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Composite structural phosphorus fire retardant containing poly-DOPO cyclic phosphate and preparation method thereof

A technology of cyclic phosphate ester and composite structure, which is applied in the field of flame retardants, can solve the problems that affect the wide use, difficult to disperse uniformly, poor compatibility, etc., and achieve the effects of good flame retardant effect, convenient use, and high flame retardant efficiency

Active Publication Date: 2017-02-22
淮安丹文化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the flame retardant has excellent performance, due to its strong molecular rigidity and poor compatibility with the flame retardant polymer matrix, it is not easy to disperse uniformly in the polymer matrix, thus affecting its wide use.

Method used

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  • Composite structural phosphorus fire retardant containing poly-DOPO cyclic phosphate and preparation method thereof
  • Composite structural phosphorus fire retardant containing poly-DOPO cyclic phosphate and preparation method thereof
  • Composite structural phosphorus fire retardant containing poly-DOPO cyclic phosphate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]Install a mechanical stirrer, h-type oil-water separator and reflux condenser, dropping funnel and nitrogen inlet on a 3-liter four-necked flask. Add 253.3 grams (1.172mol) DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), 100.6 grams p-xylene, 800 grams PXE (1,1-bis (3,4-Dimethylphenyl)ethane) solvent and 56.45 g of glycerol solution (53.9 g (0.586 mol) of glycerol dissolved in 2.55 g of sodium iodide). After the oil-water separator was filled with p-xylene, the reaction mixture was heated to 200° C. for 14 hours under the protection of nitrogen flow, and the generated water was continuously discharged through the oil-water separator during the reaction. In the later stage of the reaction, less water is produced, so the reaction temperature is increased to 205° C. for another 2 hours. After the reaction, the temperature of the system was lowered to room temperature, and 29.94 grams (0.195 mol) of phosphorus oxychloride was added dropwise through the dropping f...

Embodiment 2

[0034] According to embodiment 1 program, only wherein reactant 56.45 gram glycerol solutions are changed into 64.67 gram butanetriol solutions (62.12 gram 1.2.4-butanetriol dissolves 2.55 gram sodium iodides), other reactant and solvent consumption are the same Change. And before the dropwise addition of phosphorus oxychloride after the reaction mixture was lowered to room temperature, 150 ml of pyridine was added to the reaction flask. The reaction product is light yellow syrupy liquid, marked as P2, the yield is about 81%, and the phosphorus content is 13.98%. 1H NMR: 7.13-7.95 ppm, m, 16H (H-Ar); 2.60-2.88-ppm, m, 6H (CH2); 3.54 ppm, m, 1H (CH). 13CNMR: 119.9-150.2ppm (C-Ar); 38.8-39.3ppm (CH2); 50.1ppm (CH). 31PNMR: 37.12-37.34ppm (mixture of chiral isomers of DOPO structure); -5.8ppm ((-O-)3P(O)).

Embodiment 3

[0036] 53.13 grams (0.391mol) of pentaerythritol were dissolved in 160 milliliters of ethanol, 2.55 grams of sodium iodide was added thereto, the mixture was heated to reflux for 2 hours, and then the ethanol was gradually distilled off to obtain a reaction mixture of pentaerythritol and sodium iodide. This mixture was used to replace the glycerol solution in Example 1 as a reactant, and the other reactants and solvents were used in the same amount, and the reaction was carried out according to the procedure in Example 1. And before the dropwise addition of phosphorus oxychloride after the reaction mixture was lowered to room temperature, 150 ml of pyridine was added to the reaction flask. The product is a white solid, marked as P3, with a yield of 86% and a phosphorus content of 13.84%. 1HNMR: 7.29-8.02ppm, m, 24H(H-Ar); 2.42ppm, s, 6H(P-CH2-C); 3.89ppm, s, 2H(C-CH2-O). 13CNMR: 119.9-150.2ppm (C-Ar); 39.7ppm (CH2); 69.0ppm (CH2), -4.8ppm (tert-C). 31PNMR: 37.12-37.34ppm (mi...

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Abstract

The invention discloses a composite structural phosphorus fire retardant containing poly-DOPO cyclic phosphate and preparation method thereof; the structural formula of the composite structural phosphorus fire retardant includes not less than 1 organophosphorus ester and not less than 2 DOPO cyclic phosphates. The DOPO is mixed with polyhydroxy alkane or substituted chain hydrocarbon, wherein there are not less than 3 hydroxide radicals of polyhydroxy alkane, and not less than 3 hydroxy carbons in the substituted chain hydrocarbon; heating a mixture to 195-210 DEG C under the protection gas and reacting for 14-17 hours, cooling to room temperature; and then adding halogenated oxygen phosphor or incomplete esterified halogenated oxygen phosphor; then raising temperature to 55-65 DEG C and reacting for 1.5-3 hours; cooling to room temperature and obtaining the composite structural phosphorus fire retardant. The invention provides fire retarding effect at two decomposing temperatures, wherein the one is appeared within 230 and 310 DEG C and the other one is appeared after 345 DEG C; the composite structural phosphorus fire retardant is simple in compound, convenient to use, high in phosphorus content, and better in fire retarding effect.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a composite structure phosphorus flame retardant containing multiple DOPO cyclic phosphates and a preparation method thereof. Background technique [0002] Among the traditional flame retardants, brominated flame retardants are widely used because of their good flame retardant effect, little impact on the properties of flame retardant polymer materials, and high cost performance. However, the flame retardant has defects in environmental protection. It will produce harmful carcinogens (such as dioxin) and a large amount of harmful smoke in the flame retardant. use. Some states in the United States have also introduced similar regulations. At the same time, some multinational companies have also formulated their own environmental protection standards, and the restriction on the use of halogens is one of the important contents. In 2007, the draft standard proposed by the...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08K5/5313C08L63/02
CPCC07F9/657172C08K3/22C08K5/5313C08L2201/02C08K2003/2227C08L63/00C07F9/6574C09K21/12C07F9/65746
Inventor 刘长坤郑洪良
Owner 淮安丹文化工科技有限公司
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