CN105964294A - Hydrogenation catalyst composition and preparation method thereof - Google Patents
Hydrogenation catalyst composition and preparation method thereof Download PDFInfo
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- CN105964294A CN105964294A CN201610348740.3A CN201610348740A CN105964294A CN 105964294 A CN105964294 A CN 105964294A CN 201610348740 A CN201610348740 A CN 201610348740A CN 105964294 A CN105964294 A CN 105964294A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/005—Mixtures of molecular sieves comprising at least one molecular sieve which is not an aluminosilicate zeolite, e.g. from groups B01J29/03 - B01J29/049 or B01J29/82 - B01J29/89
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/08—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y
- B01J29/10—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y containing iron group metals, noble metals or copper
- B01J29/106—Y-type faujasite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
- B01J29/76—Iron group metals or copper
- B01J29/7615—Zeolite Beta
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/82—Phosphates
- B01J29/84—Aluminophosphates containing other elements, e.g. metals, boron
- B01J29/85—Silicoaluminophosphates (SAPO compounds)
Abstract
The invention discloses a hydrogenation catalyst composition and a preparation method thereof. The hydrogenation catalyst composition consists of the following substances in parts by weight: 30 parts of amorphous silicon-aluminum, 40 parts of molecular sieve, 12 parts of magnesium oxide, 15 parts of diboron trioxide, 20 parts of iron trioxide, 25 parts of nano zinc oxide particles and 8 parts of calcium oxide. The hydrogenation catalyst composition provided by the technical scheme can be adopted to effectively regulate a hydrogenation function and an acidic function, is high in raw material conversion rate, is good in stability, is high in activity, further can effectively prevent active component crystal grains from growing in a reaction process of the catalyst, is long in service life, has relatively great pore volume and specific surface area, is strong in capacity of treating macromolecules in heavy oil, can be used for a single-section hydrogenation cracking process without a refining section, and also can be used for a one-section series-connected hydrogenation cracking process with a refining section.
Description
Technical field
The invention belongs to oil product processing technique field, concretely relate to a kind of hydrogenating catalyst composition and preparation thereof
Method.
Background technology
Hydrocracking technology is one of important means of crude oil secondary operations, heavy oil lighting.Fit owing to it has raw material
Ying Xingqiang, production operation and products scheme flexibly and the feature such as good product quality, have become production high-quality lightweight cleaning the most
Oil product and the important channel in solution industrial chemicals source.
Hydrocracking catalyst is usually bifunctional catalyst, and its lytic activity and hydrogenation activity are by the acid in catalyst
Property component and hydrogenation active component provide respectively.Acidic components in catalyst are usually by molecule contained in catalyst
The refractory inorganic oxides of sieve and/or composition carrier provides.Refractory inorganic oxides generally comprises amorphous silica-alumina, nothing
One or more in setting aluminium oxide.
The conjugation between molecular sieve and refractory inorganic oxides and dispersion in carrier react and have between performance
The relation of interwoveness, affect the activity of catalyst and the selectivity to various purpose products to a great extent.Right
For hydrocracking catalyst, between cracking function and hydrogenating function, the difference of coupling can produce different reaction effects,
That is for different purpose products, need to regulate cracking function and the hydrogenating function of catalyst.Existing hydrogenation catalyst is deposited
In less stable, service life is short, and pore volume and surface area are little, processes in heavy oil the shortcomings such as macromole ability.
Summary of the invention
The technical problem to be solved in the present invention is to provide one can effectively regulate hydrogenation for the deficiencies in the prior art
Function and acid function, feed stock conversion is high, good stability, and activity is high, it is also possible to be effectively prevented catalyst in course of reaction
In the growing up of active component crystal grain, service life is long, has large hole and holds and specific surface area, processes the energy of macromole in heavy oil
Power is strong, can be used for the single-stage hydrocracking technique without refining stage it can also be used to there is the one-stage serial hydrocracking technique of refining stage
Hydrogenating catalyst composition.
