CN108816295A - A kind of high-nickel catalyst activation method - Google Patents
A kind of high-nickel catalyst activation method Download PDFInfo
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- CN108816295A CN108816295A CN201810590601.0A CN201810590601A CN108816295A CN 108816295 A CN108816295 A CN 108816295A CN 201810590601 A CN201810590601 A CN 201810590601A CN 108816295 A CN108816295 A CN 108816295A
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- 230000004913 activation Effects 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000012190 activator Substances 0.000 claims abstract description 73
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims description 23
- 239000001257 hydrogen Substances 0.000 claims description 23
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 21
- 229920006395 saturated elastomer Polymers 0.000 claims description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 230000003213 activating effect Effects 0.000 claims description 7
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 230000013011 mating Effects 0.000 claims description 3
- 239000000567 combustion gas Substances 0.000 claims description 2
- 230000008859 change Effects 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 3
- 230000001351 cycling effect Effects 0.000 abstract description 2
- 238000001994 activation Methods 0.000 description 41
- 239000003054 catalyst Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 238000004064 recycling Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000005984 hydrogenation reaction Methods 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 150000001993 dienes Chemical class 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000011143 downstream manufacturing Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- B01J38/10—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst using elemental hydrogen
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The present invention provides a kind of high-nickel catalyst activation method, includes the following steps：S1, high-nickel catalyst are lived again：The high-nickel catalyst for entering latter stage is added in reaction kettle, and control the temperature and pressure of reaction kettle, it is passed through activator, being passed through the time is not less than 36h, after to be activated, activator and high-nickel catalyst are separated for the activation for carrying out high-nickel catalyst, the high-nickel catalyst completed up to activation and the activator that has used, activate completion high-nickel catalyst be dried in vacuo after can reuse；S2, activator are lived again：The step S1 isolated activator used is lived again by the method for rectifying, and the activator after living again is lived again for high-nickel catalyst.Activation method proposed by the present invention, good to the activation effect of high-nickel catalyst, significant change does not occur for the high-nickel catalyst molecule crystal form after activation, and duct does not occur obviously to collapse, can continue cycling through using 8000~10000h.
Description
Technical field
The present invention relates to catalyst activation process fields, and in particular to a kind of high-nickel catalyst activation method.
Background technique
High-nickel catalyst refers to the catalyst that nickel content is higher than 22%, main frequently as the anti-catalyst of oil hydrogenation one
Acting on is to carry out adding hydrogen for oil product unsaturated carbon four, light dydrocarbon, carbon six, and diene all adds Qing , Unit alkene partial hydrogenation, nickelic to urge
The service life of agent is 12000h, and in catalyst latter stage, high-nickel catalyst diolefin hydrogenation rate is lower, and diolefin hydrogenation is not thorough, one
Anti- product can not as hydrogenating materials carry out using.
After high-nickel catalyst enters latter stage, product is unable to satisfy downstream process raw materials for production requirement, at present most common means
For more catalyst changeout, recyclings can only be reached by recycling wherein noble metal after catalyst change, re-using cost is larger.Electricity
Under sub- microscope, destructive destruction does not occur for catalyst nickel structure and duct, can using the method lived again to catalyst into
Row activates, and activation temperature used in traditional activation of catalyst is 450~520 DEG C, but such method is directed to high-nickel catalyst,
It is easy to cause high-nickel catalyst crystal form aggregation duct to damage and need to live again using other methods.Based on this, the present invention proposes one
Kind high-nickel catalyst activation method.
Summary of the invention
The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of high-nickel catalyst proposed is lived
Change method.
In order to achieve the above object, the present invention is achieved by the following technical programs：
A kind of high-nickel catalyst activation method, includes the following steps：
S1, high-nickel catalyst are lived again：The high-nickel catalyst for entering latter stage is added in reaction kettle, and controls reaction kettle
Temperature and pressure, be passed through activator, be passed through the time be not less than 36h, carry out the activation of high-nickel catalyst, end to be activated
Afterwards, activator and high-nickel catalyst separation have been activated to get the high-nickel catalyst completed and the activator used is activated
At high-nickel catalyst be dried in vacuo after can reuse；
S2, activator are lived again：The step S1 isolated activator used carries out weight by the method for rectifying
It is raw, activator the living again for high-nickel catalyst after living again.
Preferably, the temperature of the reaction kettle is 180~240 DEG C.
Preferably, the pressure of the reaction kettle is 2.5MPa.
Preferably, the activator be C4~C8 saturated alkane in any one, and the temperature of reaction kettle be 220~
240℃。
Preferably, the activator is any one in the saturated alkane of C5~C7.
Preferably, when the activator is C4 saturated alkane, activator is passed through the time not less than 72h.
Preferably, when the activator is C8 saturated alkane, activator is passed through the time not less than 36h.
Preferably, the activator is purity in 99% or more hydrogen, and activator is passed through the time not less than 36h.
Preferably, the activator is hydrogen of the purity 99% or more, and the temperature of reaction kettle for activating high-nickel catalyst is
180~200 DEG C, activating the hydrogen used and duration is recycled is more than that 2h then needs to release hydrogen, introduces new hydrogen.
