Condensed polynuclear polycyclic aromatic hydrocarbon resin and preparation method thereof
A nuclear polycyclic aromatic hydrocarbon and resin technology, which is applied in the field of condensation polynuclear polycyclic aromatic hydrocarbon resin and its preparation, can solve the problems of complex preparation process, etc., and achieve the effect of simple process route, mild reaction conditions and conventional equipment
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[0026] At present, there are many main literatures on the utilization of coal liquefaction residues, but none of them involve the technology of preparing condensed polynuclear polycyclic aromatic hydrocarbons (Condensed Polynuclear Aromatics, COPNA for short) resins from coal liquefaction residues. In order to make full use of the coal direct liquefaction residue and provide a new raw material and method for the preparation of COPNA resin, the present invention provides a preparation method of condensed polynuclear polycyclic aromatic hydrocarbon resin, such as figure 1 As shown, it includes the following steps: S1, deashing the direct coal liquefaction residue to obtain direct coal liquefaction high-temperature pitch; Polynuclear polycyclic aromatic hydrocarbon resins.
[0027] By mixing the coal direct liquefaction high-temperature asphalt obtained after deashing the coal direct liquefaction residue with a cross-linking agent, and heat-treating cross-linking polymerization u...
Embodiment 1
[0043] Mix the coal direct liquefaction residue and the liquefied medium oil at a weight ratio of 1:1, raise the temperature of the mixture to 280°C at 10°C / h, stir at a constant temperature of 300r / min under 1.0MPa, and perform hot-melt extraction for 60min to obtain a hot-melt extraction mixture , the solid-liquid separation of the hot solution extraction mixture is obtained to obtain the coal direct liquefaction high-temperature bitumen. The coal direct liquefaction residue was processed by hot solution extraction, solid-liquid separation, and vacuum distillation to obtain a coal direct liquefaction high-temperature asphalt with a softening point of 115°C, a β resin content of 5wt.%, and an ash content of 0.35wt.%.
[0044] Weigh 50g of the above-mentioned coal direct liquefaction high-temperature bitumen and 5g of cross-linking agent tere-phenylenedimethanol (the amount of cross-linking agent added accounts for 10wt%) and place them in the reactor, and raise the temperature...
Embodiment 2 to 7
[0047] The operating steps of Examples 2 to 7 and Comparative Examples 1 to 2 are the same as those of Example 1, and the differences are specifically shown in Table 1. The coal direct liquefaction high-temperature bitumen in Table 1 is referred to as high-temperature bitumen for short. Examples and comparative examples are all operated under normal pressure.
[0048] Among them, the standards ASTMD3461-83 and GB / T212 were used to measure the softening point and ash content of the coal direct liquefaction modified asphalt, the standard GB / T2293-1997 was used to test the toluene insoluble matter, and the standard GB / T2292-1997 was used to test the quinoline insoluble content, the difference between toluene insoluble content and quinoline insoluble content is the β resin content. See Table 1 for details.
[0049] Table 1
[0050]
[0051]
[0052] As can be seen from Table 1, adopt technical scheme of the present invention, under the parameter condition in embodiment 3 ...
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