Present invention also offers the preparation method of a kind of above-mentioned catalyst, it is easy to operation, the prices of raw materials are cheap, preparation
Process is discharged without NOx, can meet cleaning and prepare catalyst requirement, and continuously, the response time is short, low cost, suitable work in reaction
Industry is applied.
For solving the above-mentioned technical problem present invention by the following technical solutions: a kind of hydrogenating catalyst composition, by following
The material composition of weight portion, amorphous silica-alumina 30 parts, 40 parts of molecular sieve, magnesium oxide 12 parts, diboron trioxide 15 parts, three oxidations two
Ferrum 20 parts, nano granular of zinc oxide 25 parts, calcium oxide 8 parts.
The following is further improvement of the present invention:
Described molecular sieve is the mixture of SAPO-11 molecular sieve, beta-zeolite molecular sieve and Y type molecular sieve, and described SAPO-11 divides
The mass ratio of son sieve, beta-zeolite molecular sieve and Y type molecular sieve is 3:2:1.
Improve further:
The relative crystallinity of described SAPO-11 molecular sieve is 98%, and crystal particle diameter is 2.5 μm.
Improve further:
The relative crystallinity 95%～110% of described Y type molecular sieve, crystal particle diameter is 1.8 μm.
Improve further:
The particle diameter of described nano granular of zinc oxide is 100-20nm, a length of 80-30nm.
Improve further:
Described amorphous silica-alumina silicon oxide-containing 8wt%-50wt%, specific surface area is 700-800m2/ g, pore volume is 1.6-
1.8ml/g, bore dia 8-15nm, shared pore volume accounts for the 95%-98% of total pore volume, and infrared total acid content is 0.30-
0.45mmol/g, middle strong acid amount/infrared total acid content is 0.56-0.81, and L acid amount/B acid amount is 1.40-2.30.
The preparation method of a kind of hydrogenating catalyst composition, comprises the steps:
1), amorphous silica-alumina, the molecular sieve of above-mentioned weight portion are sufficiently mixed in kneading machine, add acetic acid and β-carboxyethyl
Crylic acid ester mixture acid solution carries out peptization, is extruded into a diameter of 0.5mm column type, is then dried 2 hours at 300 DEG C,
Roasting 2 hours at 800 DEG C, prepare the catalyst carrier of molding；
2), by magnesium oxide 12 parts, diboron trioxide 15 parts, iron sesquioxide 20 parts, nano granular of zinc oxide 25 parts, calcium oxide 8
Part mix homogeneously, sends in calcining furnace, and at 1500-2000 DEG C, roasting obtains granule in 4-6 hour；
3), by above-mentioned granule incorporate in the zinc nitrate solution that concentration is 0.5mol/L, prepare metallic compound mixed solution；
4) in above-mentioned metallic compound mixed solution, by said catalyst carrier carry out dip operation, time 50min, then
It is dried；
5), dried material concentration be that the ammonia of 8mol/L carries out impregnation process, ammonia volume is that dried material is inhaled
The 90% of water rate, is dried and roasting the most again, obtains final catalyst.
Improve further:
In step 4), baking temperature is 150 DEG C, 6 hours drying times.
Improve further:
In step 5), sintering temperature is 450 DEG C, and roasting time is 3 hours.
Improve further:
Acetic acid concentration described in step 1) is 6mol/L.
The present invention uses the hydrogenating catalyst composition of technique scheme, can effectively regulate hydrogenating function and acid
Sexual function, feed stock conversion is high, good stability, and activity is high, it is also possible to be effectively prevented catalyst activity in course of reaction
Growing up of component crystal grain, service life is long, has large hole and holds and specific surface area, processes the ability of macromole in heavy oil strong, can
For without the single-stage hydrocracking technique of refining stage it can also be used to there is the one-stage serial hydrocracking technique of refining stage.The present invention
Using above-mentioned preparation method easily operated, the prices of raw materials are cheap, and preparation process is discharged without NOx, can meet cleaning preparation
Catalyst requirement, continuously, the response time is short, low cost in reaction, and Suitable commercial is applied.
