CN105944754A - Light oil etherification catalyst and preparation method thereof - Google Patents
Light oil etherification catalyst and preparation method thereof Download PDFInfo
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- CN105944754A CN105944754A CN201610348737.1A CN201610348737A CN105944754A CN 105944754 A CN105944754 A CN 105944754A CN 201610348737 A CN201610348737 A CN 201610348737A CN 105944754 A CN105944754 A CN 105944754A
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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
- B01J29/80—Mixtures of different zeolites
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING 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
- C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
- C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
-
- 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
- B01J2229/186—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself not in framework positions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1037—Hydrocarbon fractions
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a light oil etherification catalyst and a preparation method thereof. The light oil etherification agent includes catalyst component A and catalyst component B having a mass ratio of 2:1; the catalyst component A comprises the following materials according to parts by weight: 30 parts of styrene solution, 20 parts of divinylbenzene solution, 10 parts of diphenol solution, 5 parts of liquid paraffin solution, 40 parts of aluminum chloride and nickel chloride mixture where aluminum chloride and nickel chloride have a mass ratio of 3:2, 50 parts of ammonia solution, 40 parts of methanol solution, and 40 parts of ammonium chloride solution; the light oil etherification catalyst using the above technical scheme is high in activity, good in low-temperature reaction cavity and mechanical strength, up to 2 years in life, continuous in reaction and short in reaction time.
Description
Technical field
The invention belongs to gasoline processing technique field, concretely relate to a kind of light oil catalyst for etherification and
Its preparation method.
Background technology
Along with the high speed development of human society, countries in the world, particularly some developed countries are increasingly paid attention to environment
Protection, the development that automobile industry is the swiftest and the most violent causes the vehicle exhaust severe contamination to air, in order to reduce this respect
Polluting, unleaded oxygen-containing and high-knock rating gasoline demand becomes increasing.
Etherification of Light FCC Gasoline technology is that the C5-C7 active olefin in catalytic cracking unit stable gasoline and methanol react raw
Become corresponding ether, thus reduce the content of alkene in gasoline.Octane number after etherified can improve 1-3 unit.
The relatively low methanol of price can be made to be the gasoline products of high added value by etherification conversion by ether-based device, improve oil plant
Economic benefit.
Current Etherification of Light FCC Gasoline Technology is catalytically cracked gasoline first to enter catalytic hydroprocessing reactive distillation column, by vapour
Diene hydrogenation removing in oil, is separated into gasoline gently simultaneously, weighs two components, and light gasoline enters with methanol through fixed bed reactors
Row etherification reaction, in light gasoline, major part Tertiary olefin is converted into ether compound, enters back into catalytic rectifying tower degree of depth etherificate.Gently
Gasoline is hydrogenated with through CDTECH technique, is etherified and skeletal isomerization, C5 Tertiary olefin etherification conversion rate ＞ 92%.
The most commonly used another kind of Etherification of Light FCC Gasoline technique is lower alcohol and the light gasoline of excess to be mixed, and first carries out
For the first time etherificate, then carries out fractional distillation, containing methanol and below C5 hydro carbons in light fraction, in heavy distillat containing ether and C5 with
Upper hydro carbons, light fraction is etherified again.Etherificate uses acidic catalyst, second time etherificate to use metal silicate catalysis for the first time
Agent, thus reduce the olefin(e) centent in gasoline, improve octane number.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of activity high for the deficiencies in the prior art, has excellent low
Temperature reactivity and mechanical strength, and service life is long, continuously, the response time is short, and unsaturated olefin will not be caused to occur in reaction
Full, have and be preferably etherified effect, activity C5 alkene total conversion can be made more than 98.5%, activity C6 alkene total conversion is big
In 70%, there is excellent heat stability, improve octane number and reduce the light oil catalyst for etherification of aromatic hydrocarbon content；
Present invention also offers the preparation method of a kind of above-mentioned catalyst, this preparation method technique is simple, low cost, Suitable commercial
Application, and there is the value in industry.