Preferably, the activator is hydrogen of the purity 99% or more, and subsequent technique uses filtering surge tank, and mating
Hydrogen flare system serves as conduction oil combustion gas use.
The present invention provides a kind of high-nickel catalyst activation method, and advantage is compared with prior art：
1, activation method proposed by the present invention is low in cost, and the processing method in traditional high-nickel catalyst latter stage is avoided to lead
The catalyst change operation difficulty of cause is big, and the catalyst of replacement can only recycle noble metal therein, the low problem of recovery utilization rate,
And the high-nickel catalyst for entering latter stage is effectively activated through activation method proposed by the present invention, nickelic catalysis after activation
Significant change does not occur for the molecule crystal form of agent, and obviously collapsing does not occur in high-nickel catalyst duct, can be to high-nickel catalyst surface
Colloid and enrichment carbon are effectively removed, and the high-nickel catalyst that activated method activates can continue cycling through using 8000~
10000h；
2, the temperature of activation method strict control activation proposed by the present invention, guarantees activation of the activator to high-nickel catalyst
Effect, when activator is the saturated alkane of C4~C8, the temperature of bacterium activation reaction kettles is controlled at 220~240 DEG C, and temperature is too low,
Activating velocity is too slow, and temperature is excessively high, causes irreversible breaking-up to catalyst duct；When activator is hydrogen of the purity 99% or more
When gas, the temperature of bacterium activation reaction kettles is controlled at 180~200 DEG C, and temperature is too low, and activating velocity is too slow, and temperature is excessively high, hydrogen temperature
It is not easy to control；
3 and test proves that, saturated alkane activation it is best with C5-C7, C4 also has activation effect, but molten in C4
Xie Qing is less, significantly extends the time required for activating, larger more than the difficulty that heavy constituent after C7 lives again to activator, lives again
Need to consume biggish energy consumption；
4, the pressure of activation method strict control activation proposed by the present invention is 2.5MPa, the experiment proved that pressure is higher than this
Not easy to control, pressure is lower than this, and activator dissolved hydrogen is less, is not easy to contact with the colloid on high-nickel catalyst surface and enrichment carbon,
It influences nickelic activator surface colloid and is enriched with the removing of carbon, the time required to significantly extending activation；
5, activation method proposed by the present invention, no three wastes generates in activation process, and by-product is few, and the present invention mentions
Activation method out applies also for the activation of tungsten, molybdenum catalyst.
Specific embodiment
Combined with specific embodiments below the present invention is made further to explain.
Embodiment one
A kind of high-nickel catalyst activation method proposed by the present invention, includes the following steps：
S1, high-nickel catalyst are lived again：The high-nickel catalyst for entering latter stage is added in reaction kettle, and controls reaction kettle
Temperature be 220 DEG C, pressure 2.5MPa is passed through the saturated alkane of C4, be passed through the time be 72h, carry out the work of high-nickel catalyst
Change, after to be activated, high-nickel catalyst that activator and high-nickel catalyst separation are completed to get activation and has used
Activator, activate completion high-nickel catalyst be dried in vacuo after can reuse；
S2, activator are lived again：The step S1 isolated activator used carries out weight by the method for rectifying
It is raw, activator the living again for high-nickel catalyst after living again.
Embodiment two
A kind of high-nickel catalyst activation method proposed by the present invention, includes the following steps：
S1, high-nickel catalyst are lived again：The high-nickel catalyst for entering latter stage is added in reaction kettle, and controls reaction kettle
Temperature be 220 DEG C, pressure 2.5MPa is passed through the saturated alkane of C8, be passed through the time be 36h, carry out the work of high-nickel catalyst
Change, after to be activated, high-nickel catalyst that activator and high-nickel catalyst separation are completed to get activation and has used
Activator, activate completion high-nickel catalyst be dried in vacuo after can reuse；
S2, activator are lived again：The step S1 isolated activator used carries out weight by the method for rectifying
It is raw, activator the living again for high-nickel catalyst after living again.
Embodiment three
A kind of high-nickel catalyst activation method proposed by the present invention, includes the following steps：
S1, high-nickel catalyst are lived again：The high-nickel catalyst for entering latter stage is added in reaction kettle, and controls reaction kettle
Temperature be 180 DEG C, pressure 2.5MPa, be passed through hydrogen of the purity 99% or more, being passed through the time is 48h, nickelic urges
The activation of agent, after to be activated, by activator and high-nickel catalyst separation to get the high-nickel catalyst for activating completion and
Activator through using, activate completion high-nickel catalyst be dried in vacuo after can reuse；
S2, activator are lived again：The step S1 isolated activator used carries out weight by the method for rectifying
It is raw, activator the living again for high-nickel catalyst after living again.
In the present invention, equipped with filtering surge tank, mating hydrogen flare system, it is super to activate the hydrogen recycling duration used
It crosses 2h then to need to release hydrogen, introduces new hydrogen.
Comparative example one
The time that activator is passed through in embodiment one is changed to 70h, other conditions are the same as embodiment one.
Comparative example two
The time that activator is passed through in embodiment two is changed to 34h, other conditions are the same as embodiment two.
