CN101574659A - Catalyst for using coal tar to prepare clean fuel oil by catalytic hydrogenation, preparation method and applications - Google Patents
Catalyst for using coal tar to prepare clean fuel oil by catalytic hydrogenation, preparation method and applications Download PDFInfo
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- CN101574659A CN101574659A CN 200910074790 CN200910074790A CN101574659A CN 101574659 A CN101574659 A CN 101574659A CN 200910074790 CN200910074790 CN 200910074790 CN 200910074790 A CN200910074790 A CN 200910074790A CN 101574659 A CN101574659 A CN 101574659A
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Abstract
The invention relates to a catalyst for using coal tar to prepare clean fuel oil by catalytic hydrogenation, comprising the following components in percentage by mass: 4 to 15 percent of molybdenum oxide, 3 to 9 percent of nickel oxide, 0.1 to 5 percent of cobalt oxide, 10 to 25 percent of tungsten oxide, 2.5 to 40 percent of silicon oxide and 26 to 65 percent of aluminium oxide. The preparation method of the catalyst comprises the following steps of: firstly, preparing a silicon oxide-aluminium oxide carrier, loading active components of Co, Mo, Ni and W on the carrier by an isosteric dipping method, drying, baking and forming. The catalyst can be used for the preparation of the clean fuel oil by catalytic hydrogenation of the coal tar, gasoline and diesel oil obtained from the prepared fuel oil after being separated respectively meet the national standard of 93# gasoline and 0# diesel oil.
Description
Technical field
The invention belongs to a kind of catalyst and preparation method and application, be specifically related to a kind of catalyst and preparation method and application that catalystic hydrogenation of coal tar prepares clean fuel oil that be used for.
Background technology
Along with World Economics and fast development of Chinese economy, the petroleum resources that act as a fuel are more and more nervous, and oil price is high in recent years, for the Coal Chemical Industry that is in the competition inferior position for a long time provides an opportunity to develop very rare.China is big coal country, abundant tar resource is arranged, coal tar is as the byproduct of producing blue carbon, coke and coal gasification, produce about 1,500 ten thousand tons per year at present, wherein most coal tar do not obtain reasonable use, except that the part high temperature coal-tar is used to extract the chemical products, most in/coalite tar and a small amount of high temperature coal-tar are used as fuel to carry out burning extensively.Because of containing a large amount of circulus compounds such as aromatic series in the coal tar, difficult fully burning.Coal tar phosphorus content height, hydrogen content is low, and easier generation carbon black during burning makes incomplete combustion and produces a large amount of flue dust.Owing to the content of sulphur in the coal tar and nitrogen is higher, does not carry out desulfurization removing nitric before the burning again and handle simultaneously, so give off a large amount of SOx and NOx when burning, cause serious environmental to pollute, the environmental protection energy of advocating energetically with the current whole world runs in the opposite direction.If this part coal tar is made the high fuel oil (gasoline and diesel oil) that cleans, not only can improve the value of coal tar, significantly reduce environmental pollution, can also be more than 300 hundred million yuan of the newly-increased gross national products of country.
Catalystic hydrogenation of coal tar prepares the Germany that clean fuel oil starts from twentieth century three, the forties, because reaction pressure is very high, does not realize industrialization at that time.Later decades are because also corresponding the stopping of this Study on Technology exploitation exploited in the discovery of oil with a large amount of.Enter 21st century, China's coking industry develops rapidly, produces a large amount of high temperature coal-tars and produces coalite tar among a large amount of that blue charcoal produced.Some research units attempt through removing moisture, mechanical admixture and pitch preliminary treatment, carry out the hydrocracking of deep hydrofinishing and heavy oil fraction again, process needs two kinds of catalyst, i.e. Hydrobon catalyst and hydrocracking catalyst, and processing technology more complicated.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of processing technology, only needs just coal tar to be processed into catalyst and the method for making and the application of clean fuel oil under a kind of effect of catalyst.
Catalyst quality percentage of the present invention consists of:
Molybdenum oxide 4-15%, nickel oxide 3-9%, cobalt oxide 0.1-5%, tungsten oxide 10-25%, silica 2.5-40%, aluminium oxide 26-65%.
