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Zirconium hydrogen phosphate synergistic nitrogen-containing phenolic resin flame-retardant aqueous polyacrylate emulsion and preparation method thereof

A technology of polyacrylate emulsion and zirconium hydrogen phosphate, which is applied in the field of flame-retardant acrylate emulsion, can solve the problems of difficult industrialization, high cost, and high cost, and achieve improved mechanical properties, good wear resistance, and good compatibility Effect

Active Publication Date: 2017-10-20
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when the reactive flame retardant is used in a small amount in this method, the ideal flame retardant effect cannot be achieved; when the amount is large, it will affect the stability of the emulsion, and it is expensive and difficult to realize industrialization
Chinese invention patent application CN102964514A introduces silicon, fluorine and phosphoric acid groups into the polyacrylate emulsion. The three have a synergistic flame-retardant effect and effectively improve the flame-retardant performance of the polyacrylate emulsion, but this method also has high costs. Shortcomings
Chinese invention patent application CN1024311725A prepared a flame-retardant polyacrylate emulsion. While using a reactive flame retardant, a small amount of antimony compounds were added as a flame-retardant synergist to achieve a relatively good flame-retardant effect, but Antimony compounds have poor dispersion in the emulsion, which affects the storage stability of the emulsion

Method used

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  • Zirconium hydrogen phosphate synergistic nitrogen-containing phenolic resin flame-retardant aqueous polyacrylate emulsion and preparation method thereof
  • Zirconium hydrogen phosphate synergistic nitrogen-containing phenolic resin flame-retardant aqueous polyacrylate emulsion and preparation method thereof
  • Zirconium hydrogen phosphate synergistic nitrogen-containing phenolic resin flame-retardant aqueous polyacrylate emulsion and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Take 3g of zirconium hydrogen phosphate and disperse it in a beaker filled with 300g of water, ultrasonically disperse for 30min, then add 11.92g of tetrabutylammonium hydroxide (TBA, mass fraction about 25%) aqueous solution to it for intercalation modification. Continue to ultrasonically disperse for 30 minutes, stir for another 8 hours, and obtain organically modified zirconium hydrogen phosphate by high-speed centrifugation and drying.

[0028] 30g water, 1.42g emulsifier propoxynonylphenol polyoxyethylene (10) ammonium sulfate (DNS-86), 7.12g 2-hydroxyethyl methacrylate phosphate (PM-1500, Guangzhou Jingde Chemical Materials Co., Ltd.) placed in a 500ml beaker and mixed evenly. Then 30g of methyl methacrylate, 30g of butyl acrylate and 1.32g of acrylic acid were mixed evenly and slowly added thereto, and pre-emulsified by a high-speed dispersing homogenizer, and the pre-emulsification time was 20 minutes. Then disperse 0.68 g of organically modified zirconium hydr...

Embodiment 2

[0032]The difference between this example and Example 1 is that the amount of water-based nitrogen-containing phenolic resin is reduced to 57.22g (25wt%). The mechanical properties and limiting oxygen index test results are shown in Table 1. It can be seen that the limiting oxygen index of the water-based polyacrylate emulsion prepared in this example is 28.5%, which is lower than that in Example 1, but still has a relatively good flame retardant performance, indicating that the amount of water-based nitrogen-containing phenolic resin has an important effect on the material. The flame retardant performance has a certain influence. And compared with Comparative Example 3, it can be seen that adding a small amount of synergist can reduce the amount of flame retardant and reduce the cost.

Embodiment 3

[0034] The difference between this example and Example 1 is that the amount of organically modified zirconium hydrogen phosphate is reduced to 0.34g (0.5wt%). The mechanical properties and limiting oxygen index test results are shown in Table 1. It can be seen that the limiting oxygen index of the water-based polyacrylate emulsion prepared in this example is 29.0%, which is lower than that in Example 1, but still has a relatively good flame retardant performance, indicating that the amount of organically modified zirconium hydrogen phosphate It also has a certain influence on the flame retardancy of the material.

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Abstract

The invention discloses a zirconium hydrogen phosphate synergistic nitrogen-containing phenolic resin flame-retardant water-based polyacrylate emulsion and a preparation method thereof. Its preparation method is: after mixing acrylate monomer, 2-hydroxyethyl methacrylate phosphate, emulsifier DNS-86 and water, high-speed stirring for pre-emulsification, the pre-emulsification time is 15min-30min, and then adding Add organically modified zirconium hydrogen phosphate, continue pre-emulsification for 10-20 minutes to obtain pre-emulsion; prepare zirconium hydrogen phosphate modified polyacrylate emulsion by semi-continuous pre-emulsification emulsion polymerization; adjust the pH of the emulsion to 8-9, add nitrogen-containing The phenolic resin aqueous solution is uniformly mixed to obtain the zirconium hydrogen phosphate synergistic nitrogen-containing phenolic resin flame-retardant aqueous polyacrylate emulsion. The zirconium hydrogen phosphate synergistic nitrogen-containing phenolic resin flame-retardant water-based polyacrylate emulsion prepared by the invention has good stability, low cost, and good flame-retardant performance and mechanical performance.

Description

technical field [0001] The invention relates to a flame-retardant acrylate emulsion, in particular to a flame-retardant water-based polyacrylate emulsion of zirconium hydrogen phosphate synergistic nitrogen-containing phenolic resin and a preparation method thereof. Background technique [0002] Water-based polyacrylate emulsion has the advantages of environmental protection, weather resistance and excellent mechanical properties, and has been widely used in architectural coatings, industrial coatings and automotive coatings. However, acrylate polymers are flammable, and once a fire breaks out, it will pose a huge threat to people's lives and property. Therefore, it is of great significance to study the flame retardancy of acrylate emulsions. [0003] Adding some traditional flame retardants such as ammonium polyphosphate, melamine, metal hydroxide, etc. to acrylate emulsion can effectively improve its flame retardant performance. Chinese invention patent application CN103...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L61/14C08L33/12C08L33/08C08F220/18C08F220/14C08F220/06C08F230/02C08F2/44C08K9/04C08K3/32
Inventor 曾幸荣雷慧敏赖学军李红强张亚军马文石边国民汪启鸿
Owner SOUTH CHINA UNIV OF TECH