CN106902878A - It is a kind of for gasoline, coal tar hydrorefining desulfurization, the catalyst of denitrogenation and preparation method thereof - Google Patents

It is a kind of for gasoline, coal tar hydrorefining desulfurization, the catalyst of denitrogenation and preparation method thereof Download PDF

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Publication number
CN106902878A
CN106902878A CN201710049488.0A CN201710049488A CN106902878A CN 106902878 A CN106902878 A CN 106902878A CN 201710049488 A CN201710049488 A CN 201710049488A CN 106902878 A CN106902878 A CN 106902878A
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China
Prior art keywords
catalyst
desulfurization
gasoline
coal tar
denitrogenation
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CN201710049488.0A
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Chinese (zh)
Inventor
姚光纯
徐刚强
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/14Phosphorus; Compounds thereof
    • B01J27/186Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J27/188Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
    • B01J27/19Molybdenum
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/60Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G45/00Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
    • C10G45/02Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
    • C10G45/04Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
    • C10G45/06Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof
    • C10G45/08Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof in combination with chromium, molybdenum, or tungsten metals, or compounds thereof
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/20Characteristics of the feedstock or the products
    • C10G2300/201Impurities
    • C10G2300/202Heteroatoms content, i.e. S, N, O, P

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Catalysts (AREA)

Abstract

The present invention discloses a kind of for gasoline, coal tar hydrorefining desulfurization, denitrification catalyst and preparation method thereof, including catalyst carrier and carrier loaded active material, through hole centered on described catalyst, 1~2mm of diameter it is cylindric, its voidage is 1.2~1.6 times of the real core catalyst carrier of same equivalent diameter, and active component is 0.2~0.5 times of the other structures catalyst of same equivalent diameter;The material of described catalyst carrier includes the mixture or the mixture of aluminum oxide series material and titanium oxide series material of aluminum oxide series material or aluminum oxide series material and silica series material, the active material of load contains cobalt, nickel, molybdenum, zinc, one or more in phosphorus.The voidage of the catalyst is 1.2~1.6 times of the real core catalyst carrier of same equivalent diameter, and the amount of active ingredients for being used is also 50~80% of other catalyst under same volume, and the usage amount of catalyst activity component is greatly saved, and has saved resource.

