Additive type phosphorus phenanthrene oxa-flame retardant and preparation method thereof

An additive type, flame retardant technology, applied in the field of flame retardants, can solve problems such as narrow application scope, and achieve the effects of reducing production costs, simple operation process and high output

Inactive Publication Date: 2013-01-23
SHOUGUANG WEIDONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this product is a reactive flame retardant, which has great limitations in application. It is only suitable for several special materials, and its scope of application is relatively narrow.

Method used

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  • Additive type phosphorus phenanthrene oxa-flame retardant and preparation method thereof
  • Additive type phosphorus phenanthrene oxa-flame retardant and preparation method thereof
  • Additive type phosphorus phenanthrene oxa-flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Mix 0.4mol DOPO, 0.4mol itaconic acid and 0.42mol ethylene glycol into the reaction kettle, heat up to 120°C and dissolve. After the dissolution is complete, the transparent solution is stirred evenly, and then distilled under normal pressure at 180°C for 4 hours ~8h, remove the water generated in the reaction;

[0038] (2) Add 0.02mol butyl titanate as a catalyst to the solution of step (1) at one time, distill in a semi-vacuum at 210°C and a vacuum of -0.04MPa for 2 hours, and distill out the residue in the solution of step (1) water;

[0039] (3) Distill the solution of step (2) at 240°C and a vacuum degree of -0.095MPa for 4 hours in full vacuum to polymerize the monomer intermediate of the product, and obtain the product after the polymerization is completed;

[0040] After the reaction is completed, release the product while it is hot, make it solidify, slice the product and pack it.

[0041] The DOPO derivatives prepared by the present invention have techni...

Embodiment 2

[0044] (1) Mix 0.4mol DOPO, 0.4mol itaconic acid and 0.6mol ethylene glycol into the reaction kettle, heat up to 160°C and dissolve. After the dissolution is complete, the transparent solution is stirred evenly, and then reflux distillation at 220°C for 8 hours , to remove the water generated in the reaction;

[0045] (2) Use 0.4 mol of antimony trioxide and butyl titanate mixture as a catalyst, add it to the solution of step (1) at one time, distill in a semi-vacuum at 230°C and a vacuum of -0.05MPa for 3 hours, and distill out the step ( 1) residual water in the solution;

[0046] (3) Distill the solution of step (2) under full vacuum at 280°C and vacuum degree of -0.096MPa for 12 hours to polymerize the monomer intermediate of the product, and obtain the product after the polymerization is completed;

[0047] After the reaction is completed, release the product while it is hot, make it solidify, slice the product and pack it.

[0048] The DOPO derivatives prepared by the ...

Embodiment 3

[0051] (1) Mix 0.4mol DOPO, 0.4mol itaconic acid and 0.44mol ethylene glycol into the reaction kettle, heat up to 140°C to dissolve, and stir to obtain a transparent solution after complete dissolution, then distill at 200°C under normal pressure for 5 hours , to remove the water generated in the reaction;

[0052] (2) Use 0.3mol triethylbenzyl ammonium chloride as a catalyst, add it to the solution of step (1) at one time, distill in a semi-vacuum at 220°C and a vacuum of -0.045MPa for 2h to 3h, and distill out the step ( 1) residual water in the solution;

[0053] (3) Fully vacuum distill the solution of step (2) at 260°C and a vacuum of -0.096MPa for 8 hours to polymerize the monomer intermediate of the product, and obtain the product after the polymerization is completed;

[0054] After the reaction is completed, release the product while it is hot, make it solidify, slice the product and pack it.

[0055] The DOPO derivatives prepared by the present invention have technic...

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Abstract

The invention discloses an additive type phosphorus phenanthrene oxa-flame retardant and a preparation method thereof. The chemical name of the additive type phosphorus phenanthrene oxa-flame retardant is poly-(10-taconic acid gylcol ester-9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide). The preparation method comprises the following steps of: firstly carrying out a reaction on DOPO, itaconic acid and ethylene glycol to generate a monomer midbody 10-taconic acid gylcol ester-9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide; and polymerizing the reacting midbody at high temperature under the function of catalyst to obtain a target product. The additive type phosphorus phenanthrene oxa-flame retardant provided by the invention is applicable to various high molecular materials with higher processing temperature such as linear polyester, fiber, polyamide, polyurethane and the like; and the preparation method is free from halogen, environment-friendly, simple in operation process, easy to control, high in yield, good in product repeatability, and less in impurity, wherein the product yield can be 98.5%-99.9%, and the production cost can be reduced.

Description

technical field [0001] The invention relates to a flame retardant, in particular to an additive-type phenanthrene-oxa flame retardant and a preparation method thereof. Background technique [0002] With the rapid rise of polymer material science, polymer materials are widely used in human production and life, and more and more fires are caused by them being ignited. Therefore, the flame retardancy of polymer materials has been widely recognized by people. focus on. Japan and Germany have conducted very in-depth research, and my country has also conducted extensive research in this field, and has also achieved some considerable achievements. Especially with the decrease of bromine resources, phosphorus series flame retardants with relatively good flame retardant properties have been developed rapidly. DOPO and its derivatives can introduce compounds containing flame retardant elements into polymer hosts through copolymerization. Chain, has the characteristics of high flame ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/02C08G63/692C07F9/6574
Inventor 刘瑞祥陈如林谢忠财朱之军
Owner SHOUGUANG WEIDONG CHEM
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