Preparation method of sulfurization type hydro-treatment catalyst

A hydrogenation catalyst and hydrotreating technology, used in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve problems such as toxicity, delayed start-up time, low metal utilization rate, etc., to avoid solubility. low, the effect of improving hydrogenation performance and improving utilization efficiency

Active Publication Date: 2014-05-07
CHINA PETROLEUM & CHEM CORP +1
View PDF7 Cites 8 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Conventional catalyst vulcanization methods use "in-vessel" vulcanization or "in-situ" vulcanization, that is, the catalyst in the oxidized state is first loaded into the hydrogenation reactor, and then hydrogen and sulfurizing agent are introduced into the reactor during the process of continuous heating. Pre-sulfurization, this method brings the following problems: (1) special pre-sulfurization equipment should be set up on the hydrogenation unit; (2) the vulcanizing agent added during the vulcanization process and the water and hydrogen sulfide generated by the reaction can easily cause high pressure Corrosion of reactors and related equipment, resulting in equipment damage and potential safety hazards; (3) The vulcanization process is longer, delaying the start-up time
(4) The vulcanizing agent used is flammable and toxic, and pollutes the environment during the vulcanization process; (5) The cost of pre-vulcanization in the device is relatively high
The above-mentioned methods all carry out pre-sulfurization treatment to the ready-made oxidized catalyst, so there are following deficiencies in the preparation process: the oxide MoO of hydrogenation catalyst active metal Mo, W, Co, Ni 3 、WO 3 , CoO, NiO have a strong interaction with the surface of the support, resulting in difficult and incomplete sulfidation of the active metal component, reducing the hydrogenation activity of the catalyst, and causing serious environmental pollution during the sulfidation process
The method is simple in process and high in sulfuration degree, so that the prepared sulfurized hydrogenation catalyst has high activity and selectivity, but the catalyst prepared by kneading method has poor metal dispersion uniformity and low metal utilization rate, which affects the activity and selectivity of the catalyst. product nature

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The catalyst catA involved in the present invention.

[0032] Prepare 250 ml of ammonium heptamolybdate solution (a), containing 10gMo / 100ml in the solution, prepare 100ml of 10wt% ammonium sulfide solution (b), prepare 40ml of phosphorus-containing nickel nitrate solution (c), contain 5g nickel / 100ml in the solution, The solution contains 0.5g of phosphorus / 100ml, weigh 150g of alumina dry rubber powder, add it into 1500g of water to make a slurry (d), dissolve 10g of polyethylene glycol ether in 100mL of water to form a solution (e), and mix (a) , (b) and (c) are slowly added to the slurry (d), while introducing the solution (e), stirring well. Control the temperature of the system at 65°C, react for 1 hour, filter, wash, and dry the obtained material at 100°C for 6 hours under the protection of an inert gas to obtain a catalyst intermediate. Put the catalyst intermediate into the rolling machine and mix evenly, then add 180g of adhesive made by peptizing nitric acid...

Embodiment 2

[0034] The catalyst catB involved in the present invention.

[0035] Prepare 600 ml of ammonium tetramolybdate solution (a), containing 5gMo / 100ml in the solution, prepare 200ml of 15wt% ammonium sulfide solution (b), prepare 40ml of phosphorus-containing nickel nitrate solution (c), contain 7g nickel / 100ml in the solution, The solution contains 0.4g of phosphorus / 100ml, weigh 160g of alumina dry rubber powder, add it into 1500g of water to make a slurry (d), dissolve 8g of polyoxyethylene amine in 100mL of water to form a solution (e), mix (a), Add (b) and (c) slowly to the slurry (d) while introducing solution (e), and stir well. Control the temperature of the system at 70°C, react for 1 hour, filter, wash, and dry the obtained material at 100°C for 6 hours under the protection of an inert gas to obtain a catalyst intermediate. Put the catalyst intermediate into the rolling machine and mix evenly, then add 180g of adhesive made by peptizing nitric acid and SB alumina, knead...

Embodiment 3

[0037] Catalyst catC involved in the present invention

[0038] Prepare 250 ml of ammonium metatungstate solution (a), the solution contains 10g tungsten / 100ml, prepare 100ml of 10wt% ammonium sulfide solution (b), prepare 40ml of phosphorus-containing nickel nitrate solution (c), and the solution contains 5g nickel / 100ml , the solution contains 0.5g phosphorus / 100ml, weigh 150g of alumina dry rubber powder, add it into 1500g of water to make a slurry (d), dissolve 15g of polyoxyethylene amide in 100ml of water to form a solution (e), and (a) , (b) and (c) are slowly added to the slurry (d), while introducing solution (e), and stirred evenly. Control the temperature of the system at 75°C, react for 1 hour, filter, wash, and dry the obtained material at 100°C for 6 hours under the protection of an inert gas to obtain a catalyst intermediate. Put the catalyst intermediate into the rolling machine and mix evenly, then add 180g of adhesive made by peptizing nitric acid and SB alu...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention provides a preparation method of a sulfurization type hydro-treatment catalyst. The preparation method comprises the following steps: adding water into carrier powder, pulping so as to obtain slurry (d), adding an ammonium molybdate and / or ammonium tungstate solution (a), an ammonium sulphide solution (b), and a nickel salt and / or cobalt salt solution (c) into the slurry (d) to carry out reactions, adding a surfactant at the same time, filtering, washing, and drying the reaction product in the protection of inert gas, adding an adhesive, kneading, extruding into strips, forming, drying in the protection of inert gas, and finally burning so as to obtain the sulfurization type hydro-treatment catalyst. The preparation method makes the active metal be evenly distributed on the carrier so as to generate more II type Ni(Co)Mo(W)S active phases with a higher activity; thus the catalyst has a high sulfurization degree and a high utilization rate of active metal, so that the hydrogenation performance of the catalyst is improved.

Description

technical field [0001] The invention relates to a preparation method of a sulfurized hydrotreating catalyst. Background technique [0002] Most of the metal active components of the current industrialized hydrotreating catalysts exist in the form of oxides, but in actual use, the active metal oxides on the catalyst need to be converted into sulfides. Therefore, the catalysts need to be sulfurized or Called pre-vulcanization. [0003] Conventional catalyst vulcanization methods use "in-vessel" vulcanization or "in-situ" vulcanization, that is, the catalyst in the oxidized state is first loaded into the hydrogenation reactor, and then hydrogen and sulfurizing agent are introduced into the reactor during the process of continuous heating. Pre-sulfurization, this method brings the following problems: (1) special pre-sulfurization equipment should be set up on the hydrogenation unit; (2) the vulcanizing agent added during the vulcanization process and the water and hydrogen sulf...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): B01J27/051B01J27/049C10G45/08
Inventor 孙晓艳樊宏飞王占宇
Owner CHINA PETROLEUM & CHEM CORP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products