Detailed description of the invention
Embodiment, a kind of hydrogenating catalyst composition, it is made up of the material of following weight portion, amorphous silica-alumina 30 parts, molecular sieve
40 parts, magnesium oxide 12 parts, diboron trioxide 15 parts, iron sesquioxide 20 parts, nano granular of zinc oxide 25 parts, calcium oxide 8 parts.
Described molecular sieve is the mixture of SAPO-11 molecular sieve, beta-zeolite molecular sieve and Y type molecular sieve, described SAPO-
The mass ratio of 11 molecular sieves, beta-zeolite molecular sieve and Y type molecular sieve is 3:2:1.
The relative crystallinity of described SAPO-11 molecular sieve is 98%, and crystal particle diameter is 2.5 μm.
The relative crystallinity 95%～110% of described Y type molecular sieve, crystal particle diameter is 1.8 μm.
The particle diameter of described nano granular of zinc oxide is 100-20nm, a length of 80-30nm.
Described amorphous silica-alumina silicon oxide-containing 8wt%-50wt%, specific surface area is 700-800m2/ g, pore volume is
1.6-1.8ml/g, bore dia 8-15nm, shared pore volume accounts for the 95%-98% of total pore volume, and infrared total acid content is 0.30
-0.45mmol/g, middle strong acid amount/infrared total acid content is 0.56-0.81, and L acid amount/B acid amount is 1.40-2.30.
The preparation method of amorphous silica-alumina described above is as follows:
A, respectively preparation sodium aluminate solution and sodium silicate solution；
B, by sodium aluminate solution adds part or all of sodium silicate solution, then pass to CO2Gas, controlling reaction temperature is
10-40 DEG C, the pH value controlling cemented into bundles is 8-11；Wherein as the CO being passed through2 Gas flow accounts for total intake
40%～100%, add excess silicon acid sodium solution；
C, at the control temperature and pH value of step b, the mixture of step b gained ventilates and stablizes 40-60 minute；
D, the solidliquid mixture of step c gained is filtered, Cake Wash；
E, the filter cake of step d gained is pulled an oar, then carry out hydrothermal treatment consists, through filtering, being dried, obtain amorphous silica-alumina；Institute
The hydrothermal conditions stated is as follows: at 120～150 DEG C, processes 2～5 under 0.5～4.0MPa water vapor pressure
Hour.
In step b, as the CO being passed through2When gas flow accounts for the 50%-80% of total intake, add residue
Sodium silicate solution.
In described step a, the concentration of sodium aluminate solution is 15-55g Al2O3/ l, sodium silicate solution dense
Degree is 50-200g SiO2/l。
Step b adds all or part of sodium silicate solution, is whole sodium silicate solutions of being added
5wt%-100wt%.
Described CO2The concentration of gas is 30v%-60v%.
The detailed process of step b uses one of following methods: after (1) adds whole sodium silicate in sodium aluminate, be passed through
CO2Gas；(2), after adding part sodium silicate in sodium aluminate, it is passed through whole CO2Gas, then adds in mixture
Excess silicon acid sodium solution；(3), after adding part sodium silicate in sodium aluminate, it is passed through part CO2Gas, more logical CO2
Gas is while adding excess silicon acid sodium solution.
Washing described in step d is that 50-90 DEG C of deionized water of filter cake is washed till neutrality.
Making beating described in step e is to be 8:1-10:1 by solid-liquid volume ratio, and add water in filter cake making beating.
Drying condition described in step e is as follows: dry 6-8 hour at 110-130 DEG C.
The preparation method of above-mentioned Y type molecular sieve includes following process: fresh NaY Crystallization of Zeolite serosity is filtering
Rinsing molecular sieve filter cake with the alkali liquor of molecular sieve butt quality 4-6 times during separation, concentration of lye is 0.001-0.5mol/L, alkali
Liquid temp is 30-90 DEG C；Then above-mentioned NaY molecular sieve filter cake is pulled an oar, adds the compound solution containing H+ ion,
The pH value making NaY molecular sieve pulp is maintained at 2.5-7.0, and reaction temperature is 5-100 DEG C, exchange reaction 0.2-6
Hour, swap with the sodium in zeolite with H+, after H+ exchange, have filtration, washing, roasting process.