Description

It is a kind of for gasoline, coal tar hydrorefining desulfurization, the catalyst of denitrogenation and its preparation Method
Technical field
Field is manufactured the present invention relates to the catalyst used by oil refining industry, is specifically related to a kind of for gasoline, coal Hydrogenation of tar refining desulfurization, catalyst of denitrogenation and preparation method thereof.
Background technology
Also more and more strong to asking for for natural resources with the progress of human civilization, the destruction to environment is also increasingly serious, And most of resources be it is limited, it is non-renewable, therefore meet permanently effective utilization and conservation of nature ring of the mankind to resource Border is the very urgent responsibilities and obligations of owner.We must accomplish to increase income and decrease expenditure, and take exploitation new technology, improve resource profit With measures such as rates, it is intended to economize on resources and be reduced or avoided the destruction to environment, Blue Sky is left to descendants.
And oil refining industry be natural resources exploitation using and environmental pollution than more serious industry;Use is urged more at present Agent carries out the removing of pollutant, to weaken the pollution to environment;Particularly it is used for gasoline, coal tar hydrorefining desulfurization, takes off The catalyst of nitrogen, the composition of such catalyst mainly includes carrier and active material, and it is straight that carrier structure therein is mainly equivalent The bar shaped reality core body of 0.5~3mm of footpath, such as " clover " type, cylindrical type etc., the catalyst carrier technology of the series structure into It is ripe, industrialize for many years, there is its advantage, also there is its inferior position, advantage is technology maturation, simple production process;Inferior position is manufacture Catalyst buildup voidage is small, with the catalyst under the conditions of equivalent responses, required more active components.
The content of the invention
Above-mentioned deficiency of the present invention for prior art, there is provided one kind is used for gasoline, coal tar hydrorefining desulfurization, denitrogenation Catalyst, the voidage of the catalyst is 1.2~1.6 times of the real core catalyst carrier of same equivalent diameter, the work for being used Property group component is also 50~80% of other catalyst under same volume, and the use of catalyst activity component is greatly saved Amount, has saved resource.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is:One kind is for gasoline, coal tar hydrogenating essence Desulfurization processed, denitrification catalyst, including catalyst carrier and carrier loaded active material, through hole centered on described catalyst, 1~2mm's of diameter is cylindric, and its voidage is 1.2~1.6 times of the real core catalyst carrier of same equivalent diameter, active component It is 0.2~0.5 times of the other structures catalyst of same equivalent diameter;The material of described catalyst carrier includes aluminum oxide series The mixture or aluminum oxide series material and titanium oxide series material of material or aluminum oxide series material and silica series material The mixture of material, the active material of load contain one kind in cobalt (Co), nickel (Ni), molybdenum (Mo), zinc (Zn), phosphorus (P) etc. or It is various.
Described aluminum oxide series material includes but is not limited to the one of the aluminum oxide series material such as boehmite, Alumina gel Plant or various powders for mixing composition.
Described silica series material is referred to but is not limited to Ludox, and aerosil etc. is mixed for one or more The material being combined into.
The present invention also provide it is a kind of it is above-mentioned for gasoline, coal tar hydrorefining desulfurization, denitrification catalyst preparation method, Specific step includes:
(1) it is 80~100 according to weight ratio by aluminum oxide and silica series material:0~20 ratio is made into mixing Material, it is the 0.5~10% of compound weight to aid in binding agent, and it is the 35~70% of compound weight to add water, and peptizing agent is mixed The 0.5~5% of material weight is closed, pug is mixed into;
