Preparation method of monohydroxy dialkyl phosphinic acid metal salt fire retardant

A technology of monohydroxydialkylphosphinic acid and monohydroxyalkylphosphinic acid, which is applied in the field of preparation of monohydroxydialkylphosphinic acid metal salt flame retardants, to improve safety, novel synthesis route, and simplify production The effect of equipment

Inactive Publication Date: 2013-12-11
PRESAFER QINGYUAN PHOSPHOR CHEM
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  • Abstract
  • Description
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  • Preparation method of monohydroxy dialkyl phosphinic acid metal salt fire retardant
  • Preparation method of monohydroxy dialkyl phosphinic acid metal salt fire retardant
  • Preparation method of monohydroxy dialkyl phosphinic acid metal salt fire retardant

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[0022] A preparation method of monohydroxy dialkylphosphinic acid metal salt flame retardant, comprising the following steps:

[0023] 1) Reaction of alkyl phosphine dichloride with alcohol to obtain mono-alkyl phosphonate;

[0024] 2) In the presence of acid and water, react the monoalkylphosphonate obtained in the previous step with aldehyde to obtain a monohydroxyalkylphosphinate solution;

[0025] 3) React the monohydroxyalkyl hypophosphite solution obtained in the previous step with Lewis acid in water to form a solid monohydroxydialkylphosphinate metal salt flame retardant, which can be separated, washed and dried.

[0026] In step 1), the alkyl phosphine dichloride is methyl phosphine dichloride, ethyl phosphine dichloride, propyl phosphine dichloride, phenyl phosphine dichloride, isopropyl phosphine dichloride , One of cyclohexylphosphine dichloride.

[0027] In step 1), the alcohol is one of methanol, ethanol, propanol, isopropanol, butanol, isobutanol, octanol, iso...

Embodiment 1

[0045] 1) Synthesis of monoethyl methylphosphite: Dissolve 1.0mol of ethanol and 0.5mol of N,N-xylaniline in 5-6 times the volume of n-hexane at 0-5°C (n-hexane The volume is 5-6 times the total volume of ethanol and N, N-xylidine), under stirring, add 0.5 mol of dichloromethyl phosphine dropwise, keep stirring at this temperature for 1.5 hours, rise to 20-25°C and continue Stir for 1.5 hours, then reflux for 1.5 hours. Cool to room temperature, filter, wash the filter cake with acetone, and use the filtrate in the next step after removing the solvent.

[0046] 2) Add 100ml of deionized water, 45ml of 36wt% hydrochloric acid and 15g of paraformaldehyde to the solvent-free filtrate in 1), stir and heat to 60°C for 15 hours to obtain 195g of monohydroxymethyl hypophosphorous acid solution, liquid phase Chromatographic analysis contained 25.6% of monohydroxymethyl hypophosphorous acid (molecular weight M=110), and the yield was 90%.

[0047] 3) Maintain the temperature at 60°C ...

Embodiment 2

[0050]1) Dissolve 1.0mol of propanol and 0.5mol of N,N-xylidine in 5-6 times the volume of n-hexane at 0-5°C, and add 0.5mol of dichloromethyl dropwise under rapid stirring Phosphine, keep stirring at this temperature for 1.0 hour, rise to 20-25°C and continue stirring for 1.5 hours, then reflux for 2 hours. Cool to room temperature, filter, wash the filter cake with acetone, and use the filtrate in the next step after removing the solvent.

[0051] 2) Add 100ml of deionized water, 45ml of 36wt% hydrochloric acid and 15g of paraformaldehyde to the solvent-free filtrate in 1), stir and heat to 65°C for 13 hours to obtain 201g of monohydroxymethyl hypophosphorous acid solution, liquid phase Chromatographic analysis contained 25.4% of monohydroxymethylphosphorous acid (M=110), yield 92%.

[0052] 3) Maintain the temperature at 65°C and add an aqueous solution prepared by adding 21g of aluminum chloride and 50ml of deionized water to the monohydroxymethyl hypophosphorous acid sol...

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Abstract

The invention discloses a preparation method of a monohydroxy dialkyl phosphinic acid metal salt fire retardant. The preparation method comprises the following steps: 1) performing reaction on alkyl phosphonium dichloride and alcohol to obtain monoalkyl phosphonate; 2) in the presence of acid and water, performing reaction on monoalkyl phosphonate obtained from the former step and aldehyde to obtain monohydroxy alkyl phosphinic acid solution; 3) performing reaction on monohydroxy alkyl phosphinic acid solution obtained from the former step and lewis acid in water, generating the monohydroxy dialkyl phosphinic acid metal salt fire retardant solid, separating out solid, washing and drying the solid to obtain the product. According to the preparation method, monosubstituted phosphonium dichloride is taken as a starting material, so that the synthetic route is novel. The risk of using gaseous state raw material such as olefin is avoided. According to the invention, the reaction conditions are mild (normal pressure, and temperature not higher than 100 DEG C); the synthetic steps are few; separate purification is needless; the technology is simple; the production equipment is simplified; the safety of the production process is improved.

Description

technical field [0001] The invention relates to a preparation method of a monohydroxy dialkyl phosphinic acid metal salt flame retardant. Background technique [0002] Halogen-free flame retardants are currently one of the main development directions of flame retardants. Intumescent flame retardant systems, inorganic flame retardants such as phosphorus, nitrogen, silicon and metal hydroxides, and different halogen-free flame-retardant compound systems together constitute a huge family of halogen-free flame retardants. However, halogen-free flame retardants generally have the problem of high addition amount and great influence on mechanical properties. In addition, it is necessary to develop different compound flame retardant systems according to different polymer matrices in order to obtain the optimal combination of flame retardant and mechanical properties. [0003] Phosphinate flame retardant products have low density, small amount of flame retardant, and high CTI value...

Claims

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Application Information

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IPC IPC(8): C07F9/30
Inventor 朱红芳周侃
Owner PRESAFER QINGYUAN PHOSPHOR CHEM
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