For solving the above-mentioned technical problem present invention by the following technical solutions: a kind of light oil catalyst for etherification, including urging
The mass ratio of agent component A and catalyst component B, catalyst component A and catalyst component B is 2:1；
Described catalyst component A is made up of the material of lower weight portion, styrene solution 30 parts, divinylbenzene solution 20 parts, biphenyl
The blended liquid 40 parts of two phenol solutions 10 parts, liquid paraffin solution 5 parts, aluminum chloride and Nickel dichloride., wherein aluminum chloride and Nickel dichloride.
Mass ratio is 3:2, ammonia spirit 50 parts, methanol solution 40 parts, ammonium chloride solution 40 parts；
Described catalyst component B is made up of the material of following weight portion, magnesium oxide 3 parts, diboron trioxide 8 parts, iron sesquioxide 6
Part, Zinc oxide particles 10 parts, calcium oxide 6 parts, sodium carbonate 8 parts, basic aluminum sulfate 6 parts, manganese oxide particle 10 parts, 8 parts of molecular sieve.
The following is further improvement of the present invention:
Described styrene solution concentration is 1mol/L, and the concentration of described divinylbenzene solution is 0.1mol/L.
Improve further:
The preparation method of catalyst component A is as follows:
1), above-mentioned solution is blended according to weight portion, under laser heating and stirring, generates precipitation, heating-up temperature
Control at 30-70 DEG C；
2), precipitation completely after, with deionized water cyclic washing precipitate to neutral, then at 300-500 DEG C
Under be dried 4-6 hour；
3), calcination steps, by dried precipitate at 550-600 DEG C, 2-6 hour prepared catalyst component A of roasting.
Improve further:
Described molecular sieve is ZSM-5, beta-zeolite molecular sieve, the mixture of MFI molecular sieve, and molecular sieve is that ZSM-5, β zeolite divides
Son sieve, the mass ratio of MFI molecular sieve are 1:2:3.
Improve further:
The preparation method of catalyst component B is as follows:
A, calcination process
By magnesium oxide 3 parts, diboron trioxide 8 parts, iron sesquioxide 6 parts, Zinc oxide particles 10 parts, calcium oxide 6 parts, sodium carbonate 8
Part, basic aluminum sulfate 6 parts, manganese oxide particle 10 parts, 8 parts of mix homogeneously of molecular sieve, send in calcining furnace, at 1500-2000 DEG C
Lower roasting obtains granule in 4-6 hour；
B, acidification
Being incorporated in the zinc nitrate solution that concentration is 0.5mol/L by above-mentioned granule, stir postactivated 2h, carries out at pulverizing
Reason, grinding particle size 10-100 mesh；
C, extruding, dry in the sun
Granule after pulverizing, keeps 10 minutes, continuously extruding and molding under high pressure 10-40MPa, so under low pressure 4MPa
Rear dry in the sun, moisture content≤30% of mixture after dry in the sun；
D, screening
Sieving by vibrosieve, compound particles fineness controls at 0.1-3mm.
E, roasting
Being put into by mixture after screening and carry out roasting in roaster, sintering temperature controls at 300-350 DEG C, and roasting time controls
At 1.5-2 hour, after cooling, obtain catalyst component B.
The preparation method of a kind of light oil catalyst for etherification, comprises the following steps:
A, that catalyst component A and catalyst component B puts into stirrer for mixing is uniform, adds aqueous solution of nitric acid, rolls plastic
Extruded moulding after bulk wet cake, it is dried, roasting, prepares catalyst semi-finished product；
B, by above-mentioned catalyst semi-finished product load activation device in, under the atmosphere of water flowing steam, be warming up to 800-1000 DEG C, and
Thermostatted water processes 20-30 hour prepared finished catalyst at such a temperature.
Improve further:
In step a, the concentration of aqueous solution of nitric acid is the aqueous solution of nitric acid of 0.25g/ml-0.5g/ml.
Improve further:
In step a, sintering temperature is 1500-2000 DEG C, and roasting time is 8-10 hour.
