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Preparation method of mesoporous TiO2 whisker, distillate oil hydrodesulfurization catalyst and preparation method of distillate oil hydrodesulfurization catalyst

A hydrodesulfurization and catalyst technology, which is applied in chemical instruments and methods, crystal growth, and hydrocarbon oil treatment, can solve the problems of high cost of whisker preparation and low desulfurization rate of hydrodesulfurization catalyst, and achieve simple preparation conditions and processes Easy to control, conducive to industrial scale preparation, and high reactivity

Active Publication Date: 2020-01-24
PETROCHINA CO LTD
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  • Claims
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Problems solved by technology

[0007] The main purpose of the present invention is to provide a kind of mesoporous TiO 2 The preparation method of whisker, distillate oil hydrogenation desulfurization catalyst and preparation method thereof, to overcome TiO in the prior art 2 Defects such as high cost of whisker preparation and low desulfurization rate of hydrodesulfurization catalyst

Method used

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  • Preparation method of mesoporous TiO2 whisker, distillate oil hydrodesulfurization catalyst and preparation method of distillate oil hydrodesulfurization catalyst
  • Preparation method of mesoporous TiO2 whisker, distillate oil hydrodesulfurization catalyst and preparation method of distillate oil hydrodesulfurization catalyst
  • Preparation method of mesoporous TiO2 whisker, distillate oil hydrodesulfurization catalyst and preparation method of distillate oil hydrodesulfurization catalyst

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preparation example Construction

[0035] The invention discloses a mesoporous TiO 2 The preparation method of whisker, this method comprises the steps:

[0036] Step 1, add water dropwise to potassium titanate, stir, then seal and let stand for 3 to 15 days;

[0037] Step 2, disperse the substance after standing in step 1 into water, the mass ratio of the substance after standing in step 1 to water is 1:100~1:500, then add hydrochloric acid dropwise, adjust the pH value to 1~10, stir 18~48h for the first ion exchange reaction;

[0038] Step 3, sedimentation and suction filtration of the emulsion after the first ion exchange reaction, washing and drying the precipitate to obtain dititanic acid; and

[0039] Step 4, immerse the dititanic acid obtained in step 3 into KOH aqueous solution to carry out the second ion exchange reaction, the concentration of KOH aqueous solution is 5-30wt%, after standing for 2-24h, filter and dry to obtain mesoporous TiO 2 whiskers.

[0040] Specifically, the technical solution is...

Embodiment 1

[0053] Add deionized water dropwise to potassium titanate at a mass ratio of 1.5:1, stir evenly, seal and let stand for 7 days to obtain a sample; disperse the above sample into excess water to make a solid-liquid ratio of 1:300, Add hydrochloric acid dropwise to adjust the pH of the solution to 2, and stir for 24 hours to carry out ion exchange; settle the exchanged emulsion, suction filter, and dry to obtain dititanic acid; immerse dititanic acid in a 15wt% KOH aqueous solution for secondary ion exchange Exchange, stand for 12h, filter and dry to obtain mesoporous TiO 2 Whiskers, specific surface area 119m 2 / g, pore volume 0.28cm 3 / g, the most probable pore diameter is 9nm.

[0054] Pseudoboehmite and mesoporous TiO 2 The mass ratio of the whiskers is 6:1, and deionized water is added according to the solid-to-liquid ratio of 1:30, stirred and mixed, placed in an oil bath and heated to 60°C and kept at a constant temperature; slowly drop HNO 3 Adjust the pH of the syst...

Embodiment 2

[0058] Add deionized water dropwise to potassium titanate at a mass ratio of 2:1, stir evenly, seal and let stand for 3 days to obtain the sample; disperse the above sample into excess water to make the solid-liquid ratio 1:400, Add hydrochloric acid dropwise to adjust the pH of the solution to 3, and stir for 20 hours to carry out ion exchange; the exchanged emulsion is sedimented, suction filtered, and dried to obtain dititanic acid; immerse dititanic acid in a 30wt% KOH aqueous solution for secondary ion exchange Exchange, stand for 8h, filter and dry to obtain mesoporous TiO 2 Whiskers, specific surface area 121m 2 / g, pore volume 0.30cm 3 / g, the most probable pore size is 10nm.

[0059] Pseudoboehmite and mesoporous TiO 2 The mass ratio of whiskers is 9:1, and deionized water is added according to the solid-to-liquid ratio of 1:25, stirred and mixed, placed in an oil bath and heated to 90°C and kept at a constant temperature; slowly drop HNO 3 Adjust the pH of the sy...

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Abstract

The invention discloses a preparation method of a mesoporous TiO2 whisker, a distillate oil hydrodesulfurization catalyst and a preparation method of the distillate oil hydrodesulfurization catalyst.The preparation method of the mesoporous TiO2 whisker comprises the following steps: 1, dropwise adding water into potassium dititanate, performing stirring, and performing sealed standing for 3-15 days; 2, dispersing the solid after standing into water in a solid-liquid ratio of (1:100)-(1:500), dropwise adding hydrochloric acid, adjusting the pH value to 1-10, performing stirring for 18-48 hours, and performing a first ion exchange reaction; 3, performing sedimentation and suction filtration on an emulsion obtained after the ion exchange reaction, and washing and drying the obtained precipitate so as to obtain dititanic acid; and 4, immersing the obtained dititanic acid into a KOH (potassium hydroxide) aqueous solution, performing a second ion exchange reaction, allowing the obtained reaction product to stand for 2-24 hours, and performing filtering and drying, so as to obtain the mesoporous TiO2 whisker. A mesoporous TiO2 whisker / gamma-Al2O3 composite material is adopted as a substrate to support active components to prepare the distillate oil hydrodesulfurization catalyst. The catalyst disclosed by the invention is high in reaction activity, sulfur in diesel fuel of which the content of sulfur is 5000ppm can be reduced to 10ppm or lower, and the sulfur content of a product meets European VI diesel oil standards.

Description

technical field [0001] The invention relates to a catalyst for hydrodesulfurization of diesel distillate oil and a preparation method thereof, and mesoporous TiO 2 Whisker preparation method. Background technique [0002] Building a resource-saving and environment-friendly oil refining industry has become one of the major key issues to be solved urgently for the sustainable development of my country's national economy and society. Coordinated development plays a key role. In order to solve the increasingly serious air pollution problem in large and medium-sized cities caused by the rapid increase in car ownership, my country has accelerated the pace of upgrading the quality of oil products. On January 1, 2017, the National V clean diesel standard equivalent to the Euro V standard has been fully implemented; and the more stringent National VI diesel standard has been released. [0003] As crude oil becomes heavier and worse, the difficulty of processing diesel oil continues...

Claims

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Application Information

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IPC IPC(8): C30B29/16C30B29/62C30B7/14C10G45/04
CPCC10G45/04C10G2300/202C30B7/14C30B29/16C30B29/62
Inventor 宋金鹤李蒙李力成温广明岳凡李瑞峰杨祝红辛明瑞徐伟池马宝利徐铁刚张国甲张文成王丹谭明伟王刚郭金涛张全国张铁珍唐成
Owner PETROCHINA CO LTD
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