Comparative example three
Activator in embodiment three is passed through the time to be changed to 34 hours, other conditions are the same as embodiment three.
Comparative example four
Activator in embodiment three is passed through the time to be changed to 36 hours, other conditions are the same as embodiment three.
Respectively to embodiment one, embodiment two, embodiment three, comparative example one, comparative example two, comparative example three and comparative example four
High-nickel catalyst after activation processing carries out catalytic cycle and uses time test, the results are shown in Table 1.
Table 1：
Table 1 is the results show that the high-nickel catalyst after embodiment one, embodiment two and embodiment three activation processing can follow
Ring uses between 8783~10000h, hence it is evident that higher than the recycling of comparative example one, comparative example two, comparative example three and comparative example four
Time shows that the time that is passed through of activator in activation method proposed by the present invention can significantly affect the activation effect of activator,
When activator is C4 saturated alkane, the time that is passed through of activator is not thorough lower than 72h activation, when activator is C8 saturated alkane
When, the time that is passed through of activator is not thorough lower than 36h activation, when activator is hydrogen of the purity 99% or more, activator
Be passed through the time lower than 36h activation be not thorough.
Activator in embodiment one is successively changed to C5 saturated alkane, C6 saturated alkane, C7 saturated alkane, C8 saturation
Alkane, C9 saturated alkane and C10 saturated alkane carry out the activation of high-nickel catalyst, other operations are as in the first embodiment, and to activation
High-nickel catalyst afterwards carries out recycling time test, the results are shown in Table 2.
Table 2：
Table 2 the results show that with C number in saturated alkane increase, when the recycling of treated high-nickel catalyst
Between increase, after C number is more than 8, though the recycling time of activator is promoted, but biggish energy consumption need to be expended, so
Comprehensive performance of the activator between C4~C8 is preferable, and wherein the performance of C5~C7 is best.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of high-nickel catalyst activation method, which is characterized in that include the following steps：
S1, high-nickel catalyst are lived again：The high-nickel catalyst for entering latter stage is added in reaction kettle, and controls the temperature of reaction kettle
Degree and pressure, are passed through activator, and being passed through the time is to carry out the activation of high-nickel catalyst not less than 36h, will after to be activated
Activator and high-nickel catalyst separation activate completion to get the high-nickel catalyst completed and the activator used is activated
High-nickel catalyst can reuse after being dried in vacuo；
S2, activator are lived again：The step S1 isolated activator used is lived again by the method for rectifying, weight
Activator living again for high-nickel catalyst after life.
2. a kind of high-nickel catalyst activation method according to claim 1, which is characterized in that the temperature of the reaction kettle
It is 180~240 DEG C.
3. a kind of high-nickel catalyst activation method according to claim 1, which is characterized in that the pressure of the reaction kettle
For 2.5MPa.
4. a kind of high-nickel catalyst activation method according to claim 1, which is characterized in that the activator be C4~
Any one in the saturated alkane of C8, and the temperature of reaction kettle is 220~240 DEG C.
5. a kind of high-nickel catalyst activation method according to claim 1 or 4, which is characterized in that the activator is
Any one in the saturated alkane of C5~C7.
6. a kind of high-nickel catalyst activation method according to claim 1 or 4, which is characterized in that the activator is
When C4 saturated alkane, activator is passed through the time not less than 72h.
7. a kind of high-nickel catalyst activation method according to claim 1 or 4, which is characterized in that the activator is
When C8 saturated alkane, activator is passed through the time not less than 36h.
8. a kind of high-nickel catalyst activation method according to claim 1, which is characterized in that the activator is purity
In 99% or more hydrogen, activator is passed through the time not less than 36h.
9. a kind of high-nickel catalyst activation method according to claim 1 or 8, which is characterized in that the activator is
Hydrogen of the purity 99% or more, the temperature of reaction kettle for activating high-nickel catalyst is 180~200 DEG C, activates the hydrogen used and follows
Ring is more than that 2h then needs to release hydrogen using duration, introduces new hydrogen.
10. a kind of high-nickel catalyst activation method according to claim 9, which is characterized in that subsequent technique used
Filter surge tank, and mating hydrogen flare system or serve as conduction oil combustion gas use.
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| CN201810590601.0A CN108816295A (en) | 2018-06-09 | 2018-06-09 | A kind of high-nickel catalyst activation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111925270A (en) * | 2020-08-20 | 2020-11-13 | 濮阳市联众兴业化工有限公司 | Preparation method of high-efficiency polyolefin refrigerant |
| CN119281333A (en) * | 2024-09-24 | 2025-01-10 | 濮阳市联众兴业化工有限公司 | A supported catalyst and its application in preparing isopropylamine from acetone |
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| CN119281333A (en) * | 2024-09-24 | 2025-01-10 | 濮阳市联众兴业化工有限公司 | A supported catalyst and its application in preparing isopropylamine from acetone |
| CN119281333B (en) * | 2024-09-24 | 2025-12-02 | 濮阳市联众兴业化工有限公司 | A supported catalyst and its application in the preparation of isopropylamine from acetone. |
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Application publication date: 20181116 |