(2) using Application No. 2016109656335, entitled《A kind of miniature catalyst carrier mould, the mould Manufacture craft and method that carrier is prepared using the mould》Described mould, with reference to step (1) pug prepare it is a diameter of The catalyst carrier base substrate of the rice-shaped of 1~2mm;
(3) billet of the 2~12mm of catalyst carrier base substrate cut-out growth for preparing step (2);Then in room temperature~200 DEG C temperature environment under dry to base substrate moisture content no more than 5%;Finally by dried base substrate by kiln 450~ 1000 DEG C of temperature calcinations 5~15 hours;
(4) the supported on carriers active ingredients substances obtained in step (3):Prepare Ni-Mo-P-Zn's or Co-Mo-P-Zn Presoma constitute active component heteropoly acid mixed solution, by isometric, saturation impregnating mode step (3) carrier The above-mentioned heteropoly acid mixed solution of upper load;
(5) dried 5~30 hours at the catalyst that step (4) is obtained being positioned over into 50~200 DEG C;
(6) product for completing step (5) is calcined 5~35 hours by kiln at 350~750 DEG C, is completed catalyst and is produced Product are manufactured.
Binding agent described in step (1) of the present invention is:Methylcellulose, cellulose ether, hydroxypropyl methyl fiber, plain hydroxyl second One or more mixture in base cellulose, carboxymethylcellulose calcium, sesbania gum, gum arabic etc..
Peptizing agent described in step (1) of the present invention is the one kind in technical pure nitric acid, technical pure acetic acid, technical pure oxalic acid etc. Or more than one.
Aluminum oxide series material described in step (1) of the present invention includes but is not limited to the oxidation such as boehmite, Alumina gel One or more powder of mixing composition in aluminium series material.
Silica series material described in step (1) of the present invention is referred to but is not limited to Ludox, gas phase titanium dioxide One or more material of mixing composition such as silicon.
Ni (nickel) presoma is the other nickel nitrate of catalyst grade, nickelous carbonate or basic carbonate in above-mentioned steps (4) of the present invention Nickel;Mo (molybdenum) presoma is the other molybdenum oxide of catalyst grade, ammonium heptamolybdate or other molybdates;P (phosphorus) predecessor is net content It is 85% phosphoric acid;Co (cobalt) presoma is the other cobalt nitrate of catalyst grade, cobalt carbonate or basic cobaltous carbonate;Zn is industrial-purity zinc Salt is (such as:ZnCl2、ZnSO4、Zn(NO3)2、Zn(ClO4)2)。
The advantages of the present invention:
1. this method production catalyst void rate be equal equivalent diameter three leaves or bunge bedstraw herb shape catalyst 1.2~ 1.6 times, big voidage can provide bigger external surface area to increase the contact frequency of catalyst and reactive material, improve reaction Efficiency, by reaction complete material also can quickly escape with avoid local pyrexia make temperature of reactor rise and induction accident;
2. the use of this catalyst amount is its of same equivalent diameter in equal volume reactor in the case where use is ensured 0.5~0.8 times of the catalyst of its structure, i.e., this catalyst is loaded under same volume can save 20~50% catalyst amounts, section About catalyst amount, cost-effective considerable;
3. using this technology produce catalyst consumed in active component be only same equivalent diameter other structures be catalyzed 0.2~0.5 times of agent, the economy and social effect for economizing on resources produced is considerable.This technology is used for gasoline, and coal tar adds The chemical processing fields such as hydrogen desulfurization, denitrogenation, can be greatly saved resource, and the gasoline produced can meet the standard of state 5.
Brief description of the drawings
Mould generalized section in Fig. 1 Application No.s 2016109656335.
Formpiston in Fig. 2 Application No.s 2016109656335 overlooks figure structure schematic representation.
Former in Fig. 3 Application No.s 2016109656335 overlooks figure structure schematic representation.
Formpiston structural representation in Fig. 4 Application No.s 2016109656335.