The preparation method of above-mentioned nano granular of zinc oxide is as follows:
1, in round-bottomed flask, first add methanol, sequentially add potassium hydroxide and two acetate hydrate zinc, electromagnetic agitation 1-5
Minute, obtain water white solution；
2, then stir 40 hours heating-up temperature 80 DEG C, being heated at reflux in device of circulating water temperature 15 DEG C, obtain milky
Solution；
3, outwell the supernatant after the milky white solution obtained being stood 4-8 hour, separate 3-5 with methanol cleaning, centrifuge
Secondary, finally granule is dried in vacuum drying oven, obtains nano granular of zinc oxide.
The mass concentration of described potassium hydroxide is not less than 85%.
The mass concentration of described two acetate hydrate zinc is not less than 99%.
The volumetric concentration of described methanol solution is not less than 99.5%.
Described baking temperature is 20-30 DEG C, and the time is 24-96 hour.
The preparation method of described SAPO-11 molecular sieve is as follows, is mixed with deionized water by the raw material phosphoric acid of 90% aqueous solution
After stir, under agitation add boehmite, add containing SiO after stirring2It is the Ludox of 25%, stirs
After mixing reaction plastic, the most again diethylamine solution and hydrofluoric acid solution are slowly added in above-mentioned gel, continue stirring and make
Gel reaction mixture；Above-mentioned reactant mixture is loaded in the crystallizing kettle with polytetrafluoroethylene bushing, spontaneous in 160 DEG C
Crystallization 48 hours under pressure, are finally washed with deionized crystallization product, filter, and dry in 100 DEG C of air, prepare
SAPO-11 molecular sieve, relative crystallinity is 98%.
The preparation method of a kind of hydrogenating catalyst composition, comprises the steps:
1), amorphous silica-alumina, the molecular sieve of above-mentioned weight portion are sufficiently mixed in kneading machine, add acetic acid and β-carboxyethyl
Crylic acid ester mixture acid solution carries out peptization, is extruded into a diameter of 0.5mm column type, is then dried 2 hours at 300 DEG C,
Roasting 2 hours at 800 DEG C, prepare the catalyst carrier of molding.
2), by magnesium oxide 12 parts, diboron trioxide 15 parts, iron sesquioxide 20 parts, nano granular of zinc oxide 25 parts, oxygen
Changing 8 parts of mix homogeneously of calcium, send in calcining furnace, at 1500-2000 DEG C, roasting obtains granule in 4-6 hour；
3), by above-mentioned granule incorporate in the zinc nitrate solution that concentration is 0.5mol/L, prepare metallic compound mixed solution.
4), said catalyst carrier is carried out dip operation, time in above-mentioned metallic compound mixed solution
50min, is then dried.
5), dried material concentration be that the ammonia of 8mol/L carries out impregnation process, ammonia volume is dried thing
The 90% of material water absorption rate, is dried and roasting the most again, obtains final catalyst.
In step 4), baking temperature is 150 DEG C, 6 hours drying times.
Step 5) roasting is roasting 3 hours at 450 DEG C.
Acetic acid concentration described in step 1) is 6mol/L.
Claims (10)
1. a hydrogenating catalyst composition, it is characterised in that: it is made up of the material of following weight portion, amorphous silica-alumina 30 parts,
40 parts of molecular sieve, magnesium oxide 12 parts, diboron trioxide 15 parts, iron sesquioxide 20 parts, nano granular of zinc oxide 25 parts, calcium oxide
8 parts.
Hydrogenating catalyst composition the most according to claim 1, it is characterised in that: described molecular sieve is SAPO-11 molecule
Sieve, beta-zeolite molecular sieve and the mixture of Y type molecular sieve, described SAPO-11 molecular sieve, beta-zeolite molecular sieve and Y type molecular sieve
Mass ratio be 3:2:1.