Improve further:
In step a, baking temperature is 100 DEG C, and drying time is 8 hours.
The present invention uses the light oil catalyst for etherification of technique scheme, and activity is high, has excellent low-temp reaction and lives
Property and mechanical strength, and service life was up to 2 years, and continuously, the response time is short in reaction, unsaturated olefin will not be caused to occur full,
Have and be preferably etherified effect；Activity C5 alkene total conversion can be made more than 98.5%, and activity C6 alkene total conversion is more than
70%；There is excellent heat stability；Improve octane number and reduce aromatic hydrocarbon content；The present invention uses above-mentioned preparation method,
Skill is simple, low cost, and Suitable commercial is applied, and has the value in industry.
Detailed description of the invention
Embodiment, a kind of light oil catalyst for etherification, including catalyst component A and catalyst component B, catalyst component A with urge
The mass ratio of agent component B is 2:1.
Described catalyst component A is made up of the material of lower weight portion, styrene solution 30 parts, divinylbenzene solution 20 parts,
The blended liquid 40 parts of '-biphenyl diphenol solution 10 parts, liquid paraffin solution 5 parts, aluminum chloride and Nickel dichloride., wherein aluminum chloride and chlorination
The mass ratio of nickel is 3:2, ammonia spirit 50 parts, methanol solution 40 parts；Ammonium chloride solution 40 parts.
Described styrene solution concentration is 1mol/L, and the concentration of described divinylbenzene solution is 0.1mol/L, '-biphenyl diphenol
The concentration of solution is 0.1mol/L, and the concentration of liquid paraffin solution is 12mol/L, and the concentration of aluminum chloride is 25mol/L, Nickel dichloride.
Concentration be 25mol/L, the concentration of ammonia spirit is 12mol/L, and the concentration of methanol solution is 2mol/L, ammonium chloride solution dense
Degree is 0.1mol/L.
The preparation method of catalyst component A is as follows,
2), above-mentioned solution is blended according to weight portion, under laser heating and stirring, generates precipitation, heating-up temperature
Control at 30-70 DEG C；
2), precipitation completely after, with deionized water cyclic washing precipitate to neutral, then at 300-500 DEG C
Under be dried 4-6 hour；
3), calcination steps, by dried precipitate at 550-600 DEG C, 2-6 hour prepared catalyst component A of roasting.
Described catalyst component B is made up of the material of following weight portion, magnesium oxide 3 parts, diboron trioxide 8 parts, three oxidations
Two ferrum 6 parts, Zinc oxide particles 10 parts, calcium oxide 6 parts, sodium carbonate 8 parts, basic aluminum sulfate 6 parts, manganese oxide particle 10 parts, molecule
Sieve 8 parts.
Described molecular sieve is ZSM-5, beta-zeolite molecular sieve, the mixture of MFI molecular sieve, and molecular sieve is ZSM-5, β boiling
Stone molecular sieve, the mass ratio of MFI molecular sieve are 1:2:3.
The preparation method of catalyst component B is as follows,
A, calcination process
By magnesium oxide 3 parts, diboron trioxide 8 parts, iron sesquioxide 6 parts, Zinc oxide particles 10 parts, calcium oxide 6 parts, sodium carbonate 8
Part, basic aluminum sulfate 6 parts, manganese oxide particle 10 parts, 8 parts of mix homogeneously of molecular sieve, send in calcining furnace, at 1500-2000 DEG C
Lower roasting obtains granule in 4-6 hour；
B, acidification
Being incorporated in the zinc nitrate solution that concentration is 0.5mol/L by above-mentioned granule, stir postactivated 2h, carries out at pulverizing
Reason, grinding particle size 10-100 mesh；
C, extruding, dry in the sun
Granule after pulverizing, keeps 10 minutes, continuously extruding and molding under high pressure 10-40MPa, so under low pressure 4MPa
Rear dry in the sun, moisture content≤30% of mixture after dry in the sun；
D, screening
Sieving by vibrosieve, compound particles fineness controls at 0.1-3mm.
