Metal type crosslinking auxiliary agent, its production method and resin composition containing it
A technology of resin composition and metal type, which is applied in the field of resin composition and novel metal type crosslinking auxiliary agent, can solve the problems that cannot be used to improve the crosslinking efficiency of polyvinyl chloride, and does not contain it, so as to improve the mechanical properties, The effect of improving cross-linking efficiency
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Embodiment 1
[0079] Use a 500ml four-necked flask equipped with a mechanical stirrer with a shaft seal, a thermometer, a feeding funnel and a Dean-Stark receiver, and put 177 grams of toluene and zinc oxide (45.00 grams, 0.553 moles) in the reaction flask, and heat and stir until the inside When the temperature is 50±5°C, acrylic acid (81.64 g, 1.133 mol) is slowly added dropwise from the addition funnel. After the addition is complete, the reaction is continued at this temperature for 2 hours to obtain the first mixture. The acrylic acid was purchased from China Taiwan Plastics Industry Co., Ltd. and contained 200±20 ppm of hydroquinone monomethyl ether.
[0080] After the first mixture was distilled under reduced pressure to remove the water (about 9.95 g) produced by the aforementioned reaction, the 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide ( 35.2 g, 0.163 mol) was added to the first mixture, and after uniform stirring for 1 hour, a second mixture was obtained.
[0081] Toluene was...
Embodiment 2
[0085] In this embodiment, the metal-type crosslinking auxiliary agent is prepared by the method as described in the foregoing embodiment 1. The difference is that: in the embodiment 2, the first mixture is distilled under reduced pressure to remove the production of the foregoing reaction. After the water and return to normal pressure, add 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (99.2 g, 0.459 mol) to the first mixture, and stir evenly After 1 hour, a second mixture was obtained.
[0086] After drying and disintegrating, 202.5 grams of white powdery product (theoretical weight 214.0 grams, yield 94.6%) is obtained. The phosphorus content of the white powdery product is calculated to be 6.64%; the melting point is about 72°C to 157°C; 1 H-NMR (400MHz, CDCl 3 +d 6 DMSO) is δ7.86-7.75(m), 7.59(t, J=7.4Hz), 7.39(m), 7.28-7.21(m), 7.16-7.05(m), 6.23(d, J=17.2Hz) ,5.99(dd,J=16.8Hz,J=10.6Hz), 5.65(d,J=9.6Hz), 2.48-2.45(br.), 2.24(br.); 31 P-NMR(202MHz, CDCl 3 +d 6 DMSO) is ...
Embodiment 3
[0090] In this example, the metal-type crosslinking auxiliary agent is prepared by the method described in the foregoing example 1, the difference is that: in example 3, the added divalent metal oxide is magnesium oxide (45.00 G, 1.117 mol), the amount of acrylic acid used was 164.8 g (2.287 mol), and the amount of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide was 56.6 g (0.262 mol).
[0091] After drying and disintegrating, 230.1 g of a white powder product (theoretical weight 246.9 g, yield 93.2%) was obtained. The calculated phosphorus content of the white powdery product is 3.34%; the melting point is about 139.4°C to 182°C; 1 H-NMR (400MHz, CDCl 3 +d 6 DMSO) is δ7.80(m), 7.14-6.74(m), 6.12(m), 5.98(m), 5.54(m), 2.22(br.s), 2.04(br.s); 31 P-NMR(202MHz, CDCl 3 +d 6 DMSO) is δ40.58,13.17(br.); FTIR is λ3400(br.),1686,1644,1558,1434,1364,1321,1276,1188,1141,1114,1097,1056,1021,987,962,837,759,679,575,489cm -1 Analytical ash value is 25.3% (calculated value 18.6%); effective ...
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Abstract
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