio of the two is (2-4):1, chelating titanate is selected as a catalyst with the dosage being 0.1-2% of the total mass of the raw materials, process parameters such as proper temperature, vacuum degree, time and the like are controlled, and ester exchange, reduced pressure distillation and epoxide deacidification agent treatment are carried out to obtain the oligomeric phosphonate flame retardant product. The method is easy in raw material source, low in cost, high in catalyst efficiency, free ofthree-waste emission, environment-friendly in process and suitable for industrial production; and the oligomeric phosphonate product prepared by the method has the advantages of low volatility, favorable compatibility with high polymer materials and excellent and durable flame retardancy, and is especially suitable for flame-retardant polyurethane.

Description

technical field [0001] The invention relates to a preparation method of an oligomeric phosphonate flame retardant, and belongs to the technical field of organic phosphorus flame retardant synthesis. Background technique [0002] Flame retardants are functional additives that endow flammable materials with flame retardancy, which can prevent or delay the occurrence of fires and gain time for rescue and escape. [0003] Among all flame retardants, phosphorus-based flame retardants have the highest efficiency, especially flame-retardant polymer materials containing oxygen and nitrogen elements, such as polyurethane, polyester, polycarbonate, nylon, epoxy resin, unsaturated resin, polyester, etc. Methacrylate, etc. [0004] Phosphorous flame retardants include inorganic phosphorus flame retardants and organic phosphorus flame retardants. Inorganic phosphorus flame retardants include red phosphorus, phosphate, polyphosphate, etc. Although the phosphorus content is large and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04C07F9/40C08L75/04C08L85/02C08K5/5333B01J31/12
CPCB01J31/122C07F9/40C08G79/04C08K5/5333C08L75/04C08L2201/02C08L2203/14C08L85/02
Inventor 韩忠山韩明序杨松慧
Owner 青岛长荣化工科技有限公司
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