CN109289932A - A kind of Ni-based high dispersive emulsion catalyst and its preparation method and application - Google Patents
A kind of Ni-based high dispersive emulsion catalyst and its preparation method and application Download PDFInfo
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- CN109289932A CN109289932A CN201811279522.4A CN201811279522A CN109289932A CN 109289932 A CN109289932 A CN 109289932A CN 201811279522 A CN201811279522 A CN 201811279522A CN 109289932 A CN109289932 A CN 109289932A
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
-
- 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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/08—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal with moving catalysts
- C10G1/086—Characterised by the catalyst used
-
- 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
- C10G47/00—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions
- C10G47/02—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions characterised by the catalyst used
-
- 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
- C10G49/00—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00
- C10G49/02—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00 characterised by the catalyst used
- C10G49/04—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00 characterised by the catalyst used containing nickel, cobalt, chromium, molybdenum, or tungsten metals, or compounds thereof
-
- 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
Abstract
The present invention discloses a kind of Ni-based high dispersive emulsion catalyst and its preparation method and application, and preparation method is the following steps are included: (1) hydrophilic surfactant and nickel salt are dissolved by heating in the deionized water of 0.3~3 times of quality；(2) by lipophilic surfactant and wax oil as in container, being heated to 50~80 DEG C and be stirred under the revolving speed of 1000~4000r/min；(3) water phase is slowly added in container by oil after mutually reaching required temperature, and shearing dispersion 5~15 minutes, is cooled to room temperature after the completion of dispersion, as Ni-based high dispersive emulsion catalyst under constant temperature conditions.The deionized water introduced in catalyst prepared by the present invention avoids previous water-soluble catalyst and removes water the problem of energy consumption is high in slurry bed system hydrogenation process, improve operating efficiency without removal, and dispersion effect is good in raw material, hydrogenation activity is high, and the burnt effect of suppression is good, coal high conversion rate.
Description
Technical field
The present invention relates to catalyst technical field, in particular to a kind of Ni-based high dispersive emulsion catalyst and preparation method thereof
And application, suitable for different types of coal and mink cell focus plus hydrogen refine altogether.
Background technique
China's energy resources are structurally characterized in that oil-poor, few gas, rich coal, and 70% is coal in these non-renewable energy, and wherein
Nearly 80% coal is electric energy by direct burning conversion, and the secondary energy sources such as thermal energy, transformation efficiency is low, and there is serious ecologies
Environmental problem.Whole world petroleum resources tend to heaviness, in poor quality in recent years, and heavy crude ratio is continuously increased, petroleum industry
It has increasing need for developing Heavy Oil Processing Technology with chemical industry.The technology of refining is to be with direct coal liquefaction technology to coal/heavy-oil hydrogenation altogether
A kind of technology for processing coal and heavy oil jointly that base growth goes out, basis is that single direct coal liquefaction technology and mink cell focus add
Hydrogen cracking technology.
Catalyst is that coal/heavy-oil hydrogenation refines and the core technology of DCL/Direct coal liquefaction altogether, and it is harsh that it can be effectively reduced reaction
Degree, improvement product qualities, the conversion ratio for improving coal, is improved and was liquefied the quality of the utilization rate for improving activation hydrogen and liquid product
The economy of journey is the research hotspot that current coal/heavy-oil hydrogenation refines technology altogether.It is mostly direct by coal that coal/heavy oil refines catalyst altogether
Deliquescence accelerant develops, this is catalysis plus is broadly divided into homogeneous catalyst and heterogeneous catalysis two major classes, homogeneous catalysis
Agent can be divided into water-soluble catalyst, oil-soluble catalyst and acidic catalyst, and heterogeneous catalysis can be divided into solid
Grain catalyst and loaded catalyst.Loaded catalyst and solid particle catalyst dispersion performance are poor；Acidic catalyst addition
Measure it is larger, and have corrosivity, be not suitable for large-scale industrial production；Oil-soluble catalyst dispersion effect is good, active height, but at
This is higher；And cost is relatively low, dispersion effect is preferable for classic water-soluble catalyst, but multiple emulsion dispersing technology is multiple in application
Miscellaneous, energy consumption is higher.
Water-soluble catalyst can be prepared as that the high dispersive emulsion catalyst of oily phase can be well dispersed in by micro emulsion method, keep away
The step of having exempted from dehydration reduces energy consumption, reduces cost.
Therefore, the high dispersive emulsion catalyst with greater activity that exploitation is suitable for that coal/heavy-oil hydrogenation refines altogether has ten
Divide important meaning.
Summary of the invention
The present invention provides a kind of Ni-based high dispersive emulsion catalysts and its preparation method and application, are coal/heavy-oil hydrogenation
Refining provides the catalyst of a kind of high activity, low cost altogether.