Preparation of catalysts method of the present invention is prepared by following step:
(1), mix after silicon source and aluminium source be made into the aqueous solution respectively, regulate the pH value of mixed solution with ammoniacal liquor and react, after filtration, promptly get carrier after the washing, dry, roasting, specifically the preparation method sees CN 1184703A;
(2), take by weighing molybdenum salt, nickel salt, cobalt salt and tungsten salt and be mixed with mixed aqueous solution, adopt equi-volume impregnating to impregnated on the carrier, and in 20～120 ℃ of dryings 5～70 hours, 200～600 ℃ of roastings 3～10 hours;
(3), catalyst through and 0.3～12g binder solution mix and to pinch aftershaping, in 20～120 ℃ of dryings 5～70 hours, 300～800 ℃ of roastings 3～12 hours promptly got the producing fuel oil from coal tar catalyst.
Aforesaid vehicle group becomes alumina support or silica and alumina support, and silica alumina ratio is at silicon: aluminium=0～50: 1 scope, the specific area of carrier are 120～450m
2/ g, the aperture is 2～15nm, pore volume is 0.3～1.1ml/g.
Aforesaid silicon source can be ethyl orthosilicate, sodium metasilicate or Ludox, and the aluminium source can be sodium aluminate, aluminum nitrate or aluminum sulfate.
Aforesaid Mo salt can be one or more in nitric acid molybdenum, ammonium molybdate, sodium molybdate or the potassium molybdate.
Aforesaid Ni salt can be one or more in nickel chloride, nickel nitrate, nickelous sulfate or the citric acid nickel.
Aforesaid Co salt can be one or more in cobalt acetate, cobalt nitrate, cobalt oxalate or the cobalt carbonate.
Aforesaid W salt can be that ammonium paratungstate, wolframic acid are received, in ammonium metatungstate or the artificial schellite one or more.
Aforesaid binding agent can be Ludox, aluminium colloidal sol, sodium carboxymethylcellulose, sesbania powder or kaolin.
The shape of aforesaid catalyst can be bar shaped, sphere or cloverleaf pattern.
Application of Catalyst condition of the present invention is: carrying out presulfurization 12 hours at 150～250 ℃ before using, is raw material with coal tar then, carries out the catalytic hydrogenation reaction of coal tar, 300～500 ℃ of reaction temperatures, reaction pressure 5～15MPa, air speed 0.2～2.0h
-1, hydrogen: the volume ratio of coal tar=1200～2600: 1.
Major advantage of the present invention is:
1. the catalystic hydrogenation of coal tar catalyst that the present invention relates to has the characteristics of high activity, high selectivity and high stability.
2. the catalystic hydrogenation of coal tar catalyst that the present invention relates to can efficiently be converted into the clean fuel oil product with coal tar, and the content of sulphur and nitrogen all satisfies the standard-required of country to clean fuel oil in the product.
3. the catalystic hydrogenation of coal tar catalyst that the present invention relates to is after moving 8000 hours on the reaction unit, and catalyst performance stabilised does not have obvious deactivation phenomenom.
4. technology of the present invention is simple, strong operability, and industrialization suits to carry out.
The specific embodiment
Embodiment 1
Take by weighing 2.66g aluminum sulfate and 56.84g sodium metasilicate, be dissolved in the 50g deionized water respectively and be made into the aqueous solution, dropping ammonia equals 8 with the pH value of regulating mixed solution, 40 ℃ were reacted 1.5 hours, product after filtration then, washing, dry, 550 ℃ of roastings promptly get the silica carrier A after 5 hours, concrete preparation method sees CN 1184703A, and the specific area of carrier A is 320m
2/ g, the aperture is 6nm, pore volume is 0.7ml/g.Take by weighing 1.01g sodium molybdate, 1.75g cobalt nitrate, 1.56g nickel chloride and and the 5.34g sodium tungstate be made into mixed aqueous solution, adopt equi-volume impregnating to impregnated on the 10g carrier A, 100 ℃ of dryings 12 hours, 500 ℃ of roastings 6 hours.To have the carrier of metal oxide and 2.5g kaolin solution and 0.3g sesbania powder to mix through the load of roasting pinches, extruded moulding on banded extruder, with the roasting 5 hours in Muffle furnace after 5 hours of 120 ℃ of dryings of this bar shaped catalyst, sintering temperature is 600 ℃, comes out of the stove and promptly gets coal tar system clean fuel oil catalyst.Consisting of of final catalyst: molybdenum oxide 4%, nickel oxide 6%, cobalt oxide 3%, tungsten oxide 25%, silica 18%, aluminium oxide 44%.
