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Phosphaphenanthrene-containing isobornyl acrylamide oxide, and preparation method and application thereof

A technology of isobornyl acrylamide and isobornyl propyl acrylamide, which is applied in the field of isobornyl acrylamide containing phosphorus phenanthrene oxide, can solve the problem that the flame retardancy cannot meet the application requirements, and it is difficult to take care of polyurethane Foam mechanical properties and other issues

Active Publication Date: 2021-09-10
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the flame retardants used in polyurethane have the following problems: 1) the flame retardant performance cannot meet the application requirements; 2) it is difficult to take into account the mechanical properties of polyurethane foam, etc.

Method used

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  • Phosphaphenanthrene-containing isobornyl acrylamide oxide, and preparation method and application thereof
  • Phosphaphenanthrene-containing isobornyl acrylamide oxide, and preparation method and application thereof
  • Phosphaphenanthrene-containing isobornyl acrylamide oxide, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Weigh 6.19g of camphene, 1.33g of ferric chloride and 7.85ml of acrylonitrile, react at 120°C for 12h to obtain N-isobornyl acrylamide. Weigh 16.21g of DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and heat it to 160°C to be in a molten state, then add 10.37g of N-isobornyl acrylamide and stir After 24 hours of reaction, the reaction was completed, and after extraction and recrystallization, the isobornyl acrylamide-containing phosphaphenanthrene oxide was obtained. Weigh 100 parts by weight of polyether polyol (ZS4110, Jiangsu Zhongshan Chemical Co., Ltd.), 3 parts by weight of foam stabilizer modified silicone oil (OFX-0193, Suzhou Spiai New Material Co., Ltd.), 1.2 parts by weight of water, 0.1 parts by weight Parts of N,N-dimethylcyclohexylamine (DMCHA), 2.54 parts by weight of isobornyl acrylamide containing phosphaphenanthrene oxide and mixed uniformly to prepare component A. Weigh 100 parts by weight of polyisocyanate (PM-200, Wanhua Chemical Group C...

Embodiment 2

[0056] Weigh 6.19g of camphene, 1.33g of ferric chloride and 7.85ml of acrylonitrile, react at 120°C for 12h to obtain N-isobornyl acrylamide. Weigh 16.21g of DOPO and heat it to 160°C to be in a molten state, then add 10.37g of N-isobornyl acrylamide, stir and react for 24 hours, after the reaction is completed, after extraction and recrystallization, the isobornyl acrylamide-containing phosphophenanthrene oxide is obtained . Weigh 100 parts by weight of polyether polyol (ZS4110, Jiangsu Zhongshan Chemical Co., Ltd.), 3 parts by weight of foam stabilizer modified silicone oil (OFX-0193, Suzhou Spiai New Material Co., Ltd.), 1.2 parts by weight of water, 0.1 parts by weight Parts of N,N-dimethylcyclohexylamine (DMCHA), 1.0 parts by weight of isobornyl acrylamide containing phosphaphenanthrene oxide and mixed uniformly to prepare component A. Weigh 100 parts by weight of polyisocyanate (PM-200, Wanhua Chemical Group Co., Ltd.), and name it as component B. A component and B co...

Embodiment 3

[0059] Weigh 6.19g of camphene, 1.33g of ferric chloride and 7.85ml of acrylonitrile, react at 120°C for 12h to obtain N-isobornyl acrylamide. Weigh 16.21g of DOPO and heat it to 160°C to be in a molten state, then add 10.37g of N-isobornyl acrylamide, stir and react for 24 hours, after the reaction is completed, after extraction and recrystallization, the isobornyl acrylamide-containing phosphophenanthrene oxide is obtained . Weigh 100 parts by weight of polyether polyol (ZS4110, Jiangsu Zhongshan Chemical Co., Ltd.), 3 parts by weight of foam stabilizer modified silicone oil (OFX-0193, Suzhou Spiai New Material Co., Ltd.), 1.2 parts by weight of water, 0.1 parts by weight Parts of N,N-dimethylcyclohexylamine (DMCHA), 4.0 parts by weight of isobornyl acrylamide containing phosphaphenanthrene oxide and mixed uniformly to prepare component A. Weigh 100 parts by weight of polyisocyanate (PM-200, Wanhua Chemical Group Co., Ltd.), and name it as component B. A component and B co...

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PUM

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Abstract

The invention discloses aphosphaphenanthrene-containing isobornyl acrylamide oxide, and a preparation method and application thereof. The structural formula of thephosphaphenanthrene-containing isobornyl acrylamide oxide is shown in the specification, the phosphaphenanthrene-containing isobornyl acrylamide oxide has excellent flame-retardant enhancement performance. N-isobornyl acrylamide reacts with 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to obtain the phosphaphenanthrene-containing isobornyl acrylamide oxide, then the phosphaphenanthrene-containing isobornyl acrylamide oxide is blended with polyhydric alcohol, and is dissolved in the polyhydric alcohol, and then the polyhydric alcohol reacts with isocyanate to prepare rigid polyurethane foam with good flame retardant property and excellent mechanical property.

Description

technical field [0001] The invention relates to an isobornyl acrylamide phosphorus-containing phenanthrene oxide, a preparation method and an application thereof, and belongs to the field of flame-retardant reinforcing materials. Background technique [0002] Polyurethane (PU) is a kind of polymer containing urethane characteristic units in the main chain. Rigid polyurethane foams are widely used in household appliances and construction materials because of their good mechanical properties, low apparent density, and thermal conductivity. However, due to the porous structure and high specific surface area of ​​rigid polyurethane foam, the foam is easy to catch fire, the flame spreads quickly, has high flammability, and has a great fire hazard. In addition, the decomposition of rigid polyurethane foam during combustion will release a large amount of toxic gases (such as CO and HCN), while generating unbearable heat and suffocating smoke, which may cause serious fire accidents...

Claims

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Application Information

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IPC IPC(8): C07F9/6571C08G18/38C08G18/66C08G101/00
CPCC07F9/657172C08G18/288C08G18/6666C08G2110/0083C08G2110/0058
Inventor 徐徐董阜豪钱约翰孙鹏昊孙彬张双胜王石发黄真
Owner NANJING FORESTRY UNIV
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