To reach above-mentioned technical purpose, the technical solution adopted by the present invention are as follows:
One kind being suitable for coal/heavy-oil hydrogenation and is total to nickel metallurgy base high dispersive emulsion catalyst, and the catalyst is with water-soluble catalyst
Oil-soluble high dispersive emulsion catalyst is prepared for raw material, catalytic active component is nickel, without it catalyst will be added after
Reaction system carries out air lift water removal water removal, and the mass content of nickel in the catalyst is 4%~9%.
A kind of Ni-based high dispersive emulsion catalyst preparation method, comprising the following steps:
(1) hydrophilic surfactant and nickel salt are dissolved by heating in the deionized water of 0.3~3 times of quality；
(2) by lipophilic surfactant and wax oil as in container, being heated to 50~80 DEG C and in 1000~4000r/
It is stirred under the revolving speed of min；
(3) water phase is slowly added in the container for containing oily phase, shearing dispersion 5~15 minutes under the conditions of 50~80 DEG C,
It is cooled to room temperature after the completion of dispersion, as Ni-based high dispersive emulsion catalyst.
Wherein it is preferred to which the weight ratio of the hydrophilic surfactant and the lipophilic surfactant is 17.3
~24.5:1, the weight ratio of the hydrophilic surfactant and nickel salt are as follows: 23~34.6:1, the wax oil and the lipophilic
The weight ratio of surfactant sum is 37.5~50:1.
Wherein it is preferred to which the nickel salt is one of nickelous carbonate, nickel nitrate, nickel chloride or combinations thereof.
Wherein it is preferred to the hydrophilic surfactant be neopelex, dodecyl sodium sulfate,
One of cetyl trimethylammonium bromide, Tween-80 or combinations thereof.
Wherein it is preferred to the lipophilic surfactant be one of Span-80, Span -85, oleic acid or its
Combination.
Wherein it is preferred to the wax oil be one of 150N base oil, 400N base oil, clay-filtered wax oil or
A combination thereof.
Wherein it is preferred to shearing dispersion is dispersed using high speed shear in the step (3), and rate of dispersion 1000~
4000r/min。
The Ni-based high dispersive emulsion catalyst of above-mentioned preparation method preparation is in the application refined altogether for coal/heavy-oil hydrogenation, institute
The total metal content that the Ni-based high dispersive emulsion catalyst stated is added in raw material is 200~1000 μ gg of raw material-1。
Beneficial effects of the present invention:
(1) deionized water introduced in the prepared catalyst of invention avoids previous water-soluble catalyst without removal
The problem of energy consumption is high is removed water in slurry bed system hydrogenation process, improves operating efficiency；
(2) process for synthetic catalyst prepared by the present invention is simple, and mild condition, use cost is low, and raw material is cheap and easily-available,
Suitable for large-scale industrial production；
(3) catalyst prepared by the present invention is uniformly dispersed in the feed, and not easy to reunite, dispersion effect is good, simplifies biography
The multiple emulsion dispersing technology of system water-soluble catalyst, hydrogenation activity is high, and the burnt effect of suppression is good, coal high conversion rate.
Detailed description of the invention
Lamination figure after Fig. 1 catalyst is stood.
Dispersity figure of the Ni-based high dispersive emulsion catalyst of Fig. 2 in feedstock oil.
Specific embodiment
Below in conjunction with the specific embodiment of the invention, technical solution of the present invention is clearly and completely described, is shown
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1
A kind of Ni-based high dispersive emulsion catalyst, the catalyst active component are nickel, the weight content of nickel in the catalyst
It is 5.01%, preparation method is as follows:
(1) 13.84g Ni (NO is taken3)2·6H2O, 4.27g deionized water is added in 0.40g dodecyl sodium sulfate；
(2) 0.80g Span-80 is separately taken, 30g 400N base oil is added, is heated to 70 DEG C and in the shearing of 2000r/min
It is stirred under speed；150N base oil, 400N base oil, clay-filtered wax oil
(3) water phase is slowly added in the container for containing oily phase, shearing dispersion 10 minutes, rate of dispersion under the conditions of 70 DEG C
It is cooled to room temperature after the completion of 2000r/min, dispersion, as Ni-based high dispersive emulsion catalyst.
Embodiment 2
A kind of Ni-based high dispersive emulsion catalyst, the catalyst active component are nickel, the weight content of nickel in the catalyst
It is 5.01%, preparation method is as follows:
(1) 13.84g nickelous carbonate, 0.60g neopelex are taken, 43.3g deionized water is added；
(2) Span -85 0.60g are separately taken, 30g 150N base oil is added, is heated to 50 DEG C and in the shearing of 4000r/min
It is stirred under speed；
(3) water phase is slowly added in the container for containing oily phase, shearing dispersion 15 minutes, rate of dispersion under the conditions of 50 DEG C
It is cooled to room temperature after the completion of 1000r/min dispersion, as Ni-based high dispersive emulsion catalyst.
