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Polymer type phosphor-containing fire retardant, preparation method and application thereof

A flame retardant and reactive technology, which is applied in the field of polymer-type phosphorus-containing flame retardants and their preparation, can solve problems such as application limitations, and achieve the effects of stable product quality, superior flame retardant performance, and high production efficiency

Inactive Publication Date: 2012-12-19
JIANGSU DAMING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Based on the requirements of environmental protection and sustainable development, some halogenated flame retardants have been banned, and some are also treated with caution by people, and their applications are restricted.

Method used

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  • Polymer type phosphor-containing fire retardant, preparation method and application thereof
  • Polymer type phosphor-containing fire retardant, preparation method and application thereof
  • Polymer type phosphor-containing fire retardant, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Use a vacuum pump to pump 767.5Kg of phosphorus oxychloride into the No. 1 reaction kettle, cool down to 10-15°C, and feed nitrogen into the kettle with a flow rate of 2m 3 / h, protect against oxidation, and slowly add 62Kg of ethylene glycol dropwise, dropwise for 8h, after the dropwise addition is completed, the temperature is raised to 18°C, and the material is stirred for 1h; the nitrogen gas is stopped, and the excess POCl 3 Distilled at -0.1MPa, 55°C under reduced pressure, after the distillation is completed, the temperature is lowered, and the discharge is passed into the No. 2 reaction kettle;

[0032] (2) Add catalyst AlCl to No. 2 reactor 3 Stir 533.4g for 0.5h, control the reaction temperature at 10-13°C with ice-salt water, add 184Kg of absolute ethanol dropwise, the dropwise addition time is 6h, after the dropwise addition, the temperature is raised to about 25°C, and the reaction is kept for 4h; the catalyst is removed by low-pressure suction filtrati...

Embodiment 2

[0034] In this example, according to the preparation process of Example 1, through multiple experiments, the molar ratio of raw materials, the amount of catalyst used, and the reaction temperature were respectively changed to obtain the optimal process.

[0035] 2.1 Molar ratio of raw materials in the first step reaction

[0036] Change the ratio of phosphorus oxychloride and ethylene glycol in the first step reaction (as table 1), other conditions carry out the first step reaction with embodiment 1, and wherein temperature refers to the temperature of dripping ethylene glycol.

[0037] Table 1

[0038]

Phosphorus oxychloride

Ethylene glycol

temperature

Group 1

2

1

10～15℃

Group 2

3

1

10～15℃

group 3

5

1

10～15℃

Group 4

7

1

10～15℃

Group 5

8

1

10～15℃

[0039] After analysis, the polymerization degree of the first group is 10-15,...

Embodiment 3

[0058] The flame retardant PNX of the present invention and the phosphorus-halogen flame retardant T101 (Tetrakis(β-chloroethyl)-1,2-ethylene bisphosphoric acid) is added in flexible polyurethane foam plastics for automobiles, the preparation process is a conventional process, and the respective formulas and properties are shown in Table 5 and Table 6.

[0059] Table 5.T 101 Formulation and Properties of Flame Retardant Flexible Polyurethane Foam

[0060] formula

[0061] Surfactant

[0062] Table 6. Formulation and performance of PNX flame-retardant flexible polyurethane foam

[0063] formula

[0064] It can be seen from Table 5 and Table 6 that PNX reaches T 101 Adding 40% of the amount can achieve the same flame retardant effect, and its oxygen index is slightly higher than that of T101 flame retardant flexible polyurethane foam, and PNX flame retardant flexible polyurethane foam does not produce toxic smoke in the combustion test , and T101...

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Abstract

Disclosed are a polymer type phosphor-containing flame retardant, preparation method and application thereof, which belong to the field of chemical materials. The polymer type phosphor-containing flame retardant PNX is a compound shown in formula (1), wherein n is an integer of 5~8 and the molecular weight of the flame retardant is between 900 and 1400. The method for preparing the flame retardant PNX is as follows: reacting phosphorus oxychloride with ethylene glycol in a nitrogen environment through a chemical reaction shown in the reaction formula (1) to obtain a compound (2), then reacting the compound (2) with anhydrous ethanol through a chemical reaction shown in reaction formula (2) under the action of a catalyst aluminum chloride to produce the flame retardant PNX. The flame retardant PNX belongs to a halogen-free, phosphorous type flame retardant. It coincides with the national concept of green-environmentally-friendly development. The content of phosphor is as high as 18%~20%, and the flame retardant properties are excellent.

Description

technical field [0001] The invention belongs to the field of chemical materials, and relates to a polymer-type phosphorus-containing flame retardant and a preparation method and application thereof. Background technique [0002] Based on the requirements of environmental protection and sustainable development, some halogenated flame retardants have been banned, and some are treated with caution by people, and their applications are restricted. Since the promulgation of the EU ROHS and WEEE directives in 2003, the application of phosphorus-halide flame retardants has also been restricted to a certain extent, so that the calls for green and environmentally friendly halogen-free phosphorus flame retardants are getting louder and louder. Contents of the invention [0003] The object of the present invention is to provide a polymer-type phosphorus-containing flame retardant to address the above-mentioned deficiencies of the prior art. [0004] Another object of the present inv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K21/14C08G79/04C08L75/04C08L85/02
CPCC09K21/14C08L85/02C07F9/093C08G79/04
Inventor 潘小明李执阶潘新明
Owner JIANGSU DAMING TECH
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