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A kind of preparation method of unsaturated polyester flame retardant composite material

A flame-retardant composite material and unsaturated technology, which is applied in the field of polymer material preparation, can solve problems such as low flame-retardant efficiency, threats to the environment and personal life safety, and reduced UV resistance of matrix materials, so as to prevent further escape, Effect of increasing high temperature stability and improving flame retardancy

Active Publication Date: 2016-05-11
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the introduction of halogen reduces the anti-ultraviolet ability of the base material, and produces a large amount of smoke and corrosive toxic gases during combustion, which poses a serious threat to the environment and personal safety.
Inorganic flame retardants (mainly Al(OH) 3 and Mg(OH) 2 ) has a low flame retardant efficiency, and requires a high addition amount (mass fraction>50%) to achieve a certain flame retardant effect, which will seriously affect the mechanical properties and processing fluidity of the composite material

Method used

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  • A kind of preparation method of unsaturated polyester flame retardant composite material
  • A kind of preparation method of unsaturated polyester flame retardant composite material
  • A kind of preparation method of unsaturated polyester flame retardant composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Under the protection of nitrogen, add 0.125mol PEPA, 0.1mol triethylamine, 100ml acetonitrile into the reaction flask equipped with magnetic stirring, reflux condensing device and drying protection device. The buret starts to add 0.05mol methyl vinyl dichlorosilane dropwise, and the dropwise addition is complete within 1-2 hours. Then the temperature was raised to 60°C for 2h, and then raised to reflux temperature for 6h, the reaction was stopped and cooled to room temperature. Filter, wash with ether and methanol, and dry for 8 hours at 80°C under a vacuum of 0.1 MPa to obtain the target flame retardant DPMVSi.

[0029] Add 90g of 191 to a 250ml beaker at room temperature #Pure unsaturated polyester and 10g target flame retardant DPMVSi, stir evenly for 20min (to prevent the generation of air bubbles), then slowly add 0.5g accelerator, continue stirring for 5min, add 1g initiator, stir for another 5min, put it in a vacuum drying oven at room temperature , 0.08MPa vac...

Embodiment 2

[0032] Under the protection of nitrogen, add 0.1mol PEPA, 0.1mol triethylamine, 100ml acetonitrile to the reaction flask equipped with magnetic stirring, reflux condensing device and drying protection device, raise the temperature to 60°C, and start dropping 0.05 mol of methyl vinyl dichlorosilane, 1 ~ 2h drop completely. Then the temperature was raised to 70°C for 2h, and then raised to reflux temperature for 6h, the reaction was stopped and cooled to room temperature. Filter, wash with ether and methanol, and dry at 80°C under 0.1MPa vacuum for 10 hours to obtain the target flame retardant DPMVSi.

[0033] attached figure 1 It is the infrared spectrogram of the target flame retardant DPMVSi that the present embodiment makes; Among the figure: 3064cm -1 for -CH=CH 2 The stretching vibration absorption peak of C-H in , 2963cm -1 for -CH 3 The stretching vibration absorption peak of the , 1411cm -1 for -CH=CH 2 scissor vibration absorption peak, 1190cm -1 It is the stre...

Embodiment 3

[0038] Under the protection of nitrogen, add 0.15mol PEPA, 0.15mol triethylamine, 150ml acetonitrile to the reaction flask equipped with magnetic stirring, reflux condensing device and drying protection device, raise the temperature to 55 °C, and start dropping 0.06 mol of methyl vinyl dichlorosilane, 1 ~ 2h drop completely. Then the temperature was raised to 75° C. for 2 h, then raised to reflux temperature for 6 h, the reaction was stopped and cooled to room temperature. Filter, wash with ether and methanol, and dry at 80°C under 0.1MPa vacuum for 10 hours to obtain the target flame retardant DPMVSi.

[0039] Add 70g of 196 to a 250ml beaker at room temperature # Pure unsaturated polyester and 30g target flame retardant DPMVSi, stir evenly for 20min (to prevent the generation of air bubbles), slowly add 0.9g accelerator, continue stirring for 5min, then add 1.8g initiator, stir for another 5min and put in vacuum Defoaming treatment was carried out in a drying oven at room ...

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Abstract

The invention discloses a preparation method of an unsaturated polyester flame-retardant composite material, which is characterized by comprising the steps of adding 1-aminophospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane, triethylamine and acetonitrile into a reactor, and heating to 50-60 DEG C; dropwise adding methylvinyl dichlorosilane, heating to 60-70 DEG C, and reacting for 2h; heating to the backflow temperature and reacting for 6h, and cooling; filtering, washing and drying the separated solid to obtain a bicyclic cage-like phosphorosilicate flame retardant with an active double bond; mixing and stirring unsaturated polyester resin and the bicyclic cage-like phosphorosilicate flame retardant with an active double bond; adding an accelerant and an initiator and stirring and mixing; treating for 5-10min in a vacuum drying oven; then pouring into a mould, curing at normal temperature and aging at high temperature to obtain the unsaturated polyester flame-retardant composite material with good flame retardance and thermal stability. The method disclosed by the invention has the advantages that the raw materials are easily available, the process is simple and the practicability is high.

Description

technical field [0001] The invention belongs to the preparation of polymer materials, and relates to a method for preparing unsaturated polyester flame-retardant composite materials, in particular to a method for flame-retardant unsaturated polyester materials using bicyclic caged phosphorus silicon flame retardants with active double bonds Methods. The unsaturated polyester flame-retardant composite material prepared by the invention can be used in the fields of traffic vehicles, building materials, electronic appliances, chemical equipment and the like. Background technique [0002] Unsaturated polyester resin (UPR for short) is a linear polymer compound formed by polycondensation reaction of unsaturated dibasic acid (maleic anhydride), saturated dibasic acid and diol. (Usually styrene) from the viscous liquid. Since the UPR molecular chain contains unsaturated double bonds, it can be copolymerized with monomers containing double bonds such as styrene and methyl methacry...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/01C08F230/08
Inventor 胡小平李良君衡惠敏徐启奎
Owner SOUTHWEAT UNIV OF SCI & TECH
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