Preparation method of nitrogen-containing phosphaphenanthrene derivative flame retardant

A technology of derivatives and flame retardants is applied in the field of preparation of nitrogen-containing phosphaphenanthrene derivatives flame retardants, which can solve the problems of harming workers' health, increasing product costs, polluting the environment, etc., and achieving increased production capacity and simple production process. , the effect of simple operation

Inactive Publication Date: 2016-12-14
PRESAFER QINGYUAN PHOSPHOR CHEM
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Problems solved by technology

[0005] Taiwan patent TW200811117A discloses a preparation method of DOPO-TAIC, the selected raw materials include N,N-dimethylformamide, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10- Oxide, triallyl isocyanurate and dibenzoyl peroxide, the preparation method is relatively simple, but it is limited to laboratory production, and organic solvents must be used in the preparation process, which not only pollutes the environment, but also endangers the health of workers Healthy, but also greatly increased product costs

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  • Preparation method of nitrogen-containing phosphaphenanthrene derivative flame retardant
  • Preparation method of nitrogen-containing phosphaphenanthrene derivative flame retardant

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[0023] A preparation method of a nitrogen-containing phosphaphenanthrene derivative flame retardant, comprising the following steps:

[0024] 1) Add 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide into the reaction kettle and heat to a molten state;

[0025] 2) adding triallyl isocyanurate and a catalyst, stirring and fully reacting to obtain a crude product;

[0026] 3) The crude product is washed, filtered, and dried to obtain DOPO-TAIC, which is a nitrogen-containing phosphaphenanthrene derivative flame retardant.

[0027] Preferably, the molar ratio of triallyl isocyanurate to 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is 1: (2-8).

[0028] Preferably, the catalyst is used in an amount of 0.5-5% of the mass of triallyl isocyanurate.

[0029] Preferably, the catalyst is at least one of diacetyl peroxide, methyl ethyl ketone peroxide, dibenzoyl peroxide and tert-butyl hydroperoxide.

[0030] Preferably, the reaction temperature in step 2) is 120-200° C., and th...

Embodiment 1

[0037] 1) Add 28kg of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide into a 100L stainless steel reaction kettle with a stirring paddle and a reflux device, stir to raise the temperature to 120°C, and add 10kg Triallyl isocyanurate and 0.075kg methyl ethyl ketone peroxide were reacted at a constant temperature of 120°C for 3 hours;

[0038] 2) Add 10kg of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, and react at a constant temperature of 135°C for 1 hour;

[0039] 3) Add 4.95kg of triallyl isocyanurate and react at a constant temperature of 135°C for 3 hours;

[0040] 4) Add 20kg of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, and react at a constant temperature of 150°C for 0.5 hours;

[0041] 5) Add 0.05kg of triallyl isocyanurate and react at a constant temperature of 150°C for 4 hours to obtain a crude product;

[0042] 6) Pour the crude product into 250kg of propanol after cooling, stir and wash at 60°C, and then filter, place the filtered solid filter...

Embodiment 2

[0044] 1) Add 16.5kg of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide into a 20L reaction kettle with stirring paddle and reflux device, stir to raise the temperature to 150°C, add 9.19 kg triallyl isocyanurate, 0.05kg dibenzoyl peroxide and 0.055kg tert-butyl hydroperoxide, stirred at 160°C for 1 hour;

[0045] 2) Add 0.1kg of triallyl isocyanurate, stir and react at a constant temperature of 160°C for 5 hours to obtain a crude product;

[0046] 3) Pour the crude product into 80kg of ethanol after cooling, stir and wash at 40°C, and then filter, place the filtered solid filter residue in an oven at 80°C to dry to obtain the target product DOPO-TAIC, and the yield of DOPO-TAIC is 86.1 %, the purity of DOPO-TAIC is higher than 95%. The infrared spectrum of the DOPO-TAIC prepared in this embodiment is as follows: figure 1 As shown, the thermogravimetric spectrum is shown as figure 2 shown.

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Abstract

The invention discloses a preparation method of nitrogen-containing phosphaphenanthrene derivative flame retardant. The preparation method includes the following steps that 1, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is added to a reaction kettle, and heating is performed to reach a molten state; 2, triallylisocyanurate and a catalyst are added, full stirring reaction is performed to obtain a coarse product; 3, the coarse product is subjected to washing, filtering and drying to obtain DOPO-TAIC, namely the nitrogen-containing phosphaphenanthrene derivative flame retardant is obtained. The preparation method adopts a melting method to prepare the nitrogen-containing phosphaphenanthrene derivative flame retardant, a reaction principle of the method is consistent to a solvent method, the adopted DOPO is a raw material and is also a solvent in the reaction process, the complicated solvent removing process in the solvent method is omitted, the yields of the same volume of reaction kettles within unit time are greatly increased, the production cost is effectively reduced, harmful organic solvents are not needed, an operation method and production processes are simple, and the method is beneficial to industrialized enlarged production.

Description

technical field [0001] The invention relates to a preparation method of a nitrogen-containing phosphaphenanthrene derivative flame retardant. Background technique [0002] In recent years, the application of polymer materials has become more and more extensive, which is closely related to people's life. However, due to the low ignition point of polymer materials, there are serious fire hazards. Therefore, improving the flame retardancy of polymer materials has become the most concerned issue. At present, the method of improving the flame retardancy of polymer materials is mainly realized by adding flame retardants, but the polymer materials added with traditional halogen flame retardants have disadvantages such as large amount of smoke and toxic gas when burned. Therefore, there is an urgent need to develop a new type of environmentally friendly halogen-free flame retardant. [0003] DOPO derivatives have a hard chemical structure of double benzene rings. Adding them as fl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
CPCC07F9/657172
Inventor 罗海荣陈志钊周侃
Owner PRESAFER QINGYUAN PHOSPHOR CHEM
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