CN107362816A - A kind of residual hydrocracking method for preparing catalyst - Google Patents
A kind of residual hydrocracking method for preparing catalyst Download PDFInfo
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- CN107362816A CN107362816A CN201710634067.4A CN201710634067A CN107362816A CN 107362816 A CN107362816 A CN 107362816A CN 201710634067 A CN201710634067 A CN 201710634067A CN 107362816 A CN107362816 A CN 107362816A
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/182—Phosphorus; Compounds thereof with silicon
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- 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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/06—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by destructive hydrogenation
-
- 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
- C10G2300/1003—Waste materials
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- Oil, Petroleum & Natural Gas (AREA)
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a kind of residual hydrocracking method for preparing catalyst, comprise the following steps：Atoleine and sepiolite powder are stirred, solid paraffin is added and stirs to dissolving completely, add magnesium stearate microwave treatment, filter, washing, be dried to obtain prefabricated material；Into prefabricated material, addition waterglass, phosphate aqueous solution are mixed with beating, and are added absolute ethyl alcohol, cerium citrate stirring, are stood, filtering, calcine and obtain residual hydrocracking catalyst.Residual hydrocracking method for preparing catalyst proposed by the present invention, gained specific surface area of catalyst is very big, and internal aperture is interconnected, and inside is not susceptible to block, and can effectively improve the speed of dregs of fat cracking, and selectivity is high.
Description
Technical field
The present invention relates to catalyst technical field, more particularly to a kind of residual hydrocracking method for preparing catalyst.
Background technology
At present, in residual oil hydrogenation-catalytic cracking combination technique, with fixed bed residual hydrogenation and catalytic cracking combination technique,
Heavy oil feedstock is mixed with hydrogen and is sent into boiling bed hydrogenation treatment reactor, hydrogenation reaction is carried out under hydrogenation catalyst catalysis,
Hydrogenation reaction product is subjected to gas-liquid separation, the hydrogen in the gas phase isolated is circulated for hydrogenation reaction, by what is isolated
Liquid phase further carries out catalytic cracking reaction, the cracking product in pyrolysis product is reclaimed, by the recycle oil in the pyrolysis product
It is mixed for hydrogenation reaction with the heavy oil feedstock；Wherein, used hydrogenation catalyst is usually using sieve and silica-sesquioxide as load
The particle of body, internal the problem of blocking, poor selectivity easily occurs be present.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of residual hydrocracking catalyst preparation side
Method, gained specific surface area of catalyst is very big, and internal aperture is interconnected, and inside is not susceptible to block, and can effectively improve the dregs of fat and split
The speed of solution, and selectivity is high.
A kind of residual hydrocracking method for preparing catalyst proposed by the present invention, comprises the following steps：
S1, atoleine and sepiolite powder stirred, add solid paraffin and stir to dissolving completely, add magnesium stearate
Microwave treatment, filter, washing, be dried to obtain prefabricated material；
S2, into prefabricated material, addition waterglass, phosphate aqueous solution are mixed with beating, and add absolute ethyl alcohol, cerium citrate stirring,
Stand, filtering, calcining obtains residual hydrocracking catalyst.
Preferably, in S1, microwave treatment time 5-12min, microwave power 400-500W.
Preferably, in S1,60-100 parts atoleine and 5-15 parts sepiolite powder is stirred into 5-10min by weight, stirred
It is 2400-2800r/min to mix speed, adds 1-3 part solid paraffins and stirs to dissolving completely, it is micro- to add 2-4 part magnesium stearates
Ripple handles 5-12min, microwave power 400-500W, filters, and washing, is dried to obtain prefabricated material.
Preferably, in S2, calcining heat is 700-900 DEG C, calcination time 5-10h.
Preferably, in S2, waterglass is added into prefabricated material, concentration is that 15-25wt% phosphate aqueous solutions are mixed with beating 15-
35min, add absolute ethyl alcohol, concentration is that 0.001-0.005mol/L cerium citrates stir 5-12min, mixing speed 400-
700r/min, 5-10h is stood, filtering, 700-900 DEG C of calcining 5-10h, obtains residual hydrocracking catalyst.
Preferably, in S2,20-40 parts waterglass is added by weight into the prefabricated material of 40-80 parts, 60-80 part concentration is
15-25wt% phosphate aqueous solutions are mixed with beating 15-35min, add 80-150 parts absolute ethyl alcohol, 2-4 parts concentration is 0.001-
0.005mol/L cerium citrates stir 5-12min, mixing speed 400-700r/min, stand 5-10h, filter, 700-900 DEG C
5-10h is calcined, obtains residual hydrocracking catalyst.
