CN105170195B - Shaping of catalyst method - Google Patents
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- CN105170195B CN105170195B CN201510581762.XA CN201510581762A CN105170195B CN 105170195 B CN105170195 B CN 105170195B CN 201510581762 A CN201510581762 A CN 201510581762A CN 105170195 B CN105170195 B CN 105170195B
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Abstract
The present invention provides a kind of shaping of catalyst methods, belong to catalyst field.The shaping of catalyst method will not destroy the active site of catalyst during shaping of catalyst, can avoid making the catalytic activity of catalyst after molding from reducing.The shaping of catalyst method includes the following steps：Catalyst powder is mixed with alkaline binding agent to obtain wet feed group, wherein, the alkalinity binding agent includes at least one of alkaline silica sol, alkaline Aluminum sol；The wet feed is rolled into a ball and carries out forming processes.The present invention can be used for shaping of catalyst.
Description
Technical field
The present invention relates to catalyst field more particularly to a kind of shaping of catalyst methods.
Background technology
Solid catalyst needs to have specific shape and size in actual use to adapt to catalytic reactor, because
And solid catalyst usually all first will pass through forming processes to obtain specific shape and size before actual use, and catalyst
Forming processes and the activity of catalyst are closely coupled, have a significant impact to the catalytic activity of catalyst, so the molding of catalyst
Processing seems extremely important in catalyst preparation.
Many influence factors involved in shaping of catalyst process, wherein the binding agent used in forming process is often right
Subsequent catalyst performance causes great influence.For example, catalyst is usually used in forming process in the prior art intends thin water
Aluminium stone and nitric acid as binding agent, the binding agent can make catalyst powder be molded well and catalyst after molding have very
High mechanical strength, however nitric acid is all extremely strong strong acid of a kind of oxidisability and corrosivity, the activity of meeting corrosion failure catalyst
Site, and need to carry out high-temperature calcination after shaping to eliminate nitric acid, this causes partial catalyst to be sintered, and further breaks
Active catalyst sites are broken, and destroy the pore structure after shaping of catalyst, reduce catalyst activity after molding.
Invention content
The present invention provides a kind of shaping of catalyst methods, and the active site of catalyst will not be destroyed in forming process,
It can avoid making the catalytic activity of catalyst after molding from reducing.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
The present invention provides a kind of shaping of catalyst method, specifically includes following steps:
Catalyst powder mix with alkaline binding agent to obtain wet feed group, wherein, alkaline binding agent be alkaline silica sol,
At least one of alkaline Aluminum sol；The wet feed is rolled into a ball and carries out forming processes.
Wherein, the solid content of the alkaline binding agent is not less than 30%.
In terms of catalyst powder weight, the additive amount of the alkalinity binding agent is 50~150%.
Specifically, it is further included later in described mix catalyst powder with alkaline binding agent：Add in neutral binding agent into
Row mixes again；Wherein, the neutral binding agent includes at least one of starch solution or polyglycol solution.
Preferably, the ratio between the additive amount of the neutral binding agent and the additive amount of the alkaline binding agent are 1:1~1:8.
The mass fraction of the starch solution or polyglycol solution is 30~50%.
Further, it is described catalyst powder is mixed with alkaline binding agent before further include：By catalyst powder with
Extrusion aid is mixed.
Further, it is further included later in described mix catalyst powder with alkaline binding agent：Expanding agent is added in carry out
It mixes again.
Wherein, the expanding agent includes at least one of ammonium carbonate, ammonium hydrogen carbonate or urea；Alternatively, the expanding agent
Including at least one of starch solution or polyglycol solution.
Specifically, in terms of catalyst powder weight, the additive amount of the expanding agent is 10%~30%.
The present invention provides a kind of shaping of catalyst method, using one kind in alkaline silica sol, alkaline Aluminum sol or several
Kind carries out forming processes, since catalyst is with simple substance or oxide as binding agent after being sufficiently mixed with catalyst powder
Form, which is carried on carrier, forms activated centre, with prior art generally use nitric acid and boehmite as binding agent phase
Than alkaline silica sol of the invention, alkaline Aluminum sol will not be chemically reacted as nitric acid with catalyst, corrode catalyst
Activated centre, thus the present invention can avoid making the activity of catalyst after molding from reducing；Moreover, at the forming site during reason only
Need to carry out appropriate drying can remove impurity component, without carrying out high-temperature calcination, thus will not make sintering of catalyst or
The pore structure after shaping of catalyst is destroyed, further avoids making the activity of catalyst after molding from reducing.