E, roasting
Being put into by mixture after screening and carry out roasting in roaster, sintering temperature controls at 300-350 DEG C, and roasting time controls
At 1.5-2 hour, after cooling, obtain catalyst component B.
The preparation method of a kind of light oil catalyst for etherification, comprises the following steps:
B, that catalyst component A and catalyst component B puts into stirrer for mixing is uniform, adds aqueous solution of nitric acid, rolls plastic
Extruded moulding after bulk wet cake, it is dried, roasting, prepares catalyst semi-finished product；
B, by above-mentioned catalyst semi-finished product load activation device in, under the atmosphere of water flowing steam, be warming up to 800-1000 DEG C, and
Thermostatted water processes 20-30 hour prepared finished catalyst at such a temperature；
In step a, the concentration of aqueous solution of nitric acid is the aqueous solution of nitric acid of 0.25g/ml-0.5g/ml；
In step a, sintering temperature is 1500-2000 DEG C, and roasting time is 8-10 hour；
In step a, baking temperature is 100 DEG C, and drying time is 8 hours.
Claims (9)
1. a light oil catalyst for etherification, it is characterised in that: include catalyst component A and catalyst component B, catalyst component
The mass ratio of A and catalyst component B is 2:1；
Described catalyst component A is made up of the material of lower weight portion, styrene solution 30 parts, divinylbenzene solution 20 parts, biphenyl
The blended liquid 40 parts of two phenol solutions 10 parts, liquid paraffin solution 5 parts, aluminum chloride and Nickel dichloride., wherein aluminum chloride and Nickel dichloride.
Mass ratio is 3:2, ammonia spirit 50 parts, methanol solution 40 parts, ammonium chloride solution 40 parts；
Described catalyst component B is made up of the material of following weight portion, magnesium oxide 3 parts, diboron trioxide 8 parts, iron sesquioxide 6
Part, Zinc oxide particles 10 parts, calcium oxide 6 parts, sodium carbonate 8 parts, basic aluminum sulfate 6 parts, manganese oxide particle 10 parts, 8 parts of molecular sieve.
Light oil catalyst for etherification the most according to claim 1, it is characterised in that: described styrene solution concentration is
1mol/L, the concentration of described divinylbenzene solution is 0.1mol/L.
Light oil catalyst for etherification the most according to claim 1, it is characterised in that: the preparation method of catalyst component A is such as
Under:
1), being blended according to weight portion by above-mentioned solution, generate precipitation under laser heating and stirring, heating and temperature control is at 30-70
℃；
2), precipitation completely after, with deionized water cyclic washing precipitate to neutral, then at 300-500 DEG C
Under be dried 4-6 hour；
3), calcination steps, by dried precipitate at 550-600 DEG C, 2-6 hour prepared catalyst component A of roasting.
Light oil catalyst for etherification the most according to claim 1, it is characterised in that: described molecular sieve is ZSM-5, β zeolite
Molecular sieve, the mixture of MFI molecular sieve, molecular sieve is ZSM-5, the mass ratio of beta-zeolite molecular sieve, MFI molecular sieve is 1:2:
3。
Light oil catalyst for etherification the most according to claim 1, it is characterised in that: the preparation method of catalyst component B is such as
Under:
A, calcination process
By magnesium oxide 3 parts, diboron trioxide 8 parts, iron sesquioxide 6 parts, Zinc oxide particles 10 parts, calcium oxide 6 parts, sodium carbonate 8
Part, basic aluminum sulfate 6 parts, manganese oxide particle 10 parts, 8 parts of mix homogeneously of molecular sieve, send in calcining furnace, at 1500-2000 DEG C
Lower roasting obtains granule in 4-6 hour；
B, acidification
Being incorporated in the zinc nitrate solution that concentration is 0.5mol/L by above-mentioned granule, stir postactivated 2h, carries out at pulverizing
Reason, grinding particle size 10-100 mesh；
C, extruding, dry in the sun
Granule after pulverizing, keeps 10 minutes, continuously extruding and molding under high pressure 10-40MPa, so under low pressure 4MPa
Rear dry in the sun, moisture content≤30% of mixture after dry in the sun；
D, screening
Sieving by vibrosieve, compound particles fineness controls at 0.1-3mm；
E, roasting
Being put into by mixture after screening and carry out roasting in roaster, sintering temperature controls at 300-350 DEG C, and roasting time controls
At 1.5-2 hour, after cooling, obtain catalyst component B.