The present invention is compounded using sepiolite powder and atoleine, and after high-speed stirred, sepiolite powder cracking is in pencil
Single fiber, under the cooperation of solid paraffin, hydrophobic performance is excellent, and magnesium stearate has certain solubility in atoleine,
It is distributed in molecular state between atoleine and solid paraffin, dispersion effect is fabulous；Prefabricated material can be effectively dispersed in waterglass,
In phosphate aqueous solution, for the sepiolite single fiber of internal pencil by further corrosion, specific surface area is very big, increases average pore size
Greatly, aperture is broadened, while internal aperture can be made to be interconnected, and inside is not susceptible to block, and is further immersed in cerium citrate
In solution, by calcining, the cerium oxide of formation is supported on said structure surface, can effectively improve the speed of dregs of fat cracking, and
Selectivity is high.
Embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of residual hydrocracking method for preparing catalyst, comprises the following steps：
S1, atoleine and sepiolite powder stirred, add solid paraffin and stir to dissolving completely, add magnesium stearate
Microwave treatment, filter, washing, be dried to obtain prefabricated material；
S2, into prefabricated material, addition waterglass, phosphate aqueous solution are mixed with beating, and add absolute ethyl alcohol, cerium citrate stirring,
Stand, filtering, calcining obtains residual hydrocracking catalyst.
Embodiment 2
A kind of residual hydrocracking method for preparing catalyst, comprises the following steps：
S1,60 parts of atoleines and 15 parts of sepiolite powders are stirred into 5min, mixing speed 2800r/min by weight,
Add 1 part of solid paraffin to stir to dissolving completely, add 4 parts of magnesium stearate microwave treatment 5min, microwave power 500W, mistake
Filter, washing, is dried to obtain prefabricated material；
S2, into 40 parts of prefabricated material, 40 parts of waterglass of addition, 60 parts of concentration are that 25wt% phosphate aqueous solutions mix by weight
Mashing 15min is closed, adds 150 parts of absolute ethyl alcohols, 2 parts of concentration are for 0.005mol/L cerium citrates stirring 5min, mixing speed
700r/min, 5h is stood, filtering, 900 DEG C of calcining 5h, obtains residual hydrocracking catalyst.
Embodiment 3
A kind of residual hydrocracking method for preparing catalyst, comprises the following steps：
S1,100 parts of atoleines and 5 parts of sepiolite powders are stirred into 10min, mixing speed 2400r/min by weight,
Add 3 parts of solid paraffins to stir to dissolving completely, add 2 parts of magnesium stearates microwave treatment 12min, microwave power 400W,
Filtering, washing, is dried to obtain prefabricated material；
S2, into 80 parts of prefabricated material, 20 parts of waterglass of addition, 80 parts of concentration are that 15wt% phosphate aqueous solutions mix by weight
Mashing 35min is closed, adds 80 parts of absolute ethyl alcohols, 4 parts of concentration are for 0.001mol/L cerium citrates stirring 12min, mixing speed
400r/min, 10h is stood, filtering, 700 DEG C of calcining 10h, obtains residual hydrocracking catalyst.
Embodiment 4
A kind of residual hydrocracking method for preparing catalyst, comprises the following steps：
S1,70 parts of atoleines and 12 parts of sepiolite powders are stirred into 6min, mixing speed 2700r/min by weight,
Add 1.5 parts of solid paraffins to stir to dissolving completely, add 3.5 parts of magnesium stearate microwave treatment 7min, microwave power is
480W, filter, washing, be dried to obtain prefabricated material；
S2, into 50 parts of prefabricated material, 35 parts of waterglass of addition, 65 parts of concentration are that 22wt% phosphate aqueous solutions mix by weight
Mashing 20min is closed, adds 120 parts of absolute ethyl alcohols, 2.5 parts of concentration are that 0.004mol/L cerium citrates stir 6min, mixing speed
For 600r/min, 6h is stood, filtering, 850 DEG C of calcining 6h, obtains residual hydrocracking catalyst.
Embodiment 5
A kind of residual hydrocracking method for preparing catalyst, comprises the following steps：
S1,90 parts of atoleines and 8 parts of sepiolite powders are stirred into 8min by weight, mixing speed 2500r/min, added
Enter 2.5 parts of solid paraffins to stir to dissolving completely, add 2.5 parts of magnesium stearate microwave treatment 10min, microwave power is
420W, filter, washing, be dried to obtain prefabricated material；
S2, into 70 parts of prefabricated material, 25 parts of waterglass of addition, 75 parts of concentration are that 18wt% phosphate aqueous solutions mix by weight
Mashing 30min is closed, adds 100 parts of absolute ethyl alcohols, 3.5 parts of concentration are that 0.002mol/L cerium citrates stir 10min, mixing speed
For 500r/min, 8h is stood, filtering, 750 DEG C of calcining 8h, obtains residual hydrocracking catalyst.
