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Pentaerythritol diphosphonate dichloride ethylenediamine macromolecular flame retardant and preparation method thereof

A technology of pentaerythritol diphosphate diphosphoryl chloride ethylenediamine and pentaerythritol diphosphate diphosphoryl, which is applied in the field of "trinity" macromolecular intumescent flame retardants, can solve the problems of high-speed stirring, difficult process control, and cost Advanced problems, achieve the effect of reducing preparation cost, low reaction temperature and short reaction time

Inactive Publication Date: 2012-08-08
SUZHOU UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the microencapsulation process has problems such as "difficult process control", "requires high-speed stirring, high energy consumption", and "high cost".

Method used

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  • Pentaerythritol diphosphonate dichloride ethylenediamine macromolecular flame retardant and preparation method thereof
  • Pentaerythritol diphosphonate dichloride ethylenediamine macromolecular flame retardant and preparation method thereof
  • Pentaerythritol diphosphonate dichloride ethylenediamine macromolecular flame retardant and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment one: preparation process sees appendix figure 1 :

[0023] [1] Add 27.2g (0.2mol) of pentaerythritol and 108.8 mL (1.2mol) of phosphorus oxychloride, heated in an oil bath, stirred, and refluxed for reaction. First react at 60°C for 1h, then at 105°C for 7h until no HCl is released. After phosphorus oxychloride was distilled off under reduced pressure, it was cooled, washed with dichloromethane, and filtered. Dry to constant weight under vacuum at 110°C to obtain pentaerythritol diphosphate diphosphoryl chloride (PDD) with a yield of about 82%.

[0024] Infrared analysis was carried out on the obtained intermediate products, such as figure 2 , shows: 1306cm -1 It is the stretching vibration peak of P=O; 856cm -1 It is the stretching vibration peak of P-O; 1024 cm -1 It is the stretching vibration peak of P - O-C; 548cm -1 It is the P-Cl stretching vibration peak. This result indicated that PDD was successfully prepared.

[0025] [2] Add 2.97g of PD...

Embodiment 2

[0027] Embodiment two, test the flame retardant property of macromolecule flame retardant:

[0028] Add the macromolecular flame retardant of Example 1 to E-44 epoxy resin at a mass fraction of 5%, 10%, 20%, and 30%, stir evenly, and then add 1g of curing agent EDA to prepare a standard sample According to the GB / T2406-93 plastic oxygen index test method and the plastic vertical burning test method in UL-94-1996, the samples were tested for the limiting oxygen index (LOI) test and the plastic combustion performance test.

[0029] The results are shown in the table below. The average limiting oxygen index (LOI) of the blank epoxy resin sample is 18%. -Level 0.

[0030] Macromolecular flame retardant content (wt%) LOI (%) UL-94 0 18 V-3 5 26 V-0 10 28 V-0 20 32 V-0 30 38 V-0

[0031] The morphology of the macromolecular flame retardant flame retardant epoxy resin splines changed obviously before and after burning. The photo of t...

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Abstract

The invention discloses a preparation method of a pentaerythritol diphosphonate dichloride ethylenediamine macromolecular flame retardant. The method is characterized by comprising the following steps of: (1) reacting phosphorus oxychloride with pentaerythritol to obtain pentaerythritol diphosphonate dichloride; and (2) dissolving the pentaerythritol diphosphonate dichloride obtained in the step (1) into dimethylfomamide to obtain a solution A, dropwise adding ethylenediamine into the solution A, raising the temperature to 150-155 DEG C, reacting for 2-4 hours, cooling, filtering, washing and drying to obtain the pentaerythritol diphosphonate dichloride ethylenediamine macromolecular flame retardant. The macromolecular flame retardant is synthesized by introducing nitrogen, phosphorus and carbon elements into the same macromolecular structure, so that the stability and the macromolecular compatibility of the flame retardant are improved.

Description

technical field [0001] The present invention relates to a flame retardant and a preparation method thereof, in particular to a halogen-free flame retardant, in particular to a "trinity" macromolecular intumescent flame retardant integrating carbon source, acid source and gas source . Background technique [0002] Among the existing flame retardants, the traditional halogenated flame retardants have the advantages of high flame retardant efficiency and little impact on the basic properties of materials, but they will produce a lot of smoke and dust, corrosive gases and some toxic gases during thermal decomposition and combustion. substances, seriously endangering human health and polluting the environment. Therefore, halogenated flame retardants are gradually being replaced by halogen-free green flame retardants. Intumescent Flame Retardant (IFR for short) is a kind of flame retardant with carbon, nitrogen and phosphorus as the core components, because it is halogen-free, l...

Claims

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Application Information

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IPC IPC(8): C08G79/02C08G79/04C08L85/02
Inventor 董延茂吉凤成鲍治宇
Owner SUZHOU UNIV OF SCI & TECH
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