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Preparation method of ammonium polyphosphate cladded microsphere flame retardant

An ammonium polyphosphate and flame retardant technology, which is applied in the field of inorganic flame retardant preparation, can solve the problems of interface problems, deterioration of polymer matrix mechanical properties, research on single-component IFR system, and large addition of single-component flame retardants. , to achieve the effect of suppressing smoke production, reducing fire risk, and improving the problem of reunion

Active Publication Date: 2019-01-11
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The main problems in the flame retardant system currently used for PET fibers include: 1) the addition of single-component flame retardants is relatively large, and the flame retardant efficiency is low; 2) although the addition of multi-component flame retardants is small, The flame retardant efficiency is high, but the interface problem between the multi-component flame retardant and the polymer will deteriorate the mechanical properties of the polymer matrix; 3) In the process of flame retardant modification of the polymer, the smoke suppression performance is not fully considered
[0014] However, most of the current research on APP and carbon materials is "staying" on the compounding of APP and carbon materials in polymers, and it has not been studied as a single-component IFR system.
[0015] At the same time, the effect of APP and CMSs compounding on the flame retardant properties of PET was studied through the direct compounding method, and it was found that although there is also an intumescent flame retardant effect between the two, and the high-efficiency flame retardant effect of low smoke and low toxicity has been achieved, but the effect on PET Tensile properties have a deteriorating effect

Method used

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  • Preparation method of ammonium polyphosphate cladded microsphere flame retardant
  • Preparation method of ammonium polyphosphate cladded microsphere flame retardant
  • Preparation method of ammonium polyphosphate cladded microsphere flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Add 80ml deionized water and 4g APP into the three-necked flask, heat to 75°C, and stir thoroughly for 1 hour to obtain APP suspension.

[0045] Add 1g of CMSs, 0.5ml of glacial acetic acid, 1ml of KH-550 and 50ml of absolute ethanol into a beaker, and perform silanization reaction at 30°C for 30min.

[0046] Pour the above-prepared silanized modified CMSs reaction dispersion into the APP suspension, reflux at 80° C. for 2 h, and pour off the supernatant to obtain a crude CMSs-APP product.

[0047] The CMSs-APP crude product was dried at 80°C for 12h, ground, washed several times with absolute ethanol to remove unreacted KH-550 and other impurities, and then dried at 80°C for 12h to prepare the CMSs-APP flame retardant.

[0048] The above results were verified by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). figure 1 The morphology diagram of the raw material CMSs is given, which shows that the CMSs are spherically distributed, with smoot...

Embodiment 2

[0058] Add 80ml of deionized water and 2g of APP into the three-necked flask, heat to 80°C, and stir thoroughly for 1 hour to obtain APP suspension.

[0059] Add 1g of CMSs, 1ml of glacial acetic acid, 1.5ml of KH-550 and 50ml of absolute ethanol into a beaker, and perform silanization reaction at 40°C for 40min.

[0060] Pour the above-prepared silanized modified CMSs reaction dispersion into the APP suspension, reflux at 85° C. for 3 h, and pour off the supernatant to obtain a crude CMSs-APP product.

[0061] The CMSs-APP crude product was dried at 90°C for 18h, ground, washed several times with absolute ethanol to remove unreacted KH-550 and other impurities, and then dried at 90°C for 12h to prepare the CMSs-APP flame retardant.

Embodiment 3

[0066] Add 100ml of deionized water and 1g of APP into the three-necked flask, heat to 85°C, and stir thoroughly for 1 hour to obtain APP suspension.

[0067] Add 1g of CMSs, 1.5ml of glacial acetic acid, 2ml of KH-550 and 50ml of absolute ethanol into a beaker, and perform silanization reaction at 50°C for 50min.

[0068] Pour the above-prepared silanized modified CMSs reaction dispersion into the APP suspension, reflux at 90°C for 4 hours, and pour off the supernatant to obtain a crude CMSs-APP product.

[0069] The CMSs-APP crude product was dried at 100°C for 24h, ground, washed several times with absolute ethanol to remove unreacted KH-550 and other impurities, and then dried at 100°C for 24h to prepare the CMSs-APP flame retardant.

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Abstract

The invention relates to a preparation method of an ammonium polyphosphate cladded microsphere flame retardant. The preparation method comprises the following steps: carrying out silylation modification on the CMSs by taking CMSs (Carbon Microspheres) as a carbon source and APP as an acid source and a gas source; dissolving the APP in hot water to prepare a suspension solution; mixing the APP suspension solution with a silylation modified CMSs dispersion solution and carrying out refluxing reaction; and cladding the silylation modified CMSs through the APP to prepare the CMSs-APP flame retardant. The flame retardant prepared by the method is used for preparing a flame-retarding PET (Polyethylene Terephthalate) composite material so that the flame-retarding performance of PET can be improved and the worsening, caused by the flame retardant, of mechanical properties of a PET matrix can be reduced to the greatest extent.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic flame retardants, relates to an environmentally friendly intumescent flame retardant, in particular to a preparation method of an efficient smoke suppression integrated intumescent flame retardant. Background technique [0002] Polyethylene terephthalate (PET) is the most widely used and most consumed synthetic fiber in the world. However, the limiting oxygen index (LOI) value of PET is only 21%, which is a flammable fiber, and PET will release a lot of smoke when burned. This disadvantage severely limits the application of PET. It is necessary to modify the flame-retardant of fiber-grade PET chips to reduce its heat release and smoke generation, so as to realize the flame-retardant and smoke suppression of PET. [0003] The main problems in the flame retardant system currently used for PET fibers include: 1) the addition of single-component flame retardants is relatively large, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/02C08K9/06C08K7/18C08K9/02C08K3/32
CPCC08K3/32C08K7/18C08K9/02C08K9/06C08K2003/323C08L2201/02C08L67/02
Inventor 牛梅宋英豪薛宝霞彭云王洁
Owner TAIYUAN UNIV OF TECH
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