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High temperature crosslinked flame retardant with Schiff base and phosphoryl (phosphonyl) structure, preparation method and application thereof

A technology of Schiff base and flame retardant, which is applied in the field of high-temperature cross-linking flame retardants and their preparation, can solve the problems of inability to cross-link, high molecular structure rigidity, easy aging and decomposition, etc., and achieve excellent flame retardancy and droplet resistance , reduce the concentration of free radicals, increase the effect of melt viscosity

Active Publication Date: 2017-08-08
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the CN102732041A report, because the Schiff base contains a double C=N structure, the molecular structure is too rigid, the relative molecular weight is low, and the phosphorus content is also low, and the flame retardant efficiency is low.
In the CN103073727A report, the Schiff base C=N structure was added with phosphite, thereby losing its cross-linking anti-droplet function, and its thermal stability is poor, easy to age and decompose, which deteriorates the performance of the material
In the CN106008993A report, due to the hyperbranched structure, the C=N double bond cannot be cross-linked, the thermal stability is not high, the phosphorus content is low, and the flame retardant efficiency is low
However, in the reports of CN1974546A and CN105273173A, the Schiff base structure is only used as an intermediate to prepare epoxy resin and copolyester respectively, which limits its application and the flame retardant efficiency is not high

Method used

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  • High temperature crosslinked flame retardant with Schiff base and phosphoryl (phosphonyl) structure, preparation method and application thereof
  • High temperature crosslinked flame retardant with Schiff base and phosphoryl (phosphonyl) structure, preparation method and application thereof
  • High temperature crosslinked flame retardant with Schiff base and phosphoryl (phosphonyl) structure, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] What this embodiment prepares is flame retardant FR1, and its reaction equation is as follows:

[0042]

[0043] Heat 30.53g of p-hydroxybenzaldehyde, 18.32g of ethanolamine, and 100mL of absolute ethanol, and reflux. As the reaction progresses, yellow precipitates gradually appear in the solution. After about 6 hours, the raw materials are basically reacted completely. Suction filtration, washing with ethanol, and drying to a shallow The yellow solid was 35.49 g, the yield was 86%, and it was recorded as monomer Ⅰ-1.

[0044] Mix 35.49g of monomer Ⅰ-1 and 63.80g of monomer Ⅱ-1, under the protection of nitrogen, stir and raise the temperature to 180°C to soften and melt the system, continue to maintain the temperature until the rod climbing phenomenon occurs, and then raise the temperature to 250°C to continue the reaction 1 h gave the product as a dark yellow solid. The hydrogen chloride gas discharged from the system is absorbed with sodium hydroxide solution. Af...

Embodiment 2

[0046] What this embodiment prepares is flame retardant FR2, and its reaction equation is as follows:

[0047]

[0048] Heat 26.04g of 3-mercaptobutyraldehyde, 15.02g of ethylenediamine and 100mL of absolute ethanol, and reflux. As the reaction progresses, a yellow precipitate gradually appears in the solution. After about 8 hours, the raw materials are basically reacted completely. Suction filtration, washing with ethanol, After drying, 29.25 g of a light yellow solid was obtained, with a yield of 80%, which was designated as monomer Ⅰ-2.

[0049] Mix 29.25g of monomer I-2, 53.99g of monomer II-1 and 2.02g of calcium chloride, under the protection of nitrogen, stir and raise the temperature to 110°C to soften and melt the system, continue to maintain the temperature until the rod climbing phenomenon occurs, and then The temperature was raised to 150° C. to continue the reaction for 5 h to obtain a dark yellow solid product. The hydrogen chloride gas discharged from the sy...

Embodiment 3

[0051] What this embodiment prepares is flame retardant FR3, and its reaction equation is as follows:

[0052]

[0053] Heat 29.04g of 2-methyl-3-methylpentanal, 22.73g of p-hydroxyaniline and 100mL of absolute ethanol, and reflux. As the reaction proceeds, a yellow precipitate gradually appears in the solution. After about 6 hours, the basic reaction of the raw materials is basically complete. Filter, wash with ethanol, and dry to obtain 37.57 g of a light yellow solid with a yield of 87%, which is designated as monomer Ⅰ-3.

[0054] Mix 37.57g of monomer I-3, 51.26g of monomer II-1 and 0.02g of aluminum chloride under the protection of nitrogen, stir and raise the temperature to 170°C to soften and melt the system, continue to maintain the temperature until the rod climbing phenomenon occurs, and then The temperature was raised to 220° C. to continue the reaction for 2 h to obtain a dark yellow solid product. The hydrogen chloride gas discharged from the system is absorb...

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Abstract

The invention discloses a high temperature crosslinked anti-dripping flame retardant with Schiff base and phosphoryl (phosphonyl) structure. The flame retardant has the following repeating structure unit shown as the specification. The flame retardant is obtained by subjecting a monomer I with a Schiff base structure and a monomer II with a phosphoryl (phosphonyl) structure to melting reaction or solution reaction under nitrogen protection. The flame retardant disclosed by the invention simultaneously introduces the Schiff base high temperature chemical crosslinking structure and the phosphoryl (phosphonyl) high efficiency flame retardant group, not only can produce a synergistic flame retardant effect of phosphorus and nitrogen, endows the polymer with excellent flame retardant and anti-dripping effects, but also can significantly reduce the heat release rate and total heat release of the material, and can be used for flame retardation of unsaturated polyester resin, epoxy resin, polyester, polyolefin and other materials. The preparation method provided by the invention is simple and easy for control, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of high temperature crosslinking flame retardant and its preparation and application. Specifically, the present invention relates to a class of high-temperature cross-linking flame retardants with Schiff base and phosphorous (phosphonic) acyl structures and a preparation method thereof. , anti-droplet and other characteristics, suitable for flame retardant of unsaturated polyester resin, epoxy resin, polyester, polyolefin and other polymers. Background technique [0002] At present, the flame retardant treatment method for most polymer materials is mainly to add flame retardants to them. Although halogen-containing flame retardants are still widely used as a class of flame retardants, their applications are gradually being restricted due to their easy release of irritating and corrosive toxic gases when burned. Inorganic flame retardants, usually added in large amounts, will have adverse effects on the phy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04C08G79/02C08L23/12C08L63/00C08L67/02C08L67/06C08L85/02
CPCC08G79/02C08G79/04C08L23/12C08L63/00C08L67/02C08L67/06C08L2201/02C08L85/02
Inventor 王玉忠赵丹王娟汪秀丽陈力
Owner SICHUAN UNIV
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