Female mould structure schematic diagram in Fig. 5 Application No.s 2016109656335.
Specific embodiment
The present invention is described in further detail below by embodiment, but the present invention is not limited solely to following examples.
Embodiment
(1) boehmite original powder 1kg, methylcellulose 30g are taken, batch mixer batch mixing is put into the lump and is added water after 5 minutes 550g and 20g nitric acid, continues batch mixing until powder all becomes pug for this;
(2) in the pug input pressure extruder for completing step (1), by Application No. 2016109656335, invention It is entitled《A kind of miniature catalyst carrier mould, the manufacture craft of the mould and the method that carrier is prepared using the mould》Middle institute The mould extrusion molding stated;
Specifically, as shown in accompanying drawing 1-5, the miniature catalyst carrier mould in Application No. 2016109656335, the mould Tool includes formpiston 1 and former 2, and described formpiston and one end of former are laminated;Described formpiston is axially disposed some Enter mud hole 3 and large knitting needle accommodating hole 4, be plugged with described large knitting needle accommodating hole and lead mud rod 5;Described former is axially arranged some Forming hole 6, when one end of formpiston and former is laminated, described forming hole and large knitting needle accommodating hole coaxial line and described Mud rod is led through forming hole and large knitting needle accommodating hole;Described former axially inwardly sets fluted 7, institute with the end face of formpiston pressing The groove stated forms interlayer gap 8 with the end face of formpiston;Internal diameter of the described external diameter for leading mud rod less than forming hole.Using above-mentioned Structure, one end of formpiston and former is laminated, and then will be led mud rod and is inserted into forming hole from large knitting needle accommodating hole one end, and Termination protrudes from forming hole;Then the catalyst carrier pug containing active material is entered by press from mud pore pressure is entered, is entered Formed to groove and be sufficiently mixed in interlayer gap, then extruded from forming hole, obtain hollow catalyst carrier, this structure Carrier is set due to boring, can cause that catalysis area becomes big, improves catalytic efficiency, reduces cost so that material use Rate is more abundant.
(3) base substrate that step (2) is manufactured is put into 70 DEG C of baking ovens freeze-day with constant temperature 8 hours, is to base substrate moisture content 0.83%;
(4) base substrate for taking step (3) is calcined 6 hours for 580 DEG C with Muffle furnace;
(5) content according to each active component in table 1 in the catalyst, with nickel nitrate, molybdenum acid ammonia, zinc nitrate, phosphorus Mixture of multi-elements liquid medicine is prepared in acid, and active component solution is impregnated by isometric method (equi-volume process);It is specifically shown in table 1 below institute Show:
Table 1 each active component content in the catalyst
Project Grain of rice ring catalyst activity content of material Real core trifolium-shaped catalyst
7 13
Co (%) 0.8 1.5
Zn (%) 0.5 0.9
Ni (%) 0.2 0.2
P (%) 0.9 1.8
(6) product of step (5) is put to baking oven, after being dried 24 hours with 60 DEG C of temperature, then is placed in Muffle furnace 500 DEG C of temperature calcinations complete catalyst manufacture for 4 hours.
Under equal conditions, the catalyst and traditional trifolium-shaped carrier for being manufactured using this patent in unit volume use effect Fruit contrast is shown in Table 2:
The embodiment of the present invention sample of table 2 and prior art sample comparative result
Knowable to above-mentioned contrast, there is catalyst of the invention big voidage can provide bigger external surface area to increase Plus catalyst and the contact frequency of reactive material, reaction efficiency being improved, also quickly can escape to avoid by the material that reaction is completed Local pyrexia makes temperature of reactor rise and induction accident;And compared with the other structures catalyst with equivalent diameter active matter The consumption of matter is more saved, but desulfurization degree and denitrification percent are higher.