Catalyst breakage to 10～20 orders are placed the stainless steel tube reactor, carried out presulfurization 12 hours in 150 ℃ before the reaction.The catalystic hydrogenation of coal tar reaction condition is: 440 ℃ of reaction temperatures, system pressure 8MPa, charging air speed 1.0h
-1, hydrogen/oil=1500.Product oil obtains gasoline and diesel oil through separating, and satisfies the standard-required (seeing attached list 1 and 2) of 93# gasoline and 0# diesel oil respectively.
Embodiment 2
Take by weighing 1.64g sodium metaaluminate and 41.7g ethyl orthosilicate, experimental procedure prepares carrier B (concrete preparation method sees CN 1184703A), the specific area 240m of carrier B with embodiment one
2/ g, aperture 15nm, pore volume 0.65ml/g.Take by weighing 1.66g ammonium molybdate, 1.75g nickel nitrate, 2.19g cobalt oxalate and 5.58g ammonium paratungstate and be made into mixed aqueous solution, adopt equi-volume impregnating to impregnated on the 10g carrier B, 20 ℃ of dryings 70 hours, 400 ℃ of roastings 10 hours.The cooling back is mixed with 5g aluminium colloidal sol and is pinched, and makes sphere on spherical make-up machine, and with the roasting in Muffle furnace after 24 hours of 80 ℃ of dryings of this spheric catalyst, sintering temperature is 300 ℃, and roasting time is 12 hours, obtains coal tar system clean fuel oil catalyst.Consisting of of final catalyst: molybdenum oxide 9%, nickel oxide 3%, cobalt oxide 5%, tungsten oxide 15%, silica 6%, aluminium oxide 62%.
Catalyst breakage to 10～20 orders are placed the stainless steel tube reactor, carried out presulfurization 12 hours in 200 ℃ before the reaction.The catalystic hydrogenation of coal tar reaction condition is: 300 ℃ of reaction temperatures, system pressure 11MPa, charging air speed 2.0h
-1, hydrogen/oil=2600.Product oil obtains specification gasoline and diesel oil (seeing attached list 1 and 2) through separating.
Embodiment 3
Take by weighing 2.5g aluminum nitrate and 20wt% Ludox 100g, prepare silica support C (concrete preparation method sees CN 1184703A), the specific area 450m of support C by embodiment one test procedure
2/ g, aperture 2nm, pore volume 0.3ml/g.Take by weighing 6.93g nitric acid molybdenum, 0.03g cobalt carbonate, 2.37g nickelous sulfate and 3.88g ammonium metatungstate and be made into mixed aqueous solution, adopt equi-volume impregnating to impregnated on the 10g support C, 120 ℃ of dryings 8 hours, 500 ℃ of roastings 3.5 hours.Cooling back is mixed with the 8g carboxymethylcellulose sodium solution and is pinched, and is extruded into bar shaped on the bar shaped make-up machine, with 120 ℃ of dryings of this bar shaped catalyst after 5 hours in 800 ℃ of roastings 3 hours, obtain coal tar system clean fuel oil catalyst.Consisting of of final catalyst: molybdenum oxide 15%, nickel oxide 4.5%, cobalt oxide 0.1%, tungsten oxide 13.7%, silica 40%, aluminium oxide 26.7%.
Catalyst breakage to 10～20 orders are placed the stainless steel tube reactor, carry out presulfurization in 210 ℃ before the reaction.The catalystic hydrogenation of coal tar reaction condition is: 500 ℃ of reaction temperatures, system pressure 5MPa, charging air speed 0.2h
-1, hydrogen/oil=1200.Product oil satisfies national standard (seeing attached list 1 and 2) through check.