Description of the drawings
Fig. 1 is the process flow chart of shaping of catalyst method provided in an embodiment of the present invention；
Fig. 2 is another process flow chart of shaping of catalyst method provided in an embodiment of the present invention.
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other without making creative work
Embodiment shall fall within the protection scope of the present invention.
As shown in Figure 1, the embodiment of the present invention provides a kind of shaping of catalyst method, specifically may comprise steps of:
S1, catalyst powder is mixed with alkaline binding agent to obtain wet feed group, wherein, alkaline binding agent includes alkaline silicon
At least one of colloidal sol, alkaline Aluminum sol；
S2, obtained wet feed is rolled into a ball to progress forming processes.
An embodiment of the present invention provides a kind of shaping of catalyst method, using one in alkaline silica sol, alkaline Aluminum sol
Kind is several as binding agent, forming processes is carried out after being sufficiently mixed with catalyst powder, since catalyst is with oxide
Form, which is carried on carrier, forms activated centre, with prior art generally use nitric acid and boehmite as binding agent phase
Than alkaline silica sol of the invention, alkaline Aluminum sol will not be chemically reacted as nitric acid with catalyst oxide, be corroded
The activated centre of catalyst, thus the present invention can avoid the reduction for the activity for making catalyst after molding；Moreover, at the forming site
Only need to carry out appropriate drying can remove impurity component during reason, without carrying out high-temperature calcination, thus will not make catalysis
Agent is sintered or destroys the pore structure after shaping of catalyst, further avoids making the activity of catalyst after molding from reducing.
It should be noted that the catalyst powder can be noble metal and its oxide catalyst, such as platinum base catalysis
Agent；It can also be transition-metals and their oxides catalyst, such as nickel-base catalyst.
In step S1, alkaline binding agent can be that one or more of alkaline silica sol, alkaline Aluminum sol are to say this hair
Bright applicable alkaline binding agent can be alkaline silica sol or alkaline Aluminum sol, can also be alkaline silica sol and alkalinity
The mixture of Aluminum sol.
Wherein, the solid content of alkaline binding agent be not less than 30%, preferably can be 30~50%, such as can be 30%,
35%th, 40%, 45%, 50% etc..Specifically, the solid content of alkaline silica sol refers to the content of silica in Ludox,
The solid content of alkaline Aluminum sol refers to the content of alundum (Al2O3) in Aluminum sol, in this way, colloidal sol can have extraordinary glue
Degree, dispersibility and permeability are all preferable when so that the colloidal sol mix with catalyst powder, and ought make subsequently through drying process
During moisture evaporation, sol particles can be securely attached to catalyst powder surface, well bonding catalyst powder.
The additive amount of alkaline binding agent should not be very little, can lead to that catalyst powder molding bonded well cannot be made very little；
Also it is unsuitable too many, the active particle of dry rear catalyst can be caused to be wrapped up by binding agent too much and covered, reduce catalyst activity.
In an embodiment of the present invention, in terms of catalyst powder weight, the additive amount of alkaline binding agent can be 50~150%, such as
Can be 50%, 70%, 80%, 90%, 100%, 125%, 130%, 150% etc..
In step sl, can also include before catalyst powder is mixed with alkaline binding agent：By catalyst powder
It is mixed with extrusion aid.That is, can first mix catalyst powder with extrusion aid, then add in alkalinity and bond
Agent is mixed again, to obtain wet feed group.
As shown in Fig. 2, first with extrusion aid be sufficiently mixed for the first time by catalyst powder, alkaline binding agent is then added in
It is sufficiently mixed for the second time.Extrusion aid can play the role of lubrication, and addition extrusion aid contributes between reduction material particles
And the friction between material particles and former, it is avoided to be broken in forming process, and can make catalyst into
The smooth impulse- free robustness of type rear surface.
Wherein, extrusion aid can be specifically one or more of sesbania powder, magnesium stearate or dried starch.It is sesbania powder, hard
Fatty acid magnesium or dried starch both have good lubricating action, and can be removed by drying in the follow-up process, can avoid helping
Squeeze pollution of the agent to catalyst.
