CN106140168A - The processing method of a kind of useless hydrogenation catalyst and the serosity prepared by described method - Google Patents
The processing method of a kind of useless hydrogenation catalyst and the serosity prepared by described method Download PDFInfo
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- CN106140168A CN106140168A CN201610483614.9A CN201610483614A CN106140168A CN 106140168 A CN106140168 A CN 106140168A CN 201610483614 A CN201610483614 A CN 201610483614A CN 106140168 A CN106140168 A CN 106140168A
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- hydrogenation catalyst
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/02—Heat treatment
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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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
- B01J38/12—Treating with free oxygen-containing gas
- B01J38/14—Treating with free oxygen-containing gas with control of oxygen content in oxidation gas
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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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/485—Impregnating or reimpregnating with, or deposition of metal compounds or catalytically active elements
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Abstract
The processing method that the present invention relates to useless hydrogenation catalyst and the serosity prepared by described method.The treating method comprises: grind after useless hydrogenation catalyst is carried out coke-burning regeneration, the useless hydrogenation catalyst powder of preparation；Lateritic nickel ore is ground and prepares lateritic nickel ore powder；Useless hydrogenation catalyst powder and lateritic nickel ore powder are mixed, adds dust technology and binding agent, prepare serosity；Described serosity passes through spray dryer drying and moulding, then carries out roasting, prepares hydrogenation catalyst.The present invention, by recycling useless hydrogenation catalyst, improves its hydrogenation activity, can prepare the cheap and callable catalyst being applicable to heavy oil floating bed hydrogenation.
Description
Technical field
The present invention relates to hydrogenation catalyst field, particularly relate to a kind of fixed bed residuum hydrodesulfurization agent of giving up and prepare heavy oil and hang
The method of floating bed hydrogenation catalyst, and the serosity prepared by the method.
Background technology
Along with heaviness day by day, in poor quality and the increase to light-end products demand of crude oil, fixed bed residual hydrogenation technology
Because the advantages such as its technology maturation, simple to operate, the stable operation of equipment have become the important means of heavy oil modification.But due to poor quality
Reaction raw materials and harsh process conditions, easily there is the phenomenon of metal deposit and carbon deposit in residual oil hydrocatalyst, causes catalysis
Agent inactivates.It is said that in general, the service life of fixed bed residual oil hydrocatalyst is 1～1.5 year, and more difficult recycling, cause
The shortcoming that fixed bed residual hydrogenation technical price is expensive.Meanwhile, discarded catalyst is higher due to tenor, easily causes ring
Environment pollution.
Based on the problems referred to above, have and prior art discloses the technique preparing macropore hydrogenation catalyst.This technique includes useless
Hydrogenation catalyst carries out heat treatment, removes charcoal and the sulfur of deposition on catalyst, then is ground, adds bauxite, kieselguhr, height
A kind of molding in ridge soil or meerschaum, i.e. prepares new hydrogenation catalyst.But, this technique only improves the hole knot of catalyst
Structure, does not recover the metal active of catalyst.
Prior art two discloses a kind of method being prepared hydrogenation catalyst by useless hydrogenation catalyst.The method is to add useless
Hydrogen catalyst grinds, then is added thereto to aluminium oxide, binding agent and acid or alkaline solution and mixes, kneading and compacting,
New hydrogenation catalyst is obtained after drying, roasting.This technical scheme can improve the pore structure of catalyst, makes macropore increase, meanwhile,
Acid treatment or alkali process and can improve the deployment conditions of metal in catalyst, make the activity of catalyst obtain a certain degree of lifting,
But the limited extent promoted.
Prior art three discloses a kind of method that useless Hydrobon catalyst prepares new Hydrobon catalyst.The method
It is that useless Hydrobon catalyst is ground, then is added thereto to reactive metal oxides or active metal salt, add viscous
Kneading and compacting, then coke-burning regeneration after knot agent.In gained catalyst, metal active constituent content increases, and improves catalyst and lives
Property.But, owing to the utilization rate of reactive metal oxides is low, cause the relatively costly of the method.