Embodiment 4
Take by weighing the 75g aluminum nitrate and 18.97g carbonic hydroammonium is made into the aqueous solution respectively, prepare carrier D (concrete preparation method sees CN 1184703A), carrier D specific area 120m by embodiment one test procedure
2/ g, aperture 13.6nm, pore volume 1.1ml/g.
Take by weighing 4.1g potassium molybdate, 5.25g nickel nitrate, 0.75g cobalt acetate and 1.86g artificial schellite and be made into mixed aqueous solution, adopt equi-volume impregnating to impregnated on the 10g carrier D, 60 ℃ of dryings 60 hours, 300 ℃ of roastings 10 hours.Cooling back is mixed with the 9g Ludox and is pinched, and is extruded into cloverleaf pattern on make-up machine, with 80 ℃ of dryings of this cloverleaf pattern catalyst after 48 hours in 400 ℃ of roastings 8 hours, obtain coal tar system clean fuel oil catalyst.Consisting of of final catalyst: molybdenum oxide 12%, nickel oxide 9%, cobalt oxide 1.5%, tungsten oxide 10%, silica 2.5%, aluminium oxide 65%.
Catalyst breakage to 10～20 orders are placed the stainless steel tube reactor, react preceding 230 ℃ and carry out presulfurization.The coal tar hydrogenating reaction condition is: 400 ℃ of reaction temperatures, system pressure 10MPa, charging air speed 0.5h
-1, hydrogen/oil=1800.Product oil separates the gasoline and the diesel product that obtain and satisfies national standard (seeing attached list 1 and 2).
Embodiment five
Take by weighing 44.4g aluminum sulfate and 100g Ludox (20wt%), prepare carrier E (concrete preparation method sees CN 1184703A), carrier E specific area 195m by embodiment one test procedure
2/ g, aperture 6.5nm, pore volume 0.5ml/g.Take by weighing 1.1g ammonium molybdate, 0.29g cobalt nitrate, 2.68g citric acid nickel and 5.37g ammonium metatungstate and be made into mixed aqueous solution, incipient impregnation on 10g carrier E, 120 ℃ of dryings 5 hours, 600 ℃ of roastings are 3 hours in Muffle furnace.Cooling back is mixed with 0.35g sesbania powder and 12g Ludox and is pinched, and makes bar shaped on make-up machine, with 100 ℃ of dryings of this bar shaped catalyst after 10 hours in 460 ℃ of roastings 7 hours, obtain coal tar system clean fuel oil catalyst.Consisting of of final catalyst: molybdenum oxide 6%, nickel oxide 7%, cobalt oxide 0.5%, tungsten oxide 19%, silica 6%, aluminium oxide 61.5%.
Catalyst breakage to 10～20 orders are placed the stainless steel tube reactor, react preceding 190 ℃ and carried out presulfurization 12 hours.The coal tar hydrogenating reaction condition is: 380 ℃ of reaction temperatures, system pressure 9MPa, charging air speed 1.5h
-1, hydrogen/oil=2000.Product oil is through verifying as specification gasoline and diesel oil (seeing attached list 1 and 2).
Claims (13)
1. the catalyst of a coal tar to prepare clean fuel oil by catalytic hydrogenation is characterized in that catalyst quality percentage consists of:
Molybdenum oxide 4-15%, nickel oxide 3-9%, cobalt oxide 0.1-5%, tungsten oxide 10-25%, silica 2.5-40%, aluminium oxide 26-65%.
2, the Preparation of catalysts method of a kind of coal tar to prepare clean fuel oil by catalytic hydrogenation as claimed in claim 1 is characterized in that comprising the steps:
(1), mix after silicon source and aluminium source be made into the aqueous solution respectively, regulate the pH value of mixed solution with ammoniacal liquor and react, after filtration, promptly get carrier after the washing, drying, roasting;
(2), take by weighing molybdenum salt, nickel salt, cobalt salt and tungsten salt and be mixed with mixed aqueous solution, adopt equi-volume impregnating to impregnated on the carrier, and in 20～120 ℃ of dryings 5～70 hours, 200～600 ℃ of roastings 3～10 hours;
(3), catalyst through and binder solution mix and to pinch aftershaping, in 20～120 ℃ of dryings 5～70 hours, 300～800 ℃ of roastings 3～12 hours promptly got the producing fuel oil from coal tar catalyst.