Claims (10)

1. it is a kind of for gasoline, coal tar hydrorefining desulfurization, denitrogenation catalyst, it is characterised in that:Including catalyst carrier With carrier loaded active material, through hole centered on described catalyst, 1~2mm of diameter it is cylindric, its voidage is with working as Measure the real core catalyst carrier of diameter 1.2~1.6 times, active component is the 0.2 of the other structures catalyst of same equivalent diameter ~0.5 times;The material of described catalyst carrier includes aluminum oxide series material or aluminum oxide series material and silica-based The mixture of row material or the mixture of aluminum oxide series material and titanium oxide series material, the active material of load contain cobalt, Nickel, molybdenum, zinc, one or more in phosphorus.
2. it is according to claim 1 for gasoline, coal tar hydrorefining desulfurization, denitrogenation catalyst, it is characterised in that: Described aluminum oxide series material includes but is not limited to the mixing of one or more in boehmite, Alumina gel.
3. it is according to claim 1 for gasoline, coal tar hydrorefining desulfurization, denitrogenation catalyst, it is characterised in that: Described silica series material includes but is not limited to Ludox, the mixing of one or more in aerosil.
4. it is a kind of for gasoline, coal tar hydrorefining desulfurization, the catalyst of denitrogenation preparation method, it is characterised in that:Step Including:
(1) it is 80~100 according to weight ratio by aluminum oxide and silica series material:0~20 ratio is made into compound, auxiliary It is the 0.5~10% of compound weight to help binding agent, and it is the 35~70% of compound weight to add water, and peptizing agent is compound weight The 0.5~5% of amount, mixes into pug;
(2) using Application No. 2016109656335, entitled《A kind of miniature catalyst carrier mould, the system of the mould The method made technique and carrier is prepared using the mould》Described mould, with reference to step (1) pug prepare a diameter of 1~ The catalyst carrier base substrate of the rice-shaped of 2mm;
(3) billet of the 2~12mm of catalyst carrier base substrate cut-out growth for preparing step (2);Then in room temperature~200 DEG C Dried under temperature environment being no more than 5% to base substrate moisture content;Finally by dried base substrate by 450~1000 DEG C of kiln Temperature calcination 5~15 hours;
(4) the supported on carriers active ingredients substances obtained in step (3):The forerunner for preparing Ni-Mo-P-Zn or Co-Mo-P-Zn The heteropoly acid mixed solution of the active component that body is constituted, is born by isometric, saturation impregnating mode on the carrier of step (3) Carry above-mentioned heteropoly acid mixed solution;
(5) dried 5~30 hours at the catalyst that step (4) is obtained being positioned over into 50~200 DEG C;
(6) product for completing step (5) is calcined 5~35 hours by kiln at 350~750 DEG C, completes catalyst prod system Make.
5. it is according to claim 4 for gasoline, coal tar hydrorefining desulfurization, the catalyst of denitrogenation preparation method, It is characterized in that:Binding agent described in step (1) is:Methylcellulose, cellulose ether, hydroxypropyl methyl fiber, plain ethoxy Cellulose, carboxymethylcellulose calcium, one or more in sesbania gum, gum arabic of mixture.
6. it is according to claim 4 for gasoline, coal tar hydrorefining desulfurization, the catalyst of denitrogenation preparation method, It is characterized in that:Peptizing agent described in step (1) is the one kind or two in technical pure nitric acid, technical pure acetic acid, technical pure oxalic acid More than kind.
7. it is according to claim 4 for gasoline, coal tar hydrorefining desulfurization, the catalyst of denitrogenation preparation method, It is characterized in that:Aluminum oxide series material described in step (1) include but is not limited to one kind in boehmite, Alumina gel or Various mixing.
8. it is according to claim 4 for gasoline, coal tar hydrorefining desulfurization, denitrification catalyst preparation method, its It is characterised by:Silica series material described in step (1) includes but is not limited to Ludox, the one kind in aerosil Or various mixing.
9. it is according to claim 4 for gasoline, coal tar hydrorefining desulfurization, the catalyst of denitrogenation preparation method, It is characterized in that:Ni presomas are the other nickel nitrate of catalyst grade, nickelous carbonate or basic nickel carbonate in step (4);Mo presomas For the other molybdenum oxide of catalyst grade, ammonium heptamolybdate or other molybdates;P predecessors are phosphoric acid that net content is 85%;Co forerunner Body is the other cobalt nitrate of catalyst grade, cobalt carbonate or basic cobaltous carbonate;Zn predecessors are technical pure zinc salt.
10. it is according to claim 9 for gasoline, coal tar hydrorefining desulfurization, the catalyst of denitrogenation preparation method, It is characterized in that:Described technical pure zinc salt is ZnCl2、ZnSO4、Zn(NO3)2、Zn(ClO4)2In one or two kinds of more than Mixing.
CN201710049488.0A 2017-01-23 2017-01-23 It is a kind of for gasoline, coal tar hydrorefining desulfurization, the catalyst of denitrogenation and preparation method thereof Pending CN106902878A (en)

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CN110756204A (en) * 2019-10-24 2020-02-07 西安石油大学 Preparation and catalysis method of catalyst for converting phenolic compounds in coal tar
CN113083270A (en) * 2021-04-14 2021-07-09 江苏扬农化工集团有限公司 Catalyst for synthesizing 6-aminocapronitrile from cyclohexanone oxime by one-step method and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN110756204A (en) * 2019-10-24 2020-02-07 西安石油大学 Preparation and catalysis method of catalyst for converting phenolic compounds in coal tar
CN110756204B (en) * 2019-10-24 2022-09-02 西安石油大学 Preparation and catalysis method of catalyst for converting phenolic compounds in coal tar
CN113083270A (en) * 2021-04-14 2021-07-09 江苏扬农化工集团有限公司 Catalyst for synthesizing 6-aminocapronitrile from cyclohexanone oxime by one-step method and preparation method thereof

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