CN108940188A - A kind of preparation method of binder free Siliceous MCM-41 adsorbent of molecular sieve - Google Patents
A kind of preparation method of binder free Siliceous MCM-41 adsorbent of molecular sieve Download PDFInfo
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G5/00—Recovery of liquid hydrocarbon mixtures from gases, e.g. natural gas
- C10G5/02—Recovery of liquid hydrocarbon mixtures from gases, e.g. natural gas with solid adsorbents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/04—Diesel oil
Abstract
The invention discloses a kind of preparation methods of binder free Siliceous MCM-41 adsorbent of molecular sieve, this method comprises: using macropore Siliceous MCM-41 molecular screen primary powder as activated adoption component, binder is added, roller forming, roasts the spheric granules for obtaining particle size range 0.3-0.8mm at drying；Then template, pH adjusting agent, silicon source are sequentially added in deionized water, it stirs evenly at room temperature, above-mentioned spheric granules is added, control liquid-solid ratio=(10~30): 1,80 DEG C of -160 DEG C of static crystallizations -84h for 24 hours, washing is taken out after crystallization to pH=7~8, then drying, roasts to obtain MCM-41 adsorbent of molecular sieve.The present invention is by recrystallizing spheric granules, binder free MCM-41 total silicon molecule sieve adsorbant is made, adsorbent heat stability is high, adsorption capacity is big, diffusion velocity is fast for this, using moving-bed adsorption separating technology, it can be achieved that in diesel component cycloalkane, mononuclear aromatics, polycyclic aromatic hydrocarbon three components separation.
Description
Technical field
The present invention relates to a kind of preparation methods of binder free Siliceous MCM-41 adsorbent of molecular sieve.
Background technique
In recent years due to Global Oil resource increasingly heaviness, in poor quality, catalytic cracking unit processes the ratio of inferior raw material
Example gradually increases, and is substantially increased so as to cause catalytic cracking diesel oil yield, refinery's diesel and gasoline ratio is higher.With domestic consumption diesel and gasoline ratio
Continuous decline, the comprehensive utilization of diesel oil becomes increasingly important.Diesel oil mainly includes straight-run diesel oil, coker gas oil, catalytic cracking
Diesel oil and residual hydrogenation diesel oil, the feature that generally existing arene content is high, Cetane number is low, it is difficult to what satisfaction will be implemented in full
VI diesel oil standard of state.Diesel oil processing mainly by hydrofinishing and adds hydrogen to restructure technology, and Hydrofining Technology hydrogen consumption is excessively high, and nothing
Method increases substantially diesel cetane-number；Add hydrogen restructuring technology to change existing apparatus larger, puts into relatively high, economic benefit
It is unobvious.Using adsorbent of molecular sieve, adsorbing separation is carried out to diesel oil by Simulation moving bed (SMB), obtains high-purity aromatic hydrocarbons
With high-purity naphthenic components, the molecule management of diesel component, more targeted reply changes in market demand, drop may be implemented
Low oil plant diesel and gasoline ratio, increases economic efficiency.
Diesel component is complicated, and movement diameter difference is larger between different component, to improve diffusion velocity and separating degree, needs
The adsorbent of molecular sieve of special pore size distribution size, MCM-41 are a kind of mesopore molecular sieves, the cellular structure that it has six sides orderly, hole
Diameter is uniformly and adjustable between 1~10nm.Large aperture MCM-41 molecular sieve can pass through hydro-thermal process, recrystallization technology and mixing
Surfactant technology obtains, and specific surface area is high, and porosity is high, and adsorption capacity is big, is conducive to organic molecule diffusion, surface is rich in
Faintly acid silicone hydroxyl, without adding active component, alternative Preferential adsorption aromatic hydrocarbon molecule is a kind of excellent adsorbing separation material
Material.But MCM-41 molecular sieve hole wall is thin (< 1nm), and thermal stability is poor, is unfavorable for high-temperature roasting regeneration；SMB adsorptive separation technology needs
The spheric granules adsorbent of certain size range is wanted, adsorbent after molding can generate adsorption capacity containing a large amount of binders
Problem small, the rate of adsorption is low, adsorption effect is poor.
Patent CN103184065A discloses a kind of method of nitrogenous compound in adsorbing and removing diesel oil, and Al-MCM-41 points
Sub- sieve adsorbant and diesel oil keep carrying out contact at 75~110 DEG C in intermittent reaction device or fixed-bed reactor
Denitrogenation is adsorbed, Al-MCM-41 is molecular screen primary powder in patent, and without forming process.Patent CN101381086A is disclosed
A kind of preparation method of Si-MCM-41 mesopore molecular sieve, it is silicon source that this method, which obtains sodium metasilicate using coal ash for manufacturing, and template is added
Agent has both mesoporous and microcellular structure by Si-MCM-41 mesopore molecular sieve prepared by hydro-thermal method, has high specific surface area, reach
1030m2/ g can be used for adsorbing separation metal ion and organic matter, it is also possible to do catalyst carrier.Patent CN1401568A is disclosed
A kind of pressurized thermal water synthetic method of MCM-41 mesoporous molecular sieve, the crystalline substance that template, water, base catalyst, silicon source are mixed to get
Change mother liquor to be put into the autoclave equipped with polytetrafluoroethyllining lining, after pouring nitrogen, system is heated and carries out crystallization, synthesis
MCM-41 molecular sieve heat and hydrothermal stability be improved.
Summary of the invention
The technical problem to be solved by the present invention is to solve presently, there are MCM-41 molecular sieve molded made using binder
Thin at adsorption capacity reduction, diffusion rate reduction, the problem of adsorbing separation effect difference and MCM-41 molecular sieve hole wall, heat is steady
Qualitative difference provides a kind of binder free for diesel oil adsorbing separation the problem of decline for diesel oil adsorbing separation regenerability
The preparation method of Siliceous MCM-41 adsorbent of molecular sieve.
In order to solve the above technical problems, the present invention is achieved through the following technical solutions:
A kind of preparation method of binder free Siliceous MCM-41 adsorbent of molecular sieve, comprising the following steps:
1) form: using Siliceous MCM-41 molecular screen primary powder as activated adoption component, addition binder, roller forming, drying,
Roasting obtains the spheric granules of particle size range 0.3-0.8mm, in spheric granules MCM-41 molecular sieve content be 85wt%~
95wt%；
2) it recrystallizes: template, pH adjusting agent, silicon source being sequentially added in deionized water, stirred evenly at room temperature, mix
The total moles group of object becomes Na2O:SiO2:Q1:H2O=(0.1~0.5): 1:(0.5~1.0): (250~400), wherein Na2O
Represent basicity, Q1 represents template, spheric granules made from addition step 1), liquid-solid ratio=(10~30): 1,80 DEG C~160 DEG C
Static crystallization for 24 hours~84h, washing is taken out after crystallization to pH=7~8, then drying, roast to obtain the absorption of MCM-41 molecular sieve
Agent；
Wherein the Siliceous MCM-41 molecular screen primary powder is greater than 5nm with the calculated aperture of BJH model；
The molding is selected from least one of waterglass, silica solution with binder.
In above-mentioned technical proposal, the template Q1 preferably is selected from ten alkyl trimethyl ammonium bromides, ten alkyl trimethyl chlorinations
At least one of ammonium, dodecyl trimethyl ammonium bromide, dodecyl trimethyl ammonium chloride.
In above-mentioned technical proposal, the silicon source preferably is selected from least one of ethyl orthosilicate, sodium metasilicate, silica solution.
In above-mentioned technical proposal, the crystallization temperature is preferably 