3, the Preparation of catalysts method of a kind of coal tar to prepare clean fuel oil by catalytic hydrogenation as claimed in claim 2, it is characterized in that described vehicle group becomes alumina support or silica and alumina support, silica alumina ratio is at silicon: aluminium=0～50: 1 scope.
4, the Preparation of catalysts method of a kind of coal tar to prepare clean fuel oil by catalytic hydrogenation as claimed in claim 2, the specific area that it is characterized in that described silica carrier is 120～450m
2/ g, the aperture is 2～15nm, pore volume is 0.3～1.1ml/g.
5, the Preparation of catalysts method of a kind of coal tar to prepare clean fuel oil by catalytic hydrogenation as claimed in claim 2 is characterized in that described silicon source is ethyl orthosilicate, sodium metasilicate or Ludox.
6, the Preparation of catalysts method of a kind of coal tar to prepare clean fuel oil by catalytic hydrogenation as claimed in claim 2 is characterized in that described aluminium source is sodium aluminate, aluminum nitrate or aluminum sulfate.
7, the Preparation of catalysts method of a kind of coal tar to prepare clean fuel oil by catalytic hydrogenation as claimed in claim 2 is characterized in that described Mo salt is one or more in nitric acid molybdenum, ammonium molybdate, sodium molybdate or the potassium molybdate.
8, the Preparation of catalysts method of a kind of coal tar to prepare clean fuel oil by catalytic hydrogenation as claimed in claim 2 is characterized in that described Ni salt is one or more in nickel chloride, nickel nitrate, nickelous sulfate or the citric acid nickel.
9,, it is characterized in that described Co salt can be one or more in cobalt acetate, cobalt nitrate, cobalt oxalate or the cobalt carbonate as the Preparation of catalysts method of a kind of coal tar to prepare clean fuel oil by catalytic hydrogenation as claimed in claim 2.
10, the Preparation of catalysts method of a kind of coal tar to prepare clean fuel oil by catalytic hydrogenation as claimed in claim 2 is characterized in that described W salt is that ammonium paratungstate, wolframic acid are received, in ammonium metatungstate or the artificial schellite one or more.
11, the Preparation of catalysts method of a kind of coal tar to prepare clean fuel oil by catalytic hydrogenation as claimed in claim 2 is characterized in that described binding agent is Ludox, aluminium colloidal sol, sodium carboxymethylcellulose, sesbania powder or kaolin.
12, the Preparation of catalysts method of a kind of coal tar to prepare clean fuel oil by catalytic hydrogenation as claimed in claim 2, the shape that it is characterized in that described catalyst is bar shaped, sphere or cloverleaf pattern.
13, the Application of Catalyst of a kind of coal tar to prepare clean fuel oil by catalytic hydrogenation as claimed in claim 1, carried out presulfurization 12 hours at 150～250 ℃ before it is characterized in that using, be raw material then with coal tar, carry out the catalytic hydrogenation reaction of coal tar, 300～500 ℃ of reaction temperatures, reaction pressure 5～15MPa, air speed 0.2～2.0h
-1, hydrogen: the volume ratio of coal tar=1200～2600: 1.
