A method of preparing spinnable mesophase pitch by hydrogen catalysis-hydrogen treatment of coal tar pitch
A technology of mesophase pitch and coal tar pitch, which is applied in the field of coal tar pitch hydrogenation catalysis-hydrogen treatment to prepare spinnable mesophase pitch, which can solve the problems of difficult to effectively improve the molecular structure and composition of pitch, difficult to control the formation and transformation of mesophase pitch, It is difficult to avoid problems such as carbon deposition in solid catalysts, and achieve the effects of high content of mesophase, excellent spinnability, and high quality
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Embodiment 1
[0027] A method for preparing spinnable mesophase pitch by hydrogen catalysis-hydrogen supplying treatment of coal tar pitch, the steps are as follows:
[0028] (1) Add medium-temperature coal tar pitch and sublimed sulfur into the stirred reactor at a mass ratio of 100:0.1, and carry out hydrogenation on coal tar pitch at a reaction temperature of 380°C, a reaction hydrogen pressure of 1 MPa, a reaction time of 4 hours, and a stirring rate of 200 rpm. Catalytic treatment, after the reaction, vacuum distillation to remove low boiling point fractions to obtain primary hydrogenated pitch, vacuum distillation heating temperature 380 ℃, absolute pressure 0.5kPa.
[0029] (2) Put primary hydrogenated pitch and tetrahydronaphthalene into the stirred reactor at a mass ratio of 1:5, and hydrogenate the pitch at a reaction temperature of 390°C, a reaction hydrogen pressure of 0.5 MPa, a reaction time of 8 hours, and a stirring rate of 200 rpm. Catalysis-hydrogen supply synergistic trea...
Embodiment 2
[0034] A method for preparing spinnable mesophase pitch by hydrogen catalysis-hydrogen supplying treatment of coal tar pitch, the steps are as follows:
[0035] (1) Add high-temperature coal tar pitch and mercaptan into the stirred reactor at a mass ratio of 100:2, and perform hydrogenation on coal tar pitch under the conditions of reaction temperature 440°C, reaction hydrogen pressure 4MPa, reaction time 1h, stirring rate 50rpm Catalytic treatment, after the reaction, vacuum distillation to remove low boiling fractions to obtain primary hydrogenated pitch, vacuum distillation heating temperature 320 ° C, absolute pressure 1kPa.
[0036] (2) Put primary hydrogenated pitch and tetrahydronaphthalene into the stirred reactor at a mass ratio of 1:0.5, and perform hydrogenation catalysis on the pitch under the conditions of reaction temperature 450°C, reaction hydrogen pressure 6MPa, reaction time 1h, stirring rate 150rpm -Hydrogen supply synergistic treatment. After the reaction, ...
Embodiment 3
[0040] A method for preparing spinnable mesophase pitch by hydrogen catalysis-hydrogen supplying treatment of coal tar pitch, the steps are as follows:
[0041] (1) Add medium-temperature coal tar pitch and carbon disulfide into the stirred reactor at a mass ratio of 100:0.5, and conduct hydrogen catalytic treatment of coal tar pitch under the conditions of reaction temperature 400°C, reaction hydrogen pressure 2 MPa, reaction time 3 h, stirring rate 150 rpm After the reaction, the low-boiling point fraction was removed by vacuum distillation to obtain primary hydrogenated pitch. The vacuum distillation heating temperature was 360°C and the absolute pressure was 10kPa.
[0042] (2) Add primary hydrogenated pitch and decahydronaphthalene into the stirred reactor at a mass ratio of 1:3, and perform hydrogenation catalysis on the pitch at a reaction temperature of 400°C, a reaction hydrogen pressure of 3 MPa, a reaction time of 4 hours, and a stirring rate of 50 rpm. -Hydrogen su...
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