Therefore, from angle economical and environmentally friendly, using discarded fixed bed residual oil hydrocatalyst as secondary resource
Carry out recycling tool to be of great significance.
Summary of the invention
It is desirable to provide the processing method of a kind of useless hydrogenation catalyst, effectively solve it and recycle problem, thus
Obtain a kind of cheap and callable hydrogenation catalyst.
For achieving the above object, the invention provides the processing method of a kind of useless hydrogenation catalyst, comprise the steps:
Step A, carries out useless hydrogenation catalyst coke-burning regeneration, and is ground by the useless hydrogenation catalyst after regeneration, system
Must be given up hydrogenation catalyst powder；
Step B, prepares lateritic nickel ore powder；
Step C, mixes described useless hydrogenation catalyst powder and described ready lateritic nickel ore powder, adds dust technology
And binding agent, make serosity；
Step D, by described serosity by spray dryer drying and moulding, afterwards by the semi-finished product catalyst after drying and moulding
Carry out roasting, prepare hydrogenation catalyst.
In the processing method of above-mentioned useless hydrogenation catalyst, described coke-burning regeneration process uses nitrogen-air regenesis
Method: described useless hydrogenation catalyst is placed in regenerator, is passed through nitrogen and replaces, temperature is slowly raised to 250～350
DEG C, it being slowly introducing air after constant temperature 3～4h, control the oxygen content 0.3%～0.5% in regenerator, heating rate is 10～20
DEG C/h, temperature rise to 400 DEG C after constant temperature 2～3h, temperature rises to 500 DEG C of constant temperature to end of making charcoal, and continues constant temperature after end of making charcoal
Start after 6h to cool to room temperature.
In the processing method of above-mentioned useless hydrogenation catalyst, in described step B, lateritic nickel ore is ground broken and obtains
Lateritic nickel ore powder, the particle size of this powder is below 5 μm, preferably 2～3 μm.
In the processing method of above-mentioned useless hydrogenation catalyst, described useless hydrogenation catalyst is that aperture is big, carbon deposit is many, metal deposit
Few useless hydrogenation catalyst, the most residue fixed-bed hydrodesulfurization is given up agent.
In the processing method of above-mentioned useless hydrogenation catalyst, the particle size of described useless hydrogenation catalyst powder is below 5 μm,
It is preferably 2～3 μm.
In the processing method of above-mentioned useless hydrogenation catalyst, based on the percentage by weight accounting for total solid material, described laterite
Nickel minerals powder is 10%～20%, and binding agent is 10%, and useless hydrogenation catalyst powder is 70%～80%；Wherein dust technology content
For total solid material 5%～15%.
In the processing method of above-mentioned useless hydrogenation catalyst, in described lateritic nickel ore powder by weight percentage containing 1%～
The nickel oxide of 3% and the ferrum oxide of 10%～20%.
In the processing method of above-mentioned useless hydrogenation catalyst, the particle diameter of the semi-finished product catalyst in described step D is 75～150
μm；Described sintering temperature is 400～450 DEG C, roasting time 4～6h.
In the processing method of above-mentioned useless hydrogenation catalyst, described binding agent is Alumina gel；Before described step A, the most right
Described useless hydrogenation catalyst carries out pretreatment: utilize toluene extracting to remove the oil product that this useless hydrogenation catalyst is adsorbed, and 100
～120 DEG C be dried, drying time is 1.5～2.5h.
Present invention also offers a kind of by the serosity prepared by the processing method of above-mentioned useless hydrogenation catalyst, comprising: red
Soil nickel minerals powder, useless hydrogenation catalyst powder, binding agent and dust technology；
Wherein, based on the percentage by weight accounting for total solid material, described lateritic nickel ore powder is 10%～20%, bonding
Agent is 10%, and dead catalyst powder is 70%～80%；Wherein dust technology content is the 5%～15% of total solid material.
In the inventive solutions, owing to the addition of lateritic nickel ore in useless hydrogenation catalyst, add and wherein add
The content of hydrogen metal, thus enhance the Hydrogenation of catalyst, the pore structure of catalyst can be improved in mineral duct simultaneously.