6. the preparation method of a light oil catalyst for etherification, it is characterised in that: comprise the following steps:
Catalyst component A and catalyst component B is put into stirrer for mixing uniform, add aqueous solution of nitric acid, be rolled into micelle
Extruded moulding after shape wet cake, it is dried, roasting, prepares catalyst semi-finished product；
B, by above-mentioned catalyst semi-finished product load activation device in, under the atmosphere of water flowing steam, be warming up to 800-1000 DEG C, and
Thermostatted water processes 20-30 hour prepared finished catalyst at such a temperature.
The preparation method of light oil catalyst for etherification the most according to claim 6, it is characterised in that: nitric acid aqueous solution in step a
The concentration of solution is the aqueous solution of nitric acid of 0.25g/ml-0.5g/ml.
The preparation method of light oil catalyst for etherification the most according to claim 6, it is characterised in that: roasting temperature in step a
Degree is for 1500-2000 DEG C, and roasting time is 8-10 hour.
The preparation method of light oil catalyst for etherification the most according to claim 6, it is characterised in that: step a is dried temperature
Degree is 100 DEG C, and drying time is 8 hours.
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Citations (7)
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|---|---|---|---|---|
| EP0055045A1 (en) * | 1980-12-19 | 1982-06-30 | Imperial Chemical Industries Plc | Production of ethers |
| US4440958A (en) * | 1980-08-01 | 1984-04-03 | The British Petroleum Company Limited | Method for promoting the activity of cation-exchangeable layered clay and zeolite catalysts in proton-catalysed reactions |
| CN1140629A (en) * | 1995-07-18 | 1997-01-22 | 南开大学 | Catalyst using for process of ether and its processing method |
| CN1289751A (en) * | 1999-09-29 | 2001-04-04 | 中国石油化工集团公司 | Process for preparing ether and its alcohol-ether mixture |
| CN1580199A (en) * | 2003-08-05 | 2005-02-16 | 中国科学院大连化学物理研究所 | Process for modifying petrol by etherification and aromatization |
| CN101138739A (en) * | 2007-09-26 | 2008-03-12 | 大庆石油管理局 | Low carbon olefin hydrocarbon etherification catalyst and method of preparing the same |
| CN105413732A (en) * | 2015-12-14 | 2016-03-23 | 夏百庆 | Composite catalyst for gasoline etherification |
-
2016
- 2016-05-24 CN CN201610348737.1A patent/CN105944754A/en active Pending
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|---|---|---|---|---|
| US4440958A (en) * | 1980-08-01 | 1984-04-03 | The British Petroleum Company Limited | Method for promoting the activity of cation-exchangeable layered clay and zeolite catalysts in proton-catalysed reactions |
| EP0055045A1 (en) * | 1980-12-19 | 1982-06-30 | Imperial Chemical Industries Plc | Production of ethers |
| CN1140629A (en) * | 1995-07-18 | 1997-01-22 | 南开大学 | Catalyst using for process of ether and its processing method |
| CN1289751A (en) * | 1999-09-29 | 2001-04-04 | 中国石油化工集团公司 | Process for preparing ether and its alcohol-ether mixture |
| CN1580199A (en) * | 2003-08-05 | 2005-02-16 | 中国科学院大连化学物理研究所 | Process for modifying petrol by etherification and aromatization |
| CN101138739A (en) * | 2007-09-26 | 2008-03-12 | 大庆石油管理局 | Low carbon olefin hydrocarbon etherification catalyst and method of preparing the same |
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| Title |
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| 李进军等编著: "《绿色化学导论》", 31 August 2015 * |
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