Hydrogenating catalyst composition the most according to claim 2, it is characterised in that: described SAPO-11 molecular sieve relative
Degree of crystallinity is 98%, and crystal particle diameter is 2.5 μm.
Hydrogenating catalyst composition the most according to claim 2, it is characterised in that: the relative crystallization of described Y type molecular sieve
Degree 95%～110%, crystal particle diameter is 1.8 μm.
Hydrogenating catalyst composition the most according to claim 1, it is characterised in that: the particle diameter of described nano granular of zinc oxide
For 100-20nm, a length of 80-30nm.
Hydrogenating catalyst composition the most according to claim 1, it is characterised in that: described amorphous silica-alumina silicon oxide-containing
8wt%-50wt%, specific surface area is 700-800m2/ g, pore volume is 1.6-1.8ml/g, and bore dia 8-15nm is shared
Pore volume account for the 95%-98% of total pore volume, infrared total acid content is 0.30-0.45mmol/g, and middle strong acid amount/infrared is always
Acid amount is 0.56-0.81, and L acid amount/B acid amount is 1.40-2.30.
7. the preparation method of a hydrogenating catalyst composition, it is characterised in that: comprise the steps:
1), amorphous silica-alumina, the molecular sieve of above-mentioned weight portion are sufficiently mixed in kneading machine, add acetic acid and β-carboxyethyl
Crylic acid ester mixture acid solution carries out peptization, is extruded into a diameter of 0.5mm column type, is then dried 2 hours at 300 DEG C,
Roasting 2 hours at 800 DEG C, prepare the catalyst carrier of molding；
2), by magnesium oxide 12 parts, diboron trioxide 15 parts, iron sesquioxide 20 parts, nano granular of zinc oxide 25 parts, calcium oxide 8
Part mix homogeneously, sends in calcining furnace, and at 1500-2000 DEG C, roasting obtains granule in 4-6 hour；
3), by above-mentioned granule incorporate in the zinc nitrate solution that concentration is 0.5mol/L, prepare metallic compound mixed solution；
4) in above-mentioned metallic compound mixed solution, by said catalyst carrier carry out dip operation, time 50min, then
It is dried；
5), dried material concentration be that the ammonia of 8mol/L carries out impregnation process, ammonia volume is that dried material is inhaled
The 90% of water rate, is dried and roasting the most again, obtains final catalyst.
The preparation method of hydrogenating catalyst composition the most according to claim 7, it is characterised in that: in step 4), it is dried
Temperature is 150 DEG C, 6 hours drying times.
The preparation method of hydrogenating catalyst composition the most according to claim 7, it is characterised in that: in step 5), roasting
Temperature is 450 DEG C, and roasting time is 3 hours.
The preparation method of hydrogenating catalyst composition the most according to claim 7, it is characterised in that: in step 1), described
Acetic acid concentration is 6mol/L.
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| CN107876085A (en) * | 2017-11-15 | 2018-04-06 | 昌邑市瑞海生物科技有限公司 | A kind of preparation method of the special-purpose catalyst of synthesizing acetonitrile |
| CN107970952A (en) * | 2017-11-24 | 2018-05-01 | 福州大学 | A kind of inferior heavy oil hydrocracking catalyst for suspension bed and preparation method |
| CN109701460A (en) * | 2017-10-26 | 2019-05-03 | 中国石油化工股份有限公司 | The method and system of the online circular regeneration of hydrocracking catalyst |
| CN109865522A (en) * | 2017-12-03 | 2019-06-11 | 潍坊双丰化工有限公司 | A kind of brominated Polystyrene catalyst for preparing |
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| CN107876085A (en) * | 2017-11-15 | 2018-04-06 | 昌邑市瑞海生物科技有限公司 | A kind of preparation method of the special-purpose catalyst of synthesizing acetonitrile |
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| CN109865522A (en) * | 2017-12-03 | 2019-06-11 | 潍坊双丰化工有限公司 | A kind of brominated Polystyrene catalyst for preparing |
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