Embodiment 3
A kind of Ni-based high dispersive emulsion catalyst, the catalyst active component are nickel, the weight content of nickel in the catalyst
It is 6.04%, preparation method is as follows:
(1) take 17.63g nickel chloride, 0.24g cetyl trimethylammonium bromide and 0.24g Tween-80, be added 10g go from
Sub- water；
(2) 0.72g oleic acid is separately taken, the clay-filtered wax oil of 30g is added, is heated to 80 DEG C and in the shearing of 1000r/min speed
It is stirred under degree；
(3) water phase is slowly added in the container for containing oily phase, shearing dispersion 5 minutes, rate of dispersion under the conditions of 80 DEG C
It is cooled to room temperature after the completion of 4000r/min, dispersion, as Ni-based high dispersive emulsion catalyst.
The stability parameter that catalyst is made is as shown in table 1.
1 catalyst stability data of table
| Catalyst title | Steadiness parameter/% after standing 5 days | Steadiness parameter/% after standing 15 days |
| Embodiment 1 | 95.83 | 91.93 |
| Embodiment 2 | 95.09 | 91.31 |
| Embodiment 3 | 95.77 | 91.57 |
Note:
Lamination is as shown in Figure 1 after standing.It should be noted that the catalyst for lamination occur can by gentle agitation
So that catalyst restores to the original state.Catalyst dispersity as shown in Fig. 2, wherein (a) be residual oil raw material, (b) for 500ppm be catalyzed
State of the agent in residual oil.
Embodiment 4
Ni-based high dispersive emulsion catalyst prepared in above-described embodiment is used for the auspicious reduced crude of horse (MRAR) and is urged
Change the oil of the quality such as cracking slurry oil (FCCS) blending and Anhui coal plus during hydrogen refine altogether, and use blank, oil-soluble Fe-Ni (1:
1) reaction that catalyst carries out under the same terms is in contrast.It blends oily oil nature and is shown in Table 2, Anhui coal property is shown in Table 3, reacts item
Part are as follows: 420 DEG C of reaction temperature, react first pressing 8MPa, the auspicious reduced crude of horse: Anhui coal=3:1, reaction time 60min, catalyst
500 μ gg of additional amount-1(based on total metal content), 1000 μ gg of vulcanizing agent-1；Reaction result is shown in Table 4.
The oily fundamental property of 2 catalyst activity of table evaluation
The Industrial Analysis of 3 Anhui coal of table and element composition and property
4 Ma Ruichang slag of table-Anhui coal hydrogenation refines distribution of reaction products altogether
As shown in Table 4, it relative to oil-soluble Fe-Ni (1:1) bimetallic catalyst is used, is urged using Ni-based high dispersive lotion
The solid content of reaction system is lower when agent；Butt ashless coal conversion ratio is higher.
Embodiment 5
By Ni-based high dispersive emulsion catalyst prepared in above-described embodiment be used in MRAR slurry bed system hydrogenation system into
Row evaluation, and it is in contrast using the reaction that oil-soluble Fe-Ni (1:1) catalyst carries out under the same terms.MRAR oil nature is shown in
Table 1, reaction condition are as follows: 420 DEG C of reaction temperature, react first pressing 8MPa, reaction time 60min, 200 μ gg of catalyst charge-1
(based on total metal content), 1000 μ gg of vulcanizing agent-1；Reaction result is shown in Table 5.
5 Ma Ruichang slurry state bed hydroprocessing distribution of reaction products of table
As shown in Table 5, it relative to oil-soluble Fe-Ni (1:1) bimetallic catalyst is used, is urged using Ni-based high dispersive lotion
The gas and coking yield of reaction system are lower when agent, and liquid yield is higher.Ni-based high dispersive emulsion catalyst is inhibiting green coke
While, it can also promote heavy oil to change to light component.This not only improves reaction effect, and due to simplifying water-soluble catalytic
The multistage emulsification pretreatment process of agent, greatly reduces the production cost of catalyst.
Embodiment 6
Ni-based high dispersive emulsion catalyst prepared in above-described embodiment is used in YLCTAR slurry bed system hydrogenation system
It is evaluated, and in contrast using the reaction that oil-soluble Fe-Ni (1:1) catalyst carries out under the same terms.YLCTAR oiliness
Matter is shown in Table 1, reaction condition are as follows: 420 DEG C of reaction temperature, reacts first pressing 8MPa, reaction time 60min, 1000 μ of catalyst charge
g·g-1(based on total metal content), 1000 μ gg of vulcanizing agent-1；Reaction result is shown in Table 6.
