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A kind of method for preparing flame retardant polymer polyol, application and polyurethane foam made by the same

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

Active Publication Date: 2022-07-12
WANHUA CHEM GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of method for preparing flame retardant polymer polyol, application and polyurethane foam made by the same
  • A kind of method for preparing flame retardant polymer polyol, application and polyurethane foam made by the same
  • A kind of method for preparing flame retardant polymer polyol, application and polyurethane foam made by the same

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preparation example Construction

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

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

[0033] In another embodiment of the present invention, a method for preparing flame retardant polymer polyol with phosphoramide, comprising t...

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, The reaction was carried out at -5 °C for 3 h, then heated to 50 °C for 3 h; then 121 g of solid sodium carbonate was added, and the solution was filtered at 50 °C for 3 h to obtain a colorless and transparent solution.

[0067] (2) 65g of 37% aqueous formaldehyde solution was added to the phenylphosphoryl diethylenediamine solution obtained in step (1), heated to 80°C, and reacted for 0.5h; the obtained solution was mixed with 350g of polyether polyol 1, heated To 100℃, react for 1h; under the conditions of pressure of -0.098MPa~-0.08MPa and temperature of 100℃, vacuuming to remove residual monomers, a flame retardant with a viscosity of 3176mP·s / 25℃ and a solid content of 30% is obtained Polymer polyol, product phosphoru...

Embodiment 2

[0069] (1) In a nitrogen atmosphere, 80g of methylphosphoryl dichloride was dissolved in 199g of dioxane, 0.36g of sodium iodide was added, and then 101g of propylenediamine dissolved in 252g of dioxane was added dropwise to It was added to the above solution, reacted at 0 °C for 2 h, then heated to 40 °C for 3 h; then added 152 g of solid sodium carbonate, reacted at 40 °C for 3 h, and filtered to obtain a colorless and transparent solution.

[0070] (2) 66g of 37% aqueous formaldehyde solution was added to the methylphosphoryldipropylenediamine solution obtained in step (1), heated to 60° C., and reacted for 2h; the obtained solution was mixed with 350g of polyether polyol 2, and heated to 90℃, reaction for 2h; under the conditions of pressure of -0.098MPa~-0.08MPa and temperature of 110℃, vacuum was used to remove residual monomers, and a flame retardant polymer with viscosity of 2886mP·s / 25℃ and 30% solid content was obtained Polyol, the product has a phosphorus content of 4...

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Abstract

The invention relates to a method for preparing a flame retardant polymer polyol by using phosphoramide, which mainly comprises the following steps: a. in a nitrogen atmosphere, react phosphoryl dichloride with an organic diamine, then add an acid binding agent, and at 60 ℃ After reaction at °C for 2 h, a colorless and transparent solution was obtained by filtration. b. The formaldehyde solution is added to the phosphoramide solution obtained in step a, and the reaction is heated for a period of time; the obtained solution is mixed with polyether polyol, and the residual monomer is removed by vacuuming after the heating reaction is completed to obtain a flame retardant polymer polyol, Based on the weight of the polymer polyol, the nitrogen content is 6-9%, and the phosphorus content is 3-5%. The polyurethane foam plastic made of the flame retardant polymer polyol has the foamed foam oxygen index of about 30 percent, good flame retardant performance and low smoke generation.

Description

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

Claims

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Application Information

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Patent Type & Authority Patents(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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