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Preparation of radiation curable halogen-free phosphor- and nitrogen-containing transparent fire-resisting paint

A kind of fireproof coating, transparent technology, applied in the field of preparation of radiation curable transparent halogen-free phosphorus and nitrogen fireproof coating, to achieve good fireproof protection, easy industrial production, and improve production efficiency

Active Publication Date: 2011-06-29
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the present invention is to propose a preparation method of a radiation-curable halogen-free phosphorus-nitrogen-containing transparent fireproof coating, so as to overcome that the existing fireproof coating cannot have good transparency at the same time , Excellent flame retardant performance and simple preparation process, expanding the application field of fire retardant coatings

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 250ml four-neck flask equipped with a mechanical stirrer, a nitrogen inlet and a condenser, add 5.55g (0.025mol) isophorone diisocyanate, 50ml chloroform, 0.01g (1000ppm) p-hydroxyanisole and 0.06g catalyst dibutyltin laurate, heat up to 50°C, slowly add 2.9g (0.025mol) hydroxyethyl acrylate dropwise under continuous stirring, react for 12 hours, cool to room temperature, then under continuous stirring 20 ml of chloroform containing 5.4 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 0.06 g of triethylamine were slowly added dropwise, and reacted at room temperature for 8 hours. The solvent was removed under reduced pressure to give the product as a viscous clear liquid.

[0019] The resulting product is analyzed by infrared, 3350cm -1 Hydroxyl characteristic peak disappears, 2235cm -1 Disappearance of isocyanate and 2384cm -1 The characteristic peak of active hydrogen of DOPO disappears; 1410cm -1 and 810cm -1 The appearance of characteristic peak...

Embodiment 2

[0021] In a 250ml four-neck flask equipped with a mechanical stirrer, a nitrogen inlet and a condenser, add 4.35g (0.025mol) toluene diisocyanate, 50ml chloroform, 0.01g (1000ppm) p-hydroxyanisole and 0.06g catalyst Dibutyltin laurate, keep the temperature below 30°C, slowly add 2.9g (0.025mol) hydroxyethyl acrylate dropwise under continuous stirring, then react for 12 hours, cool to room temperature, then slowly dropwise add 5.4 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 0.06 g of triethylamine in 20 ml of chloroform were reacted at room temperature for 8 hours. The solvent was removed under reduced pressure to obtain a viscous clear liquid.

[0022] The resulting product is analyzed by infrared, 3350cm -1 Hydroxyl characteristic peak disappears, 2235cm -1 Disappearance of isocyanate and 2384cm -1 The characteristic peak of active hydrogen of DOPO disappears; 1410cm -1 and 810cm -1 The appearance of characteristic peaks of double bonds. It can be seen t...

Embodiment 3

[0023] Example 3: Radiation Curing of Radiation Curable Transparent Fire Protection Coatings

[0024] Get 5 grams of the radiation-curable phosphorus-containing nitride prepared in Example 1, get the initiator α, α-dimethyl-α-hydroxyacetophenone (Darocur 1173) 0.15 grams (3wt%), at 60 ° C Stir to combine well. Then use a coater to coat a 100-micron film on a glass plate, and then cure it on a light curing machine or under low-energy electron beam irradiation at room temperature. The curing time is 10 seconds, and the conversion rate of double bonds is 85%. It can be seen that the material of the present invention can be rapidly formed into a film at room temperature by ultraviolet radiation, which can greatly improve production efficiency and save energy, and is easy for industrial production.

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Abstract

The invention discloses a preparation method for a radiation curable halogen free phosphorus-containing transparent flame retardant composite coating. The preparation method is characterized by comprising the following steps: taking trichloromethane as a solvent, taking partly acrylic acidified or partly methacrylic acidified polyol or polyatomic phenol as a reaction medium, adding diisocyanate according to the mol ratio under the protection of inert gas and in the presence of a catalyst and at 30 to 50 DEG C, stirring the mixture for reaction till the hydroxyl value is lower than 10mgKOH / g, adding a phosphorus-containing compound with active hydrogen and a catalyst of triethylamine according to the mol ratio after cooling, stirring the mixture at room temperature for reaction for 8 to 10hours, and carrying out decompression to remove the solvent and obtain a viscous colorless liquid which is the product of the radiation curable halogen free phosphorus-containing transparent flame retardant composite coating. The product can be quickly solidified under the condition of radiation to obtain the transparent coating which has body oxygen index of 33, V0 level vertical firing, 16.1 percent residue mass fraction at 600 DEG C, and maximal heat release rate of 208.8W / g.

Description

technical field [0001] The invention belongs to the technical field of fireproof coatings, in particular to a preparation method of radiation-curable transparent halogen-free phosphorus-nitrogen-containing fireproof coatings. Background technique [0002] At present, fire retardant coatings generally need to add a large amount of organic or inorganic flame retardants, and must be blended with the base material during construction; blending not only brings a lot of labor and complicated steps to the construction, but also the volatilization of organic solvents It will cause harm to the environment and the human body; due to the addition of a large amount of flame retardants, the overall performance of the system will be affected, for example, the transparency will be significantly reduced. Reported a kind of transparent fireproof coating that is made up of borax 26-32%, sodium sulfate 12-16%, sodium chloride 40%-50%, talcum powder 6-10% mass ratio as Chinese patent publicati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/04
Inventor 胡源邢伟义宋磊
Owner UNIV OF SCI & TECH OF CHINA
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