Phosphorus-based flame-retardant block polyether, preparation method thereof and application of phosphorus-based flame-retardant block polyether to rigid polyurethane foam

A technology of rigid polyurethane and flame-retardant polyether, which is applied in the field of flame-retardant polyurethane foam materials, can solve the problems of rigid polyurethane foam, poor dimensional stability, and low flame-retardant efficiency, and achieve excellent flame-retardant and mechanical properties, Good dimensional stability and high flame retardant efficiency

Inactive Publication Date: 2018-07-31
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the application process, it was found that when powder additive flame retardants such as ammonium polyphosphate were used, there were problems of poor dispersion, low flame retardant efficiency, and large addition amount; while liquid flame retardants such as organic phosphates were used When used as a flame retardant, there are problems such as small molecular weight of the flame retardant, easy migration from the matrix, easy shrinkage of the foam, and poor dimensional stability, which have an impact on the application of rigid polyurethane foam

Method used

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  • Phosphorus-based flame-retardant block polyether, preparation method thereof and application of phosphorus-based flame-retardant block polyether to rigid polyurethane foam
  • Phosphorus-based flame-retardant block polyether, preparation method thereof and application of phosphorus-based flame-retardant block polyether to rigid polyurethane foam
  • Phosphorus-based flame-retardant block polyether, preparation method thereof and application of phosphorus-based flame-retardant block polyether to rigid polyurethane foam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step (1): Dissolve 11.21g (0.0575mol) of phenylphosphoryl dichloride in 35ml of tetrahydrofuran solvent and slowly add dropwise to 23g (0.0575mol) of polyether (ester) polyol with an average molecular weight of 400 and 5.82g ( 0.0575mol) in 35ml tetrahydrofuran solvent of triethylamine, stirring at 0°C to complete the dropwise addition process;

[0028] Step (2): After the dropwise addition, raise the temperature to 40°C, and continue stirring for 6 hours;

[0029] Step (3): After the reaction is over, the phosphorus-based block flame-retardant polyether is obtained through vacuum distillation;

[0030] Step (4): 20 parts of expandable graphite, 60 parts of magnesium hydroxide, 10 parts of water, 6 parts of catalyst, 10 parts of foam stabilizer and 100 parts of phosphorus-based block flame-retardant polyether and polyether (ester) polyol The mixture is mixed (10 parts of phosphorus-based block flame-retardant polyether, 90 parts of polyether (ester) polyol), and stirre...

Embodiment 2

[0033] Step (1): Dissolve 12.13g (0.0575mol) of phenyl phosphate dichloride in 30ml of 1,4-dioxane solvent and slowly add dropwise to 23g (0.115mol) of polyether polyol with an average molecular weight of 200 and 11.64g (0.115mol) of triethylamine in 35ml of 1,4-dioxane solvent, stirring at 20°C to complete the dropwise addition process;

[0034] Step (2): After the dropwise addition, raise the temperature to 65°C, and continue stirring for 12 hours;

[0035] Step (3): After the reaction is over, the phosphorus-based block flame-retardant polyether is obtained through vacuum distillation;

[0036] Step (4): 50 parts of expandable graphite, 60 parts of aluminum hydroxide, 20 parts of water, 10 parts of catalyst, 12 parts of foam stabilizer and 100 parts of phosphorus-based block flame-retardant polyether and polyether (ester) polyol The mixture is mixed (20 parts of phosphorus-based block flame-retardant polyether, 80 parts of polyether (ester) polyol), and stirred evenly at r...

Embodiment 3

[0039] Step (1): Dissolve 8.70g (0.06mol) of vinylphosphonyl chloride in 20ml of N,N-dimethylformamide solvent and slowly add dropwise to 7.2g (0.072mol) of polyether polyol with an average molecular weight of 100 and 8.29g (0.06mol) of potassium carbonate in 25ml of N,N-dimethylformamide solvent, stirring at 30°C to complete the dropwise addition process;

[0040] Step (2): After the dropwise addition, the temperature is still maintained at 30°C, and the reaction is continued for 4 hours with stirring;

[0041] Step (3): After the reaction is over, the phosphorus-based block flame-retardant polyether is obtained through vacuum distillation;

[0042] Step (4): 100 parts of expandable graphite, 15 parts of aluminum hydroxide, 15 parts of magnesium hydroxide, 25 parts of n-pentane, 1 part of catalyst, 15 parts of foam stabilizer and 100 parts of phosphorus-based block flame-retardant polyether Mix with polyether (ester) polyol mixture (30 parts of phosphorus-based block flame-r...

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Abstract

The invention relates to a phosphorus-based flame-retardant block polyether and a preparation method thereof. The preparation method comprises the steps: reacting a compound containing two P-Cl bondswith low-molecular-weight polyether glycol or polyether diamine according to a certain molar ratio to obtain a hydroxy-terminated or amino-terminated phosphorus-based flame-retardant block polyether which is high in molecular weight, good in compatibility with polyurethane, not easy to migrate and high in flame-retardant efficiency. The hydroxy-terminated or amino-terminated phosphorus-based flame-retardant block polyether serves as a part of raw material to be mechanically stirred together with polyether (polyester) polyols, isocyanate, expansible graphite, metal hydroxides, a foaming agent,a catalyst and a foam stabilizer at normal temperature according to a certain ratio, so that flame-retardant rigid polyurethane foam is prepared. The foam is not easy to shrink, good in dimensional stability and excellent in flame retardance and mechanical property.

Description

technical field [0001] The invention relates to the field of flame-retardant polyurethane foam materials, in particular to a phosphorus-based block flame-retardant polyether, a preparation method thereof and an application in rigid polyurethane foam. Background technique [0002] Rigid polyurethane foam is widely used as building insulation exterior wall materials, insulation board materials or decorative materials due to its low thermal conductivity, low density, and high strength. However, pure rigid polyurethane foam is extremely flammable after contact with an external heat source, and its limiting oxygen index is only about 18%. Therefore, there is a need to improve the flame retardancy of rigid polyurethane foams. [0003] Due to the requirements of environmental protection, the flame retardants currently used for flame retardant of polyurethane foam are mainly phosphorus-based flame retardants, including liquid organic phosphates, such as TEP, RDP, BDP, etc., and sol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/337C08G18/50C08J9/14C08J9/08C08K7/24C08K3/22C08G101/00
CPCC08G18/5078C08G65/337C08J9/141C08J2203/14C08J2375/08C08K3/22C08K7/24C08K2003/2224C08K2003/2227C08G2110/0025C08G2110/0083
Inventor 陈雅君李琳珊钱立军王建利
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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