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| CN102784653A (en) * | 2012-07-31 | 2012-11-21 | 宁波市化工研究设计院有限公司 | Catalyst for producing clean fuel oil by using coal tar and preparation method of catalyst |
| CN103055881A (en) * | 2012-08-27 | 2013-04-24 | 王小英 | Coal tar hydrofining catalyst and preparation method thereof |
| CN103418397A (en) * | 2012-05-25 | 2013-12-04 | 中国石油化工股份有限公司 | Catalyst having hydrogenation catalysis effect, preparation method and application thereof, and hydrotreatment method |
| CN103418398A (en) * | 2012-05-25 | 2013-12-04 | 中国石油化工股份有限公司 | Catalyst having hydrogenation catalysis effect, preparation method and application thereof, and hydrotreatment method |
| CN104069868A (en) * | 2014-06-17 | 2014-10-01 | 宁波市化工研究设计院有限公司 | Catalyst for coal tar all-distillate hydrocracking as well as preparation method and application method thereof |
| CN105170195A (en) * | 2015-09-14 | 2015-12-23 | 新奥科技发展有限公司 | Forming method of catalyst |
| CN106390972A (en) * | 2016-08-29 | 2017-02-15 | 王慧美 | Porous catalyst |
| CN108927204A (en) * | 2018-07-09 | 2018-12-04 | 中国科学院山西煤炭化学研究所 | The catalyst and its preparation method of coal tar hydrogenating processing distillate selective hydrogenation cracking light aromatic hydrocarbons and application |
| CN110935453A (en) * | 2019-12-16 | 2020-03-31 | 山东科技大学 | Dolomite catalyst without noble metal and its prepn and use |
| CN111054447A (en) * | 2019-11-29 | 2020-04-24 | 山西永东化工股份有限公司 | Catalyst capable of purifying and condensing catalytic cracking of coal tar and application thereof |
| CN113522300A (en) * | 2020-04-20 | 2021-10-22 | 广元市天森煤化有限公司 | Catalyst for preparing fuel oil from coal tar and preparation method thereof |
| CN115254119A (en) * | 2021-04-29 | 2022-11-01 | 中国石油化工股份有限公司 | Coal tar hydrogenation catalyst, and preparation method and application thereof |
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| CN103418397B (en) * | 2012-05-25 | 2015-08-26 | 中国石油化工股份有限公司 | There is the Catalysts and its preparation method of hydrogenation catalyst effect and application and hydrotreating method |
| CN103418398B (en) * | 2012-05-25 | 2016-01-13 | 中国石油化工股份有限公司 | There is the Catalysts and its preparation method of hydrogenation catalyst effect and application and hydrotreating method |
| CN103418397A (en) * | 2012-05-25 | 2013-12-04 | 中国石油化工股份有限公司 | Catalyst having hydrogenation catalysis effect, preparation method and application thereof, and hydrotreatment method |
| CN103418398A (en) * | 2012-05-25 | 2013-12-04 | 中国石油化工股份有限公司 | Catalyst having hydrogenation catalysis effect, preparation method and application thereof, and hydrotreatment method |
| CN102784653B (en) * | 2012-07-31 | 2014-06-04 | 宁波市化工研究设计院有限公司 | Catalyst for producing clean fuel oil by using coal tar and preparation method of catalyst |
| CN102784653A (en) * | 2012-07-31 | 2012-11-21 | 宁波市化工研究设计院有限公司 | Catalyst for producing clean fuel oil by using coal tar and preparation method of catalyst |
| CN103055881A (en) * | 2012-08-27 | 2013-04-24 | 王小英 | Coal tar hydrofining catalyst and preparation method thereof |
| CN104069868A (en) * | 2014-06-17 | 2014-10-01 | 宁波市化工研究设计院有限公司 | Catalyst for coal tar all-distillate hydrocracking as well as preparation method and application method thereof |
| CN105170195A (en) * | 2015-09-14 | 2015-12-23 | 新奥科技发展有限公司 | Forming method of catalyst |
| CN106390972A (en) * | 2016-08-29 | 2017-02-15 | 王慧美 | Porous catalyst |
| CN108927204A (en) * | 2018-07-09 | 2018-12-04 | 中国科学院山西煤炭化学研究所 | The catalyst and its preparation method of coal tar hydrogenating processing distillate selective hydrogenation cracking light aromatic hydrocarbons and application |
| CN111054447A (en) * | 2019-11-29 | 2020-04-24 | 山西永东化工股份有限公司 | Catalyst capable of purifying and condensing catalytic cracking of coal tar and application thereof |
| CN110935453A (en) * | 2019-12-16 | 2020-03-31 | 山东科技大学 | Dolomite catalyst without noble metal and its prepn and use |
| CN113522300A (en) * | 2020-04-20 | 2021-10-22 | 广元市天森煤化有限公司 | Catalyst for preparing fuel oil from coal tar and preparation method thereof |
| CN115254119A (en) * | 2021-04-29 | 2022-11-01 | 中国石油化工股份有限公司 | Coal tar hydrogenation catalyst, and preparation method and application thereof |
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Open date: 20091111 |