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Novel preparation method of polymeric phosphate ester flame retardant containing active hydroxyl

A phosphoric acid ester and flame retardant technology is applied in the new field of preparation of active hydroxyl-containing polymerized phosphoric acid ester flame retardants. The overall performance of the product is improved and the process is easy to operate.

Active Publication Date: 2012-07-25
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patent has the following defects: (i) the process conditions cannot guarantee that phosphorus oxychloride reacts with monohydric alcohol to form a monoester, which is not conducive to obtaining a polymeric phosphate product with a small distribution index; (ii) triethylamine is used as an acid-binding agent, forming About 7% of triethylamine hydrochloride is dissolved in the product and cannot be completely removed by filtration, which will affect the performance of the product
The polymeric phosphate ester products are very soluble in water, even completely soluble in water, and the actual purification will be difficult

Method used

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  • Novel preparation method of polymeric phosphate ester flame retardant containing active hydroxyl
  • Novel preparation method of polymeric phosphate ester flame retardant containing active hydroxyl
  • Novel preparation method of polymeric phosphate ester flame retardant containing active hydroxyl

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Add 5% mass (based on theoretical product) melamine and stir for 1 h, filter to remove melamine salt, distill off solvent and low boiling point to obtain polymeric phosphate. Yield 89.2%, viscosity 2.45Pa.s, acid value 0.46mgKOH / g, phosphorus content 18.64%, hydroxyl value 21.2mgKOH / g, decomposition temperature 182°C, density 1.096 (25°C), refractive index n D 25 =1.4550, number average molecular weight M n GPC = 3750, distribution index PD = 1.27 (see the appendix image 3 ).

[0032] Embodiment 2. In the 500mL four-neck flask that agitator, thermometer, reflux condenser and hydrogen chloride absorption device are equipped, add 153.5g (1mol) newly distilled phosphorus oxychloride, 100mL dichloroethane and 0.38g stannous octoate , stir, cool to 0°C with an ice-water bath, slowly add 46g (1mol) of absolute ethanol dropwise, keep the system below 6°C during the dropwise addition, after the dropwise addition, slowly raise the temperature to 20-30°C and keep it warm for...

Embodiment 2

[0033] Add 3% mass (based on theoretical product) melamine and stir for 1 h, filter to remove melamine salt, distill off solvent and low boiling point to obtain polymeric phosphate. Product yield 89.5%, viscosity 2.42Pa.s, acid value 0.37mgKOH / g, phosphorus content 18.60%, hydroxyl value 23.2mgKOH / g, decomposition temperature 182°C, density 1.096 (25°C), refractive index n D 25 = 1.4553.

[0034] In order to show the application performance of this product, the application example in polyurethane rigid foam is given below. Active hydroxyl-containing polymeric phosphate, trichloroethyl phosphate and dimethyl methylphosphonate were used for application tests. Mix 30g of the above flame retardant with 100g of polyether polyol (KIF3027), use 142g of crude MDI as curing agent, and add auxiliary materials such as foaming agent and foam stabilizer to carry out free foaming experiment of polyurethane rigid foam. Test rigid foam properties. The foaming environment temperature is 25...

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Abstract

The invention discloses a novel preparation method of a polymeric phosphate ester flame retardant containing active hydroxyl. The preparation method comprises the following steps of: by using dichloroethane as a solvent and using stannous octoate as a catalyst, mixing phosphorus oxychloride and ethanol with the same molar weight at a temperature of 6 DEG C below; then heating to the temperatureof 20 to 30 DEG C and performing heat preservation reaction for 2h; slowly and dropwise adding excessive 5 percent of ethylene glycol; heating to the temperature of 45 DEG C to carry out heat preservation for 2 to 3h and heating to the temperature of 65 DEG C to carry out heat preservation for 1 to 2h; completely discharging hydrogen chloride; removing trace of acid by melamine and distilling thesolvent and low boiling point substances to obtain the polymeric phosphate ester flame retardant containing the active hydroxyl. The polymerization product prepared by the method has narrow molecularweight distribution and high comprehensive performances. The recovered melamine can be recycled after being processed. The cost can be reduced. The novel preparation method has simple process and is easy to operate.

Description

technical field [0001] The invention relates to a new method for preparing a flame retardant of a halogen-free phosphate polymer containing an active hydroxyl group. The polymer is used for polyurethane flame retardant without migration and without affecting its physical properties. technical background [0002] Polyurethane is one of the widely used polymer materials. Because of its good heat insulation, moisture resistance, low temperature resistance and excellent mechanical properties, it has grown in the fields of building insulation, elastomers, car seat soft foam and furniture integral skin foam. very quickly. Since polyurethane materials are flammable, the flame retardant modification of polyurethane has become a research hotspot in this field. Dimethyl methylphosphonate, trichloroethyl phosphate, etc. are typical flame retardants used in polyurethane foam, but these compounds have small molecular weight, easy to precipitate, poor migration resistance, and strong odo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04C08G18/64
Inventor 王彦林康天飞
Owner SUZHOU UNIV OF SCI & TECH