Dilute nitric acid solution is conducive to the metal component in useless hydrogenation catalyst and lateritic nickel ore again to disperse, and improves useless hydrogenation
The accumulation of metal phenomenon that catalyst occurs in running, strengthens the Hydrogenation of catalyst.
By the technical solution of the present invention process to useless hydrogenation catalyst, one can be obtained and be applicable to heavy oil floating bed hydrogenation
Cheap and callable catalyst.
Accompanying drawing explanation
Fig. 1 is that the present invention gives up the process flow schematic diagram of hydrogenation catalyst.
Detailed description of the invention
Below in conjunction with drawings and Examples, the detailed description of the invention of the present invention is described in more details, in order to energy
The advantage being enough more fully understood that the solution of the present invention and its various aspects.But, specific embodiments described below and reality
Executing example is only descriptive purpose rather than limitation of the present invention.
As it is shown in figure 1, the present invention gives up, the processing method of hydrogenation catalyst comprises the following steps:
Step A, the useless hydrogenation catalyst powder of preparation: pretreated useless hydrogenation catalyst is carried out coke-burning regeneration, then
Useless hydrogenation catalyst after regeneration is ground.The useless hydrogenation catalyst used in the embodiment of the present invention is residue fixed-bed adding
Hydrogen desulfurization is given up agent, described useless hydrogenation catalyst also include other apertures compared with big, carbon deposit is more, the less useless hydrogenation of metal deposit is urged
Agent.
Above-mentioned preprocessing process by: utilize toluene extracting to remove the oil product that adsorbed of this useless hydrogenation catalyst, and 100～
120 DEG C are dried 1.5～2.5h.
The method that coke-burning regeneration process is nitrogen-air regenesis used in the embodiment of the present invention: add residue fixed-bed
Hydrogen desulfurization agent of giving up is placed in regenerator, is passed through nitrogen and replaces, temperature is slowly raised to 250～350 DEG C, constant temperature 3～4h
After be slowly introducing air, the oxygen content controlled in regenerator is 0.3%～0.5%, and heating rate is 10～20 DEG C/h, temperature liter
Constant temperature 2～3h after 400 DEG C, temperature rises to 500 DEG C of constant temperature to end of making charcoal, and starts cooling after continuing constant temperature 6h after end of making charcoal
To room temperature.By this coke-burning regeneration process, major part can be removed and cover at the supercentral carbon deposit of useless activity of hydrocatalyst, favorably
In recovering its hydrogenation activity, and improve pore passage structure.
Above-mentioned residue fixed-bed hydrodesulfurization is given up after the ground pulverizing of agent, and the particle size obtained is below 5 μm, and basis
The preferred size of inventive embodiments is 2～3 μm.
Step B, prepares lateritic nickel ore powder: ground by lateritic nickel ore and i.e. obtain required lateritic nickel ore powder.This
The lateritic nickel ore used in bright embodiment, contains nickel oxide and the oxidation of 10%～20% of 1%～3% by weight percentage
Ferrum.
After the ground pulverizing of above-mentioned lateritic nickel ore, the particle size obtained is below 5 μm, and the embodiment of the present invention is excellent
Choosing a size of 2～3 μm.
Step C, prepares serosity: mixed with lateritic nickel ore powder by useless hydrogenation catalyst powder, add dilute nitric acid solution and
Binding agent, i.e. prepares required serosity.Wherein in the embodiment of the present invention, described binding agent is Alumina gel.
In above-mentioned serosity, each component is based on the percentage by weight accounting for total solid material: lateritic nickel ore powder be 10%～
20%, binding agent is 10%, and useless hydrogenation catalyst powder is 70%～80%；Dust technology content is the 5% of total solid material
～15%.
Step D, serosity molding: by above-mentioned serosity by, after spray dryer drying and moulding, obtaining semi-finished product catalyst, then
Heavy oil floating bed hydrogenation catalyst is i.e. prepared after roasting.
In the embodiment of the present invention, the particle diameter of described semi-finished product catalyst should control in 75～150 μm.Above-mentioned roasting process
Sintering temperature is 400～450 DEG C, roasting time 4～6h.