The normal slag hydrogenation reaction product distribution of 6 Yulin coal tar of table
| Catalyst | Suspension coke/wt% | Deposit coke/wt% | Coking yield |
| Fe-Ni(1:1) | 2.38 | 0.03 | 2.39 |
| High dispersive Ni | 2.09 | 0.01 | 2.10 |
As shown in Table 6, it relative to oil-soluble Fe-Ni (1:1) bimetallic catalyst is used, is urged using Ni-based high dispersive lotion
The suspension of reaction system is burnt when agent, and it is all lower to deposit burnt and total burnt amount.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. one kind, which is suitable for coal/heavy-oil hydrogenation, is total to nickel metallurgy base high dispersive emulsion catalyst, it is characterised in that: the catalyst is with water-soluble
Property catalyst be raw material prepare oil-soluble high dispersive emulsion catalyst, catalytic active component is nickel, is urged without that will be added
Reaction system after agent carries out air lift water removal water removal, and the mass content of nickel in the catalyst is 4%~9%.
2. a kind of preparation method of Ni-based high dispersive emulsion catalyst described in claim 1, which is characterized in that including following step
It is rapid:
(1) hydrophilic surfactant and nickel salt are dissolved by heating in the deionized water of 0.3~3 times of quality；
(2) by lipophilic surfactant and wax oil as in container, being heated to 50~80 DEG C and 1000~4000r/min's
It is stirred under revolving speed；
(3) water phase is slowly added in the container for containing oily phase, shearing dispersion 5~15 minutes, dispersion under the conditions of 50~80 DEG C
It is cooled to room temperature after the completion, as Ni-based high dispersive emulsion catalyst.
3. the preparation method of Ni-based high dispersive emulsion catalyst according to claim 2, it is characterised in that: the hydrophilic
The weight ratio of surfactant and the lipophilic surfactant be 17.3~24.5:1, the hydrophilic surfactant and
The weight ratio of nickel salt are as follows: the weight ratio of 23~34.6:1, the wax oil and the lipophilic surfactant sum is 37.5~50:
1。
4. the preparation method of Ni-based high dispersive emulsion catalyst according to claim 2, it is characterised in that: the nickel salt
For one of nickelous carbonate, nickel nitrate, nickel chloride or combinations thereof.
5. the preparation method of Ni-based high dispersive emulsion catalyst according to claim 2, it is characterised in that: described is hydrophilic
Type surfactant is neopelex, in dodecyl sodium sulfate, cetyl trimethylammonium bromide, Tween-80
One kind or combinations thereof.
6. the preparation method of Ni-based high dispersive emulsion catalyst according to claim 2, it is characterised in that: the oleophylic
Type surfactant is one of Span-80, Span -85, oleic acid or combinations thereof.
7. the preparation method of Ni-based high dispersive emulsion catalyst according to claim 2, it is characterised in that: the wax oil
For one of 150N base oil, 400N base oil, clay-filtered wax oil or combinations thereof.
8. the preparation method of Ni-based high dispersive emulsion catalyst according to claim 2, it is characterised in that: the step
(3) shearing dispersion is dispersed using high speed shear in, and rate of dispersion is in 1000~4000r/min.
9. a kind of Ni-based high dispersive emulsion catalyst of any one of claim 2-8 preparation method preparation adds for coal/heavy oil
The application that hydrogen refines altogether, it is characterised in that: the total metal content that the Ni-based high dispersive emulsion catalyst is added in raw material is raw material
200~1000 μ gg-1。
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| CN112717939A (en) * | 2021-01-06 | 2021-04-30 | 中国船舶重工集团公司第七一九研究所 | Emulsion Ni/ZrO for catalytic hydrogenation upgrading of caprylic acid2Process for preparing catalyst |
| CN112717939B (en) * | 2021-01-06 | 2023-02-10 | 中国船舶重工集团公司第七一九研究所 | Emulsion Ni/ZrO for catalytic hydrogenation upgrading of caprylic acid 2 Process for preparing catalyst |
| CN114832865A (en) * | 2022-06-15 | 2022-08-02 | 中国石油大学(华东) | Preparation method of molybdenum-based microemulsion catalyst applied to hydrocracking |
| CN114832865B (en) * | 2022-06-15 | 2023-08-22 | 中国石油大学(华东) | Preparation method of molybdenum-based microemulsion catalyst applied to hydrocracking |
| CN115212887A (en) * | 2022-07-05 | 2022-10-21 | 南京大学 | Preparation method of reforming catalyst with high dispersion degree of active metal components |
| CN115212887B (en) * | 2022-07-05 | 2023-06-06 | 南京大学 | Preparation method of reforming catalyst with high dispersity of active metal component |
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