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Phosphorus-nitrogen synergistic flame-retardant polyol resin containing phenylethynyl group, and preparation method and application thereof

A polyol resin, phenylacetylene-based technology, applied in the field of phosphorus-nitrogen synergistic intrinsic flame retardant polyol resin and its preparation, can solve the problems of inconspicuous flame retardant effect of condensed phase, and achieve excellent intrinsic flame retardancy , the effect of strong applicability and simple preparation process

Pending Publication Date: 2020-08-07
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, melamine-derived phosphorus-nitrogen synergistic intrinsically flame-retardant polyols containing phenylacetylene groups have not been reported yet.
As an effective flame retardant element, phosphorus and nitrogen in PUF belong to the acid source and gas source respectively, and most of them play a flame retardant role in the gas phase during combustion, and the flame retardant effect of the condensed phase is not obvious.

Method used

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  • Phosphorus-nitrogen synergistic flame-retardant polyol resin containing phenylethynyl group, and preparation method and application thereof
  • Phosphorus-nitrogen synergistic flame-retardant polyol resin containing phenylethynyl group, and preparation method and application thereof
  • Phosphorus-nitrogen synergistic flame-retardant polyol resin containing phenylethynyl group, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1: Preparation of phenylethynyl-containing phosphorus-nitrogen synergistic flame-retardant polyol resin (HMMM-P-Ar)

[0028] 1) Add 19.5g of hexamethoxymethylmelamine (HMMM) and 38.25g of phosphate diol (FRC-6) into a 250mL three-necked flask connected with a fractionation device (to collect the methanol produced in the reaction), and then 0.05g P-toluenesulfonic acid (p-TsOH), under nitrogen protection, was mechanically stirred in an oil bath at 120°C for 4 hours;

[0029] 2) Lower the temperature of the oil bath to 110°C, add 53.1g of 4-phenylethynylphthalate bis(ethylene glycol)phthalate (PEPE) and 0.05g of p-TsOH, and continue mechanical stirring for 12 hours;

[0030] 3) Cool the oil bath to 70°C, and remove the non-volatile methanol in the system under reduced pressure to obtain a brown-yellow viscous polyol resin (HMMM-P-Ar), with a hydroxyl value of 159.6 mg KOH / g. The reaction formula is as follows:

[0031]

[0032] R=-CH 3 or

Embodiment 2

[0033] Embodiment 2: Flame-retardant polyol resin HMMM-P-Ar prepares rigid polyurethane foam

[0034] In an open plastic container of about 1000mL, add 59.4g HMMM-P-Ar, 25g common polyether polyol (YD-380), 2g silicone oil emulsifier (8804), 1.5g catalyst (0.75g PC-8 and 0.75g DMP-30), blowing agent (0.5gH 2 O and 16g 141b) and 14.8g dimethyl phosphate (DMMP) flame retardant, then high-speed stirring to form a uniform mixture emulsion. Finally, 75 g of liquefied isocyanate (PM-200) was added to the emulsion, stirred and mixed at a high speed, poured into an open mold, and freely foamed to obtain a rigid polyurethane foam. The density of the flame retardant foam material is about 43kg / m 3 , the compressive strength can reach 0.25MPa, the LOI can reach 28%, the UL-94 can reach the V-0 level, and the carbon residue rate can reach 27% at 800°C (nitrogen). According to the formula in Table 1, the control sample was prepared by the same method, and its density was about 36kg / m 3...

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Abstract

The invention discloses a phosphorus-nitrogen synergistic intrinsic flame-retardant polyol resin containing a phenylethynyl group. The structural formula of the polyol resin is shown in the specification. The invention also discloses a preparation method of phosphorus-nitrogen synergistic intrinsic flame-retardant polyol resin containing the phenylethynyl group. The preparation method comprises the following steps of: subjecting hexamethoxymethyl melamine (HMMM), phosphate dihydric alcohol (FRC-6) and diethylene glycol 4-phenylacetylene phthalate (PEPE) to an ether exchange reaction in a nitrogen atmosphere with p-toluenesulfonic acid (p-TsOH) as a catalyst, and then removing methanol under reduced pressure to obtain the intrinsic flame-retardant polyol resin (HMMM-P-Ar). The HMMM-P-Ar resin is used for preparing rigid polyurethane foam plastic. A preparation method for the rigid polyurethane foam plastic comprises the following steps: uniformly stirring a mixture of the HMMM-P-Ar, common polyether polyol (YD-380), a silicone oil emulsifier (8804), catalysts (PC-8 and DMP-30) and foaming agents (H2O and 141b), adding a stoichiometric amount of liquefied isocyanate (PM-200), carrying out uniform stirring and mixing at a high speed, and then pouring a formed mixture into an opened mold for free foaming to obtain the rigid polyurethane foam plastic. The foam plastic has good flameretardance and pressure resistance and high charring performance.

Description

technical field [0001] The invention relates to the technical field of flame-retardant polymer materials, in particular to a phosphorus-nitrogen synergistic intrinsic flame-retardant polyol resin containing phenylethynyl groups, a preparation method and application thereof. Background technique [0002] Rigid polyurethane foam (PUF) is widely used in external wall insulation materials, pipelines, refrigeration equipment, home appliances, etc. due to its light weight, heat insulation, and good compression resistance. As the main component of PUF, polymer polyol is usually composed of carbon, hydrogen, oxygen and other atoms, and does not contain flame-retardant elements or flame-retardant structures. Low oxygen index, belonging to flammable polymer materials. At present, from additive flame retardant to reactive flame retardant, and then to intrinsic structure flame retardant, it has become the main research trend to improve the fire resistance of flammable polymers. A varie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/32C08J9/08C08J9/14C08L75/08C07D251/70C07F9/576C08G101/00
CPCC08G18/3889C08G18/3851C08J9/08C08J9/144C07D251/70C07F9/576C08J2203/02C08J2203/142C08G2110/0025
Inventor 何吉宇贾代坤杨荣杰
Owner BEIJING INSTITUTE OF TECHNOLOGYGY