Embodiment 1
Select the useless Hydrobon catalyst of fixed bed residual hydrogenation equipment, use toluene extracting to remove useless hydrogenation catalyst
The oil product of absorption, 120 DEG C of dry 2h, useless hydrogenation catalyst is carried out coke-burning regeneration, regenerated catalyst weighs 70g after grinding, with
20g lateritic nickel ore powder mixes, and adding 10g Alumina gel with 120ml concentration is the dilute nitric acid solution of 2mol/L, after making serosity,
Make, by spray drying, the sample that particle diameter is 75～150 μm, sample is made raw catelyst after roasting 4h at 450 DEG C.
Embodiment 2
Select the useless Hydrobon catalyst of fixed bed residual hydrogenation equipment, use toluene extracting to remove useless hydrogenation catalyst
The oil product of absorption, 120 DEG C of dry 1.5h, useless hydrogenation catalyst is carried out coke-burning regeneration, regenerated catalyst weighs 80g after grinding,
Mixing with 10g lateritic nickel ore powder, adding 10g Alumina gel with 120ml concentration is the dilute nitric acid solution of 0.7mol/L, makes serosity
After, make, by spray drying, the sample that particle diameter is 75～150 μm, sample is made raw catelyst after roasting 4h at 450 DEG C.
Embodiment 3
Select the useless Hydrobon catalyst of fixed bed residual hydrogenation equipment, use toluene extracting to remove useless hydrogenation catalyst
The oil product of absorption, 110 DEG C of dry 2.5h, useless hydrogenation catalyst is carried out coke-burning regeneration, regenerated catalyst weighs 70g after grinding,
Mixing with 20g lateritic nickel ore powder, adding 10g Alumina gel with 100ml concentration is the dilute nitric acid solution of 2mol/L, makes serosity
After, make, by spray drying, the sample that particle diameter is 75～150 μm, sample is made raw catelyst after roasting 5h at 400 DEG C.
Embodiment 4
Select the useless Hydrobon catalyst of fixed bed residual hydrogenation equipment, use toluene extracting to remove useless hydrogenation catalyst
The oil product of absorption, 100 DEG C of dry 2.5h, useless hydrogenation catalyst is carried out coke-burning regeneration, regenerated catalyst weighs 80g after grinding,
Mixing with 10g lateritic nickel ore powder, adding 10g Alumina gel with 200ml concentration is the dilute nitric acid solution of 0.7mol/L, makes serosity
After, make, by spray drying, the sample that particle diameter is 75～150 μm, sample is made raw catelyst after roasting 6h at 400 DEG C.
Comparative example
Select the useless Hydrobon catalyst of fixed bed residual hydrogenation equipment, use toluene extracting to remove useless hydrogenation catalyst
The oil product of absorption, after 120 DEG C of dry 2h, it is 75～150 μm that useless hydrogenation catalyst is ground to particle diameter.
Prepared raw catelyst carries out in autoclave coal tar hydrogenating experiment, and gained evaluation result is as shown in table 1.
Table 1 catalyst activity evaluation result
| Project | Raw material | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example |
| Toluene insolubles, wt% | 10.04 | 2.16 | 2.53 | 2.21 | 2.48 | 9.86 |
(note: the wt% in table is weight percentage.)
As shown in Table 1, the inventive method the regenerated catalyst prepared has preferable Hydrogenation, can convert in coal tar
Major part toluene insolubles, the inventive method is particularly well-suited to be prepared coal tar suspension bed hydrogenation catalyst by useless hydrogenation catalyst
Agent.
It is last that it is noted that obviously above-described embodiment is only for clearly demonstrating example of the present invention, and also
The non-restriction to embodiment.For those of ordinary skill in the field, can also do on the basis of the above description
Go out change or the variation of other multi-form.Here without also cannot all of embodiment be given exhaustive.And thus drawn
What Shen went out obviously changes or changes among still in protection scope of the present invention.
