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HPCP resin with polyhydroxy structure and preparation method thereof

A technology of cyclotriphosphazene and polyhydroxyl, which is applied in the field of cyclotriphosphazene resin and its preparation, and can solve the problems of high price, lack of large-scale application, difficult processing and moldability, etc.

Active Publication Date: 2015-04-22
杨彦威 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first is that the yield of hexachlorocyclotriphosphazene synthesis technology is too low, and the second is that all researchers are studying the ring-opening polymerization of hexachlorocyclotriphosphazene to make phosphorus nitrile elastic rubber. Due to its expensive price and its very difficult Due to its excellent processing and formability, this excellent material has not been used on a large scale all over the world.

Method used

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  • HPCP resin with polyhydroxy structure and preparation method thereof
  • HPCP resin with polyhydroxy structure and preparation method thereof
  • HPCP resin with polyhydroxy structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Synthesis of Ethylene Glycol Etherified Dihydroxycyclotriphosphazene Resin

[0057] 1) Product Description

[0058] Product Name: Ethylene Glycol Etherified Dihydroxycyclotriphosphazene Resin

[0059] Molecular weight: 381.14

[0060] Molecular Structure:

[0061]

[0062] Quality Index:

[0063] Appearance: light yellow transparent viscous liquid

[0064] Acid value: (mgKOH / g) ≤0.2

[0065] Chromaticity: (APHA) ≤55

[0066] Ignition point: ℃ ------

[0067] Specific gravity: (20 / 25°C) 1.117-1.123

[0068] Moisture: Wt.% ≤0.5

[0069] Soluble in water, alcohol, phosphate ester and other solvents.

[0070] Uses: Reactive P-N polyurethane resin flame retardant. Flame retardant polyether starter.

[0071] 2) Synthesis technology

[0072] The hexamethoxycyclotriphosphazene resin and ethylene glycol undergo ether exchange reaction to generate ethylene glycol etherified dihydroxycyclotriphosphazene resin.

[0073] Raw material ratio

[0074]

[0075] Che...

Embodiment 2

[0079] Ethylene Glycol Etherified Trihydroxycyclotriphosphoryl Resin

[0080] Raw material ratio

[0081]

[0082] Chemical reaction formula:

[0083]

[0084] In the reactor, add ethylene glycol: 37.24Kg, add hexamethoxycyclotriphosphazene resin (VI): 64.23Kg, add zirconium sulfate catalyst: 1.2Kg. Raise the temperature to 110-130°C, carry out the ether exchange reaction for 4-5 hours, distill off the methanol generated in the reaction, cool to room temperature, filter out the catalyst (reuse 8-10 times), and obtain the product: Ethylene glycol etherified trihydroxyl ring Triphosphonitrile resin: 81.25Kg. Yield: 98.8%, viscosity: 7680mPa.S / 25℃.

Embodiment 3

[0086] Ethylene Glycol Etherified Tetrahydroxycyclotriphosphoryl Resin

[0087] Raw material ratio

[0088]

[0089] Chemical reaction formula:

[0090]

[0091] In the reaction kettle, add ethylene glycol: 49.66Kg, add hexamethoxy cyclotriphosphazene resin (VI): 64.23Kg, add zirconium sulfate: 1.3Kg. Raise the temperature to 110-130°C, carry out the ether exchange reaction for 4-5 hours, distill off the methanol generated in the reaction, cool to room temperature, filter out the catalyst (reuse 8-10 times), and obtain the product: tetrahydroxyl ring etherified with ethylene glycol Triphosphazene resin: 87.26Kg. Yield: 98.9%, viscosity: 7460mPa.S / 25℃.

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Abstract

The invention discloses a HPCP resin with a polyhydroxy structure which has the representative structural formula as follows, wherein R=-(CH2)n-or -(CH2)mO(CH2)m-; and n is larger than 2 or equal to 6, and m is larger than 2 or equal to 6. A preparation method the HPCP resin with the polyhydroxy structure comprises the following steps of: having a trans-etherification reaction between HMPN HPCP resin and dihydric alcohol under the catalysis of solid acid catalyst, and carrying out aftertreatment, so that the HPCP resin with the polyhydroxy structure can be obtained. According to the technical scheme disclosed by the invention, the methyl on the HMPN HPCP resin can be exchanged into the HPCP resin with 2-6 hydroxy structures through the trans-etherification technology, and can be further reacted with the isocyanate, so that the phosphorus fine polyurethane foamed plastics can be generated, wherein the foamed plastics is novel polyurethane material: the oxygen combustion index of the phosphorus fine polyurethane foamed plastic can reach to be more than 40-50, the inflaming retarding grade can reach B1 grade of GB / T8624-2012 standard, and each physical performance index of the phosphorus fine polyurethane foamed plastics is better than that of the other polyurethane foamed plastics.

Description

technical field [0001] The invention relates to a cyclotriphosphazene resin with a polyhydroxy structure and a preparation method thereof, belonging to the field of organic synthesis. Background technique [0002] Polyphosphoryl cyanide resin has the characteristics of non-combustibility and high temperature resistance, and it can be used as a highly efficient phosphorus-nitrogen flame retardant in organic materials, and has attracted people's attention. However, in the polyurethane industry, polyphosphoryl resins are all solid and do not have hydroxyl groups or amino groups that can react with isocyanates. [0003] After the advent of phosphorus cyanide materials, due to technical reasons, they have not been applied on a large scale. The first is that the yield of hexachlorocyclotriphosphazene synthesis technology is too low, and the second is that all researchers are studying the ring-opening polymerization of hexachlorocyclotriphosphazene to make phosphorus nitrile elast...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6593C08G18/32
Inventor 杨彦威陈玉邢礼娜施海云
Owner 杨彦威
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