Embodiment 6
A kind of residual hydrocracking method for preparing catalyst, comprises the following steps：
S1,80 parts of atoleines and 10 parts of sepiolite powders are stirred into 7min, mixing speed 2600r/min by weight,
Add 2 parts of solid paraffins to stir to dissolving completely, add 3 parts of magnesium stearate microwave treatment 8min, microwave power 450W, mistake
Filter, washing, is dried to obtain prefabricated material；
S2, into 60 parts of prefabricated material, 30 parts of waterglass of addition, 70 parts of concentration are that 20wt% phosphate aqueous solutions mix by weight
Mashing 25min is closed, adds 110 parts of absolute ethyl alcohols, 3 parts of concentration are for 0.003mol/L cerium citrates stirring 8min, mixing speed
550r/min, 7h is stood, filtering, 800 DEG C of calcining 7h, obtains residual hydrocracking catalyst.
Performance test is carried out using the gained residual hydrocracking catalyst of embodiment 6, its result is as follows：
| Test event | Detection method | Standard No. | Test result |
| Pore volume, mL/g | Water droplet method | Q/SYLS 0521-2002 | 0.47 |
| Abrasion index, % | Gas lift method | Q/SYLS 0518-2002 | 1.57 |
| Micro-activity (4h), % | Miniature fixed bed reaction | Q/SYLS 0589-2002 | 88 |
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (6)
1. a kind of residual hydrocracking method for preparing catalyst, it is characterised in that comprise the following steps：
S1, atoleine and sepiolite powder stirred, add solid paraffin and stir to dissolving completely, add magnesium stearate microwave
Processing, filter, washing, be dried to obtain prefabricated material；
S2, into prefabricated material, addition waterglass, phosphate aqueous solution are mixed with beating, and add absolute ethyl alcohol, cerium citrate stirring, quiet
Put, filter, calcining obtains residual hydrocracking catalyst.
2. residual hydrocracking method for preparing catalyst according to claim 1, it is characterised in that in S1, during microwave treatment
Between be 5-12min, microwave power 400-500W.
3. residual hydrocracking method for preparing catalyst according to claim 1 or claim 2, it is characterised in that in S1, by weight
By 60-100 parts atoleine and 5-15 parts sepiolite powder stirring 5-10min, mixing speed 2400-2800r/min, 1- is added
3 parts of solid paraffins are stirred to dissolving completely, add 2-4 part magnesium stearates microwave treatment 5-12min, microwave power 400-
500W, filter, washing, be dried to obtain prefabricated material.
4. according to any one of the claim 1-3 residual hydrocracking method for preparing catalyst, it is characterised in that in S2, forge
It is 700-900 DEG C to burn temperature, calcination time 5-10h.
5. according to any one of the claim 1-4 residual hydrocracking method for preparing catalyst, it is characterised in that in S2, to
Waterglass is added in prefabricated material, concentration is that 15-25wt% phosphate aqueous solutions are mixed with beating 15-35min, add absolute ethyl alcohol, dense
Spend and stir 5-12min, mixing speed 400-700r/min for 0.001-0.005mol/L cerium citrates, stand 5-10h, mistake
Filter, 700-900 DEG C of calcining 5-10h, obtains residual hydrocracking catalyst.
6. according to any one of the claim 1-5 residual hydrocracking method for preparing catalyst, it is characterised in that in S2, press
Parts by weight add 20-40 parts waterglass into the prefabricated material of 40-80 parts, 60-80 parts concentration mixes for 15-25wt% phosphate aqueous solutions
15-35min is beaten, adds 80-150 parts absolute ethyl alcohol, 2-4 parts concentration is that 0.001-0.005mol/L cerium citrates stir 5-
12min, mixing speed 400-700r/min, 5-10h is stood, filtering, 700-900 DEG C of calcining 5-10h, residual hydrogenation is obtained and splits
Change catalyst.
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| CN201710634067.4A CN107362816A (en) | 2017-07-29 | 2017-07-29 | A kind of residual hydrocracking method for preparing catalyst |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114874810A (en) * | 2022-04-28 | 2022-08-09 | 海南汉地阳光石油化工有限公司 | 60N white oil agent for artificial fibers and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101138740A (en) * | 2006-09-05 | 2008-03-12 | 北京盛大京泰化学研究所 | Cracking catalyst containing nanometer rare-earth oxide and method of preparing the same |
| CN104371795A (en) * | 2014-09-18 | 2015-02-25 | 洛阳师范学院 | Low density foamed concrete product demolding agent and preparation method thereof |
-
2017
- 2017-07-29 CN CN201710634067.4A patent/CN107362816A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101138740A (en) * | 2006-09-05 | 2008-03-12 | 北京盛大京泰化学研究所 | Cracking catalyst containing nanometer rare-earth oxide and method of preparing the same |
| CN104371795A (en) * | 2014-09-18 | 2015-02-25 | 洛阳师范学院 | Low density foamed concrete product demolding agent and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114874810A (en) * | 2022-04-28 | 2022-08-09 | 海南汉地阳光石油化工有限公司 | 60N white oil agent for artificial fibers and preparation method thereof |
| CN114874810B (en) * | 2022-04-28 | 2024-04-12 | 海南汉地阳光石油化工有限公司 | 60N white oil agent for artificial fiber and preparation method thereof |
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