Claims (10)
1. a processing method for useless hydrogenation catalyst, comprises the steps:
Step A, carries out useless hydrogenation catalyst coke-burning regeneration, and is ground by the useless hydrogenation catalyst after regeneration, prepare useless
Hydrogenation catalyst powder；
Step B, prepares lateritic nickel ore powder；
Step C, mixes described useless hydrogenation catalyst powder and described ready lateritic nickel ore powder, adds dust technology and glues
Knot agent, makes serosity；
Step D, by described serosity by spray dryer drying and moulding, is carried out the semi-finished product catalyst after drying and moulding afterwards
Roasting, prepares hydrogenation catalyst.
Method the most according to claim 1, it is characterised in that described coke-burning regeneration process uses nitrogen-air again
Raw method: described useless hydrogenation catalyst is placed in regenerator, is passed through nitrogen and replaces, temperature is slowly raised to 250
～350 DEG C, it being slowly introducing air after constant temperature 3～4h, control the oxygen content 0.3%～0.5% in regenerator, heating rate is 10
～20 DEG C/h, temperature rise to 400 DEG C after constant temperature 2～3h, temperature rises to 500 DEG C of constant temperature to end of making charcoal, and continues after end of making charcoal
Start to cool to room temperature after constant temperature 6h.
Method the most according to claim 1, it is characterised in that in described step B, lateritic nickel ore is ground broken and
Obtaining lateritic nickel ore powder, the particle size of this powder is below 5 μm, preferably 2～3 μm.
Method the most according to claim 1 and 2, it is characterised in that described useless hydrogenation catalyst is that aperture is big, carbon deposit is many,
The useless hydrogenation catalyst that metal deposit is few, the most residue fixed-bed hydrodesulfurization is given up agent.
Method the most according to claim 1, it is characterised in that the particle size of described useless hydrogenation catalyst powder is 5 μm
Hereinafter, preferably 2～3 μm.
Method the most according to claim 1, it is characterised in that based on the percentage by weight accounting for total solid material, described
Lateritic nickel ore powder is 10%～20%, and binding agent is 10%, and useless hydrogenation catalyst powder is 70%～80%；Wherein dust technology
Content is the 5%～15% of total solid material.
Method the most according to claim 1, it is characterised in that contain by weight percentage in described lateritic nickel ore powder
The nickel oxide of 1%～3% and the ferrum oxide of 10%～20%.
Method the most according to claim 1, it is characterised in that the particle diameter of the semi-finished product catalyst in described step D is 75
～150 μm；Described sintering temperature is 400～450 DEG C, roasting time 4～6h.
Method the most according to claim 1, it is characterised in that described binding agent is Alumina gel；Before described step A,
Also described useless hydrogenation catalyst is carried out pretreatment: utilize toluene extracting to remove the oil product that this useless hydrogenation catalyst is adsorbed, and
Being dried at 100～120 DEG C, drying time is 1.5～2.5h.
10. the serosity that prepared by the processing method of the useless hydrogenation catalyst that one of claim 1 to 9 is described, comprising: laterite
Nickel minerals powder, useless hydrogenation catalyst powder, binding agent and dust technology；
Wherein, based on the percentage by weight accounting for total solid material, described lateritic nickel ore powder is 10%～20%, and binding agent is
10%, dead catalyst powder is 70%～80%；Wherein dust technology content is the 5%～15% of total solid material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107233887A (en) * | 2017-06-09 | 2017-10-10 | 太原理工大学 | A kind of preparation method and application of the catalyst of hydrogenation of dinitro toluene synthesis toluencediamine |
| CN107737591A (en) * | 2017-09-22 | 2018-02-27 | 北京华福工程有限公司 | Catalyst for heavy oil floating bed hydrogenation pretreatment and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107233887A (en) * | 2017-06-09 | 2017-10-10 | 太原理工大学 | A kind of preparation method and application of the catalyst of hydrogenation of dinitro toluene synthesis toluencediamine |
| CN107233887B (en) * | 2017-06-09 | 2020-10-13 | 太原理工大学 | Preparation method and application of catalyst for synthesizing toluenediamine by hydrogenating dinitrotoluene |
| CN107737591A (en) * | 2017-09-22 | 2018-02-27 | 北京华福工程有限公司 | Catalyst for heavy oil floating bed hydrogenation pretreatment and preparation method thereof |
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Application publication date: 20161123 |