4579-03-7Relevant articles and documents
Flame-retardant medicinal preparation three hydroxy methyl phosphine cage shape phosphorous acid ester compound preparation method (by machine translation)
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Paragraph 0012; 0025-0030, (2018/03/26)
The invention relates to a preparation method for a flame retardant trishydroxymethyl phosphine caged phosphite ester compound. The structure of the compound is as shown in the following formula: FORMULA as shown in the specification; the preparation method comprises: under the protection of nitrogen gas, sufficiently and uniformly mixing equimolar trihydroxymethyl phosphine and phosphorus trichloride at a temperature lower than 0 DEG C to obtain a mixture; heating the mixture to 20 DEG C and preserving the temperature for 1 hour; then, heating the mixture to 60-80 DEG C and preserving the temperature to react for 3-6 hours; exhausting hydrogen chloride of the mixture; and purifying the mixture to obtain the product trishydroxymethyl phosphine caged phosphite ester . The compound is high in phosphor content, is excellent in flame retardant property, and is suitable for being used as the flame retardant of polyester, polyurethane, epoxy resin, unsaturated resin, polyolefin and the like. And the preparation method is one-step reaction, is simple in process, less in equipment investment, and easy to realize industrial production.
Flame retardant with the cage double-phosphorus phosphite compound of preparation method
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Paragraph 0012; 0026-0034, (2017/10/14)
The invention relates to a method for preparing a fire retardant same-cage diphosphine phosphite ester compound. Please refer to the specification for the structural formula of the compound. According to the preparing method, tris (hydroxymethyl) phosphine and triphenyl phosphite which are equimolar react for 5-10 h at a temperature between 100 DEG C and 150 DEG C under the protection of nitrogen and the action of a catalyst, and same-cage diphosphine phosphite ester is obtained through purification. The compound is a fire retardant high in phosphorus content, excellent in fire retardance, and suitable for serving as the fire retardant of materials including polyester, polyurethane, epoxy resin, unsaturated polyester resin and polyolefin. Furthermore, manufacturing technique is simple, equipment investment is low, and industrial production is facilitated.
The Synthesis of 2,6,7-Trioxa-1,4-diphosphabicyclo[2.2.2]octane Revisited: The Synthesis of 2,6,7-Triphenyl-2N,6N,7N-triaza-1,4-diphosphabicyclo[2.2.2]octane and the Synthesis of 1λ5-Phosphiranol
Kisanga, Philip,Verkade, John
, p. 114 - 117 (2007/10/03)
We report herein a reliable synthesis of P(OCH2)3P in a study aimed at understanding the factors that control its formation. We also report the serendipitous synthesis of the novel phosphiranol (CH2)2PO2H and the synthesis of P(PhNCH2)3P in good yield.
NOVEL HIGH-YIELD TRANSESTERIFICATION AND TRANSAMINATION ROUTES TO P(OCH2)3CCH3 AND P3CCH3, RESPECTIVELY
Volcko, E. J.,Verkade, J. G.
, p. 111 - 118 (2007/10/02)
High yields (93-96percent) in a one-step syntheses of CH3C(CH2OP(o-O2C6H4))3 (3), (4) and (5) are reported.Compounds 4 and 5 at 100-110o give P(OCH2)3CCH3 (2) and P(N(CH3)CH2)3CCH3 (7) in 97 and 96percent yield, respectively, plus the diphosphite (CH3)2C(CH2O)2POCH2C(CH3)2CH2OP(OCH2)2C(CH3)2 (8).Compound 8 was also characterized as its dithiophosphate derivative.Experiments designed to synthesize the adamantane-like P(OCH)3(CH2)3 (9) and P(CH2O)3P (10) in an analogous manner met with only partial success.The tris-phosphate analogue of 4 was also synthesized but it did not thermolyze to OP(OCH2)3CCH3 under the conditions used for 4 and 5 even after prolonged heating.
