Preparation method for polyphosphoester fire retardant with dual-DOPO as branch chain

A technology of polyphosphate ester and flame retardant, which is applied in the field of preparation of polyphosphate ester flame retardant, can solve the problems such as steric hindrance, inability to obtain polyphosphoric acid flame retardant with high degree of polymerization, poor matrix compatibility, and high volatility. To achieve the effect of easy control of reaction conditions, good compatibility, and difficult migration

Active Publication Date: 2017-06-13
BEIJING INSTITUTE OF TECHNOLOGYGY
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Problems solved by technology

[0007] The purpose of the present invention is to solve the disadvantages of poor heat resistance, high volatility, easy migration and poor matrix compatibility of commonly used small molecule phosphate flame retardants, and to overcome the disadvantages of flame retardants in the conventional polymerization process. In view of the difficulty of obtaining polyphosphoric acid flame retardants with

Method used

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  • Preparation method for polyphosphoester fire retardant with dual-DOPO as branch chain
  • Preparation method for polyphosphoester fire retardant with dual-DOPO as branch chain
  • Preparation method for polyphosphoester fire retardant with dual-DOPO as branch chain

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Experimental program
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Example Embodiment

[0038] Example 1:

[0039] (1) Synthesis of polymeric intermediate P-PDCP

[0040] Measure 21.40g (0.10mol) of 4,4'-dihydroxybenzophenone, 19.50g (0.10mol) of phenylphosphoryl dichloride and 300mL of anhydrous acetonitrile, and add them to the In the 500mL reaction vessel with protective gas inlet and outlet, under the condition of feeding nitrogen, pre-react at 70°C for 2h, then raise the temperature to 80°C, and react until there is no HCl gas (reaction ends). The obtained precipitate was suction filtered while it was hot, washed several times with anhydrous acetonitrile, and dried in a vacuum oven at 80°C for 2 hours to obtain 29.8 g of a light yellow solid product with a yield of 88.6%.

[0041] The polymeric intermediate prepared above was subjected to infrared testing. The machine model used was a Bruker Tensor 27 Fourier transform infrared spectrometer. Potassium bromide was pressed into tablets for sample preparation, and the scanning range was 4000-500cm -1 . Analy...

Example Embodiment

[0051] Example 2:

[0052] (1) Synthesis of polymeric intermediate P-PPDC

[0053] The synthesis steps of the polymeric intermediate P-PPDC are carried out according to the synthesis steps of P-PDCP in Example 1, except that 0.10 mol of phenylphosphoryl dichloride (PDCP) in Example 1 is replaced by 0.10 mol of dichloride Phenyl phosphate (PPDC). After purification and drying, a yellow solid product was obtained with a yield of 90.6%.

[0054] According to the infrared test method in Example 1, the intermediate P-PPDC is tested, and the infrared spectrum obtained by the test is analyzed. In the infrared spectrum of the intermediate P-PPDC, O-H in 4,4'-dihydroxybenzophenone is in The strong and broad characteristic peaks at 3250-3350cm-1 and the sharp characteristic peaks of the P-Cl bond at 541-583cm-1 in phenyl phosphate dichloride (PPDC) disappear, corresponding to 929cm-1 and 1189cm-1 The characteristic peak of P-O-Ph appeared. It can be known that 4,4'-dihydroxybenzophe...

Example Embodiment

[0059] Example 3:

[0060] (1) Synthesis of polymeric intermediate P-SPDPC

[0061] The synthesis steps of polymeric intermediate P-SPDPC are carried out according to the synthesis steps of P-PDCP in Example 1, except that 0.10mol of phenylphosphoryl dichloride (PDCP) in Example 1 is replaced by 0.10mol of pentaerythritol diphosphate Ester diphosphoryl chloride (SPDPC). After purification and drying, a yellow solid product was obtained with a yield of 78.9%.

[0062] According to the infrared test method in Example 1, the intermediate P-SPDPC is tested, and the infrared spectrum obtained by the test is analyzed. In the infrared spectrum of the intermediate P-SPDPC, O-H in 4,4'-dihydroxybenzophenone is in The strong and broad characteristic peak at 3250-3350cm-1 and the sharp characteristic peak of the P-Cl bond in pentaerythritol diphosphate diphosphoryl chloride (SPDPC) at 541-583cm-1 disappeared, and the positions at 929cm-1 and 1189cm-1 The corresponding characteristic p...

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Abstract

The invention belongs to the technical field of a phosphorus-containing fire retardant and specifically relates to a preparation method for a polyphosphoester fire retardant with dual-DOPO as a branch chain. The method comprises the following steps: under the protection of inert gases, reacting 4,4'-dyhydroxyl benzophenone with phenyldichlorophosphate, phenyl dichlorophosphate or pentaerythritol diphosphate diphosphoryl chloride in an anhydrous acetonitrile solvent till no halogen hydride gas is emitted, thereby acquiring a polymerized fire retardant midbody; performing heating for reaction on the midbody, initiator and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide at the temperature of 130-160 DEG C; and performing melt grafting reaction, reducing the reaction temperature to 50-70 DEG C, adding ethyl alcohol, stirring and flowing back, performing suction filtration and drying, thereby acquiring the fire retardant. According to the invention, the difficulty of the traditional process that a highly polymerized fire retardant cannot be acquired under the effect of larger steric hindrance in the process of polymerizing after compounding micro-molecule midbody can be overcome; the compounded fire retardant has higher molecular weight and narrower molecular weight distribution; and the compounded fire retardant has excellent compatibility with substance, is difficult to migrate and has excellent durability.

Description

technical field [0001] The invention belongs to the technical field of phosphorus-containing flame retardants, and in particular relates to a preparation method of a polyphosphate flame retardant whose branch chain is double DOPO. Background technique [0002] The non-halogenation of flame retardants is the general trend of the development of flame retardants at present. As an important branch of flame retardants, phosphorus-based flame retardants can exert flame retardant effects in both condensed phase and gas phase, and have low smoke and low toxicity. As well as the advantages of environmental protection and high efficiency, it has been extensively studied by many scholars at home and abroad. [0003] Phosphorus-based flame retardants are mainly used in phosphoric acid esters, such as resorcinol bis(diphenyl phosphate) (RDP), bisphenol A bis(diphenyl phosphate) (BDP) and triphenyl phosphate (TPP), etc. Most of these commonly used phosphate flame retardants are liquid an...

Claims

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Application Information

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IPC IPC(8): C08G65/48C08G65/40C08L63/00C08L71/10
CPCC08G65/4006C08G65/48C08L63/00C08L2201/02C08L71/10
Inventor 王银杰李树磊
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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