Preparation method of reaction type halogen-free phosphorous flame retardant polyester polyol

A flame-retardant polyester and polyol technology, which is applied in the field of preparation of organic polymer compounds, can solve the problems of non-environmental protection in the production process, migration of flame retardants, and low flame-retardant performance, and achieve easy industrial production, improved compressive strength, The effect of meeting environmental protection requirements

Active Publication Date: 2013-04-17
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the additive-type halogen-containing flame-retardant polyurethane foam materials widely used in the market have low flame-retardant performance and are not environmentally friendly.
There are many technical defects in these polyurethane foam materials: due to the excessive amount of added flame retardant, not only it is easy to cause the migration of flame retardant, the flame retardant effect cannot be maintained for a long time, but also the physical properties of the main material are destroyed; polyurethane foam is a flammable material , can easily cause catastrophic fires, causing serious personnel and property losses; more bromine flame retardants are used, which produce toxic, harmful and strongly irritating hydrogen halide gases during combustion, which is difficult to meet environmental protection requirements
Chinese patent application publication 101747371A uses the method of collecting toxic gas phosphine, reacting it with formaldehyde, and then reacting with epoxy compounds to generate halogen-free flame-retardant hydrolyzed phosphorus-containing polyether / polyester polyols. This method is not conducive to industrialization
The polyester polyols researched and developed above all have limitations such as containing non-environmentally friendly halogens, low flame retardancy, or the production process is not environmentally friendly, and cannot provide reactive halogen-free flame-retardant polyester polyols required by the market.
It also cannot solve the technical problem of the easy migration of additive flame retardants, and cannot realize the environmental protection and permanent flame retardancy of polyurethane materials

Method used

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  • Preparation method of reaction type halogen-free phosphorous flame retardant polyester polyol
  • Preparation method of reaction type halogen-free phosphorous flame retardant polyester polyol
  • Preparation method of reaction type halogen-free phosphorous flame retardant polyester polyol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Mix 200kg of malonic acid, 155kg of ethylene glycol, 17.75kg of hydroxymethylphenyl hypophosphorous acid and 0.37kg of tetramethyl titanate into the reaction kettle, heat up under stirring, when the temperature reaches 60-90°C, fill it with nitrogen Evacuate and continue to heat up. When the temperature reaches 125-155°C, react for 2-8 hours, then continue to heat up to 180°C, vacuumize to 100-5000Pa, and control the reaction temperature to 180-245°C. After reacting for 2 to 4 hours under this condition, take samples to test the acid value every 10 to 40 minutes. When the acid value drops below 2mgKOH / g, stop heating and stop stirring. When the temperature in the kettle drops to 130 to 160°C, stop the vacuum. The material is discharged to obtain a reactive halogen-free phosphorus-containing flame-retardant polyester polyol.

Embodiment 2

[0028] Mix 234kg of malonic acid, 222kg of propylene glycol, 22.8kg of flame retardant (hydroxymethylphenylphosphorous acid: hydroxypropylphenylphosphorous acid = 3:1 mass ratio) and 0.96kg of tetraisopropyl titanate into the reaction In the still, others are with embodiment 1.

Embodiment 3

[0030] 234kg succinic acid, 196kg propylene glycol, 22.8kg hydroxyethyl phenyl hypophosphorous acid and 0.96kg antimony trioxide were mixed into the reactor, and the others were the same as in Example 1.

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Abstract

The invention discloses a preparation method of reaction type halogen-free phosphorous flame retardant polyester polyol. The preparation method is characterized by comprising following steps: taking binary acid, dihydric alcohol, halogen-free phosphorous copolymer fire retardant and catalyst to be put into a reaction kettle, stirring and warming up, filling nitrogen to empty, reacting for 2 to 8h when the temperature reaches 125 to 155 DEG C, then warming up to 180 DEG C, vacuumizing to ensure the air pressure to be 100 to 5000 Pa, controlling reaction temperature to be 180 to 245 DEG C, after reacting for 2 to 4h, sampling at an interval of 10 to 40 min to test acid value, stopping heating when the acid value is reduced below 2 mgKOH/g, and stirring for cooling so as to obtain the reaction type halogen-free phosphorous flame retardant polyester polyol. The reaction type halogen-free phosphorous flame retardant polyester polyol is applied to synthesis of rigid or soft polyurethane foamed plastic, and the prepared polyurethane foamed plastic has excellent flame retardant property, and the limit oxygen index can be up to more than 32%.

Description

technical field [0001] The invention belongs to the preparation of organic polymer compounds, and relates to a preparation method of reactive halogen-free phosphorus-containing flame-retardant polyester polyol for polyurethane foam materials. Background technique [0002] In the various applications of polyurethane materials, because polyurethane foam has many advantages such as light weight and low thermal conductivity, especially in many fields such as construction and product packaging, polyurethane foam is widely used, and it has become a representative of polyurethane. application field. At present, most of the additive-type halogen-containing flame-retardant polyurethane foam materials widely used in the market have low flame-retardant performance and are not environmentally friendly. There are many technical defects in these polyurethane foam materials: due to the excessive amount of added flame retardant, not only it is easy to cause the migration of flame retardant...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692C08G18/46C08G101/00
Inventor 周艳玲梁倩倩刘健飞罗金安
Owner SICHUAN DONGFANG INSULATING MATERIAL
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