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Method for preparing flame-retardant polymer polyol, application of flame-retardant polymer polyol, and polyurethane foam plastic prepared from flame-retardant polymer polyol

A technology of flame-retardant polymers and polyether polyols, applied in the field of polyurethane synthetic materials, can solve the problems of high-temperature release of toxic gases containing halogens and poor flame-retardant performance, and achieve good synergistic effects, low smoke generation, and strong applicability Effect

Active Publication Date: 2021-01-22
WANHUA CHEM GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to overcome the defects of poor flame retardancy of existing flame retardant polymer polyols and the release of toxic gases at high temperatures containing halogens, and to provide a method for preparing flame retardant polymer polyols with phosphoramide. Flame retardant polymer polyol contains phosphorus and nitrogen two kinds of flame retardant elements at the same time, high flame retardant performance, low smoke generation, good fluidity, good storage stability

Method used

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  • Method for preparing flame-retardant polymer polyol, application of flame-retardant polymer polyol, and polyurethane foam plastic prepared from flame-retardant polymer polyol
  • Method for preparing flame-retardant polymer polyol, application of flame-retardant polymer polyol, and polyurethane foam plastic prepared from flame-retardant polymer polyol
  • Method for preparing flame-retardant polymer polyol, application of flame-retardant polymer polyol, and polyurethane foam plastic prepared from flame-retardant polymer polyol

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preparation example Construction

[0031]1) Preparation of phosphoramide: in an inert atmosphere, dissolve phosphoryl dichloride in an organic solvent, add organic diamine dissolved in the organic solvent to the above solution drop by drop, at -30°C to 20°C React at low temperature for 1-6 hours, then raise the temperature to 30-100°C for 0.5-6 hours; then add an acid-binding agent, react at 30-100°C for 1-6 hours, and then filter to obtain a colorless and transparent solution.

[0032] 2) Polymerization reaction: Add formaldehyde solution to the phosphoramide solution obtained in step 1), heat to 60-80°C, and react for 0.5-2 hours; mix the obtained solution with polyether polyol, heat to 80-100°C, and react for 1 ~3h; under the conditions of pressure of -0.098MPa~-0.08MPa and temperature of 90~120°C, vacuumize to remove residual monomers to obtain flame retardant polymer polyol.

[0033] In another embodiment of the present invention, a kind of method that prepares flame-retardant polymer polyol with phosphora...

Embodiment 1

[0066] (1) In a nitrogen atmosphere, 111g of phenylphosphoryl dichloride was dissolved in 223g of tetrahydrofuran, 0.2g of sodium iodide was added, and then 86g of ethylenediamine dissolved in 172g of tetrahydrofuran was added dropwise to the above solution, React at -5°C for 3 hours, then raise the temperature to 50°C for 3 hours; then add 121 g of solid sodium carbonate, react at 50°C for 3 hours, and filter to obtain a colorless and transparent solution.

[0067] (2) Add 65g of 37% formaldehyde solution into the phenylphosphoric diethylenediamine solution obtained in step (1), heat to 80°C, and react for 0.5h; mix the resulting solution with 350g of polyether polyol 1, heat To 100°C, react for 1h; vacuumize and remove residual monomers at a pressure of -0.098MPa~-0.08MPa and a temperature of 100°C to obtain a flame retardant with a viscosity of 3176mP·s / 25°C and a solid content of 30%. Polymer polyol, product phosphorus content 3.6%, nitrogen content 6.4%.

Embodiment 2

[0069] (1) In a nitrogen atmosphere, dissolve 80g of methylphosphoryl dichloride in 199g of dioxane, add 0.36g of sodium iodide, then dissolve 101g of propylenediamine in 252g of dioxane dropwise Add it to the above solution, react at 0°C for 2 hours, then raise the temperature to 40°C for 3 hours; then add 152g of sodium carbonate solid, react at 40°C for 3 hours, and filter to obtain a colorless and transparent solution.

[0070] (2) 66g of 37% formaldehyde solution is added to the obtained methylphosphoryldipropylenediamine solution of step (1), heated to 60°C, and reacted for 2h; the resulting solution is mixed with 350g of polyether polyol 2, heated to 90°C, react for 2h; vacuumize to remove residual monomers under the pressure of -0.098MPa~-0.08MPa and temperature of 110°C, and obtain a flame-retardant polymer with a viscosity of 2886mP·s / 25°C and a solid content of 30%. Polyol, product phosphorus content 4.2%, nitrogen content 7.6%.

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Abstract

The invention relates to a method for preparing flame-retardant polymer polyol from phosphamide. The method mainly comprises the following steps: a, reacting phosphoryl dichloride with organic diaminein a nitrogen atmosphere, adding an acid-binding agent, reacting at 60 DEG C for 2 hours, and filtering to obtain a colorless transparent solution; and b, adding a formaldehyde solution into the phosphamide solution obtained in the step a, heating to react for a period of time, mixing the obtained solution with polyether polyol, heating to react completely, and vacuumizing to remove residual monomers to obtain the flame-retardant polymer polyol with the nitrogen content of 6-9% and the phosphorus content of 3-5% in terms of the weight of the polymer polyol. The polyurethane foam plastic prepared from the flame-retardant polymer polyol has a foaming foam oxygen index of about 30%, good flame retardancy and low smoke generation amount.

Description

technical field [0001] The invention belongs to the field of polyurethane synthetic materials, and in particular relates to a method for preparing flame-retardant polymer polyol by using phosphoramide. Background technique [0002] Polyurethane materials have the advantages of chemical corrosion resistance, weather resistance, and excellent mechanical processing performance. They are widely used in clothing, shoes and hats, building exterior walls, pipelines, aerospace, furniture, automobiles, medical care and other fields. However, ordinary polyurethane materials have a low oxygen index, are easy to burn, and release a large amount of toxic smoke when burning, which has brought great harm to people's life and property safety. Polyether polyol is one of the main raw materials of polyurethane. If polyether polyol contains flame retardant elements, the flame retardant performance of polyurethane materials can be effectively improved. At present, flame retardant polyether poly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/335C08G18/50C08G101/00
CPCC08G65/3356C08G18/509
Inventor 姜明刘洋李传亮秦承群隋美玉李付国
Owner WANHUA CHEM GRP CO LTD
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