Specifically, in terms of catalyst powder weight, the additive amount of extrusion aid can be 3%~5%, such as 3%, 3.5%,
4%th, 5% etc..Contribute to shaping of catalyst in this way, and there is smooth surface shape after making shaping of catalyst.
In a preferred embodiment, can also include after catalyst powder is mixed with alkaline binding agent：
Neutral binding agent is added in be mixed again.That is, first catalyst powder can be mixed with alkaline binding agent, so
Neutral binding agent is added in afterwards to be mixed to obtain wet feed group again.
Further, as shown in Fig. 2, being first sufficiently mixed catalyst powder and extrusion aid, alkaline binding agent is then added in
It is sufficiently mixed for the second time, then can also add in neutral binding agent and be sufficiently mixed for the third time, finally obtain wet feed group.
Wherein, applicable neutral binding agent can include starch solution or PEG (polyethylene glycol, polyethylene
Glycol) one or more of solution.Starch solution or PEG solution can play the role of binding agent, can uniformly disperse
In the mixed system formed in alkaline binding agent and catalyst, filling and supporting role are played after wet feed rolls into a ball shaping and drying,
It is cooperated with Ludox or Aluminum sol, improves the mechanical strength of catalyst after molding.
For starch solution or PEG solution make neutral binding agent, the mass fraction of starch solution or PEG solution can be
30~50%, such as 30%, 45%, 50% etc..
It should be noted that starch, which is only dissolved in, can just play the role of binding agent when water forms starch solution, and form sediment
Powder does not dissolve in cold water, needs to be configured with the hot water at 40~60 DEG C.
Wherein, the ratio between the additive amount of neutral binding agent and the additive amount of alkaline binding agent can be 1:1~1:8, such as can
Think 1:1、1:2、1:4、1:5、1:7、1:8 etc..If this ratio is more than 1:1, that is, the additive amount of neutral binding agent is big
In the additive amount of alkaline binding agent, the then mixed system for being distributed to that alkaline binding agent is formed with catalyst in neutral binding agent
When, alkaline binding agent can be made excessively to disperse with catalyst, catalyst after molding is caused to cave in use, it is impossible to keep
Required shape；And if this ratio is less than 1:8, that is, additive amount the adding less than 1/8 alkaline binding agent of neutral binding agent
Dosage then leads to wet feed group after shaping and drying, and neutral binding agent does not have enough filling and supporting role, is unfavorable for carrying
The mechanical strength of high catalyst after molding.
In order to improve the specific surface area of catalyst, the catalytic activity of catalyst is further improved, it can be first by catalyst powder
Body is mixed with alkaline binding agent, is then added in expanding agent and is mixed to obtain wet feed group again.
The process is specifically as follows：After adding in alkaline binding agent and carrying out second mixing, expanding agent can also be added in
Third time mixing is carried out to obtain wet feed group；Alternatively, as shown in Fig. 2, after adding in neutral binding agent and carrying out third time mixing,
Expanding agent is added in again carries out the 4th mixing to obtain wet feed group.
In an embodiment of the present invention, expanding agent preferably can be one kind or several in ammonium carbonate, ammonium hydrogen carbonate or urea
Kind, these expanding agents have alkalescent, will not be chemically reacted with metal oxide, because of the activity without destroying catalyst
Site, and be easily removed in the follow-up process, the pollution to catalyst can be avoided.
In terms of catalyst powder weight, the additive amount of expanding agent can be 10%~30%, such as 10%, 15%, 20%,
30% etc..Suitable small structure can be both generated in this way, increase specific surface area, and have after also can ensure that shaping of catalyst
Enough mechanical strengths.
It should be noted that neutral binding agent switchs to gas in the drying process due to being easy to, thus it also is used as reaming
Agent.When the mass fraction of starch solution or PEG solution is smaller, such as 10%~30%, at this point, starch solution or PEG solution
At least one of be also used as expanding agent；And when its mass fraction is larger, it is as described above 30~50%, leads at this time
Play the role of binding agent, can cooperate with Ludox or Aluminum sol, enhance the mechanical strength after shaping of catalyst.
In step s 2, the forming processes refer to wet feed group being added in shaping of catalyst equipment with obtain it is spherical,
Catalytic reactor requires the shape that it should have to the catalyst such as bar shaped in actual use, then again by dry
Reason then can also pass through the size finally to be wanted such as broken, sieving.The former can be extruder, such as
Screw-type extruder.
As shown in Fig. 2, obtained wet feed group can be put in extrusion in banded extruder, then obtained catalyst wet bar is existed
It is dried at 60~150 DEG C, it is about 24~48 hours dry, it then crushes, be sieved, you can obtain the catalysis of final molding
Agent.
It is further detailed with specific embodiment below preferably to state shaping of catalyst method provided in an embodiment of the present invention
It describes in detail bright.Wherein, used extrusion aid, binding agent and expanding agent etc. all can be commercial product.
Embodiment 1
1st, 200g nickel-base catalysts powder, 10g sesbania powders are first sufficiently mixed.
2nd, 50% alkaline silica sols of 100g are added in be sufficiently mixed again, obtains wet feed group.
3rd, after wet feed group being put into banded extruder extrusion, 100 DEG C of dryings are for 24 hours.
4th, it crushes, be sieved.
Embodiment 2
1st, 200g nickel-base catalysts powder, 10g sesbania powders are first sufficiently mixed
2nd, 50% alkaline silica sols of 100g are added in be sufficiently mixed again.
3 then add 50% starch solutions of 80g carry out third time mixing.
4th, 20g ammonium carbonates are eventually adding and carry out the 4th mixing, obtain wet feed group.
5th, after wet feed group being put into banded extruder extrusion, 100 DEG C of dryings are for 24 hours.
6th, it crushes, be sieved.
Embodiment 3
1st, 200g nickel-base catalysts powder, 6g magnesium stearates are first sufficiently mixed
2nd, the alkaline Aluminum sol of 30% alkaline silica sols of 200g, 100g 30% is added in be sufficiently mixed again.
3 then add 30% starch solutions of 20g, 20g 50% PEG solution carry out third time mixing
4th, be eventually adding 30g ammonium hydrogen carbonate, 30g urea carry out the 4th time mixing, obtain wet feed group.
5th, after wet feed group being put into banded extruder extrusion, 100 DEG C of dryings are for 24 hours.
6th, it crushes, be sieved.
Embodiment 4
1st, 200g nickel-base catalysts powder, 4g sesbania powders, 4g magnesium stearates are first sufficiently mixed
2nd, the alkaline Aluminum sols of 200g 50% are added in be sufficiently mixed again.
3 then add 100g 30% PEG solution carry out third time mixing.
4th, 20g ammonium carbonates are eventually adding, 20g urea carry out the 4th time mixing, obtain wet feed group.
5th, after wet feed group being put into banded extruder extrusion, 100 DEG C of dryings are for 24 hours.
6th, it crushes, be sieved.
Embodiment 5
1st, 200g nickel-base catalysts powder, 2g sesbania powders, 4g magnesium stearates, 4g dried starch are first sufficiently mixed
2nd, the alkaline Aluminum sol of 40% alkaline silica sols of 100g, 100g 40% is added in be sufficiently mixed again.
3 then add 40% starch solutions of 50g, 50g 40% PEG solution carry out third time mixing.
4th, 10g ammonium carbonates are eventually adding, 10g ammonium hydrogen carbonate carry out the 4th time mixing, obtain wet feed group.
5th, after wet feed group being put into banded extruder extrusion, 100 DEG C of dryings are for 24 hours.
6th, it crushes, be sieved.
Comparative example
1st, 200g nickel-base catalysts powder, 40g boehmites, 10g sesbania powders are first sufficiently mixed
2nd, the dilute nitric acid solution for adding in 100mL 10% is sufficiently mixed again, obtains wet feed group.
3rd, after wet feed group being put into banded extruder extrusion, 100 DEG C of dryings are for 24 hours.
4th, dried catalyst item is placed at 500 DEG C and calcined 4 hours.
5th, it crushes, be sieved.
Performance test
Each 2g of catalyst that above example and comparative example is taken to prepare, is packed into reactor, after being warming up to 500 DEG C of reaction temperature
It is passed through flow and is the methane gas of 76ml/min, while be passed through water flow 0.15ml/min, make molar ratio H2O/CH4=2.5,200
DEG C evaporation after and methane gas mixing, by catalyst bed carry out reforming reaction, test 500 DEG C when reforming effect, it is as follows
Table.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example | |
| Methane conversion | 30.8% | 31.2% | 30.5% | 29.4% | 29.8% | 20.3% |
According to table 1 as can be seen that Examples 1 to 5 is compared with comparative example, methane conversion has at least been higher by 47%, thus
As it can be seen that remaining active catalyst sites well using shaping of catalyst method provided in an embodiment of the present invention, effectively avoid
Reduce the catalytic activity of catalyst after molding.
Obviously, the above embodiments are merely examples for clarifying the description, and is not intended to limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation thus extended out or
Change the protection domain still in the invention.
Claims (9)
- A kind of 1. shaping of catalyst method, which is characterized in that include the following steps：Catalyst powder is mixed with alkaline binding agent to obtain wet feed group, wherein, the catalyst powder is noble metal, your gold Belong to oxide, transition metal or transition metal oxide, the alkalinity binding agent is included in alkaline silica sol, alkaline Aluminum sol At least one, in terms of catalyst powder weight, the additive amount of the alkalinity binding agent is 70~150%；The wet feed is rolled into a ball and carries out forming processes, the forming processes are：The obtained wet feed group is put in banded extruder and is squeezed Then obtained catalyst wet bar is dried at 60~150 DEG C for item, 24~48 hours dry, without being calcined, so It crushes, be sieved afterwards, you can obtain the catalyst of final molding.
- 2. shaping of catalyst method according to claim 1, which is characterized in that the solid content of the alkalinity binding agent is not low In 30%.
- 3. shaping of catalyst method according to claim 1 or 2, which is characterized in that described by catalyst powder and alkali Property binding agent mixing after further include：Neutral binding agent is added in be mixed again；Wherein, the neutral binding agent includes starch At least one of solution or polyglycol solution.
- 4. shaping of catalyst method according to claim 3, which is characterized in that in terms of catalyst powder weight, in described Property binding agent the ratio between additive amount and the additive amount of the alkaline binding agent be 1:1~1:8.
- 5. shaping of catalyst method according to claim 3, which is characterized in that the starch solution or polyglycol solution Mass fraction be 30~50%.
- 6. shaping of catalyst method according to claim 1 or 2, which is characterized in that described by catalyst powder and alkali Property binding agent mixing before further include：Catalyst powder is mixed with extrusion aid.
- 7. shaping of catalyst method according to claim 1 or 2, which is characterized in that described by catalyst powder and alkali Property binding agent mixing after further include：Expanding agent is added in be mixed again.
- 8. shaping of catalyst method according to claim 7, which is characterized in that the expanding agent includes ammonium carbonate, carbonic acid At least one of hydrogen ammonium or urea；Alternatively, including at least one of starch solution or polyglycol solution.
- 9. shaping of catalyst method according to claim 7, which is characterized in that in terms of catalyst powder weight, the expansion The additive amount of hole agent is 10%~30%.
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| CN107597099B (en) * | 2017-10-16 | 2020-08-14 | 河南能源化工集团研究总院有限公司 | Forming method of Mg/Sn/W composite oxide catalyst |
| JP7444894B2 (en) | 2019-01-25 | 2024-03-06 | 中国石油化工股▲ふん▼有限公司 | Solid acid catalyst, its production, and its use |
| CN110194665B (en) * | 2019-07-18 | 2022-04-19 | 平顶山市信瑞达石墨制造有限公司 | Graphite cooker and preparation process thereof |
| CN112871173A (en) * | 2021-02-03 | 2021-06-01 | 河南省科学院 | Preparation method of reaction catalyst for preparing synthesis gas by dry reforming of methane and carbon dioxide |
| CN113184919A (en) * | 2021-05-28 | 2021-07-30 | 金川集团股份有限公司 | Preparation method of aluminum-doped cobaltosic oxide |
| CN114768885A (en) * | 2022-05-18 | 2022-07-22 | 常州瑞华化工工程技术股份有限公司 | Extrusion molding method and application of copper acetophenone hydrogenation catalyst |
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| CN1123389C (en) * | 1998-08-26 | 2003-10-08 | 中国科学院大连化学物理研究所 | Preparation of catalyst for preparing low-carbon alcohol by low-carbon oleffine hydration and its application |
| CN101745415B (en) * | 2008-11-28 | 2011-11-02 | 中国石油化工股份有限公司 | Alkaline silica sol composition and application thereof in preparation of cracking catalyst |
| CN101574659A (en) * | 2009-06-15 | 2009-11-11 | 中国科学院山西煤炭化学研究所 | Catalyst for using coal tar to prepare clean fuel oil by catalytic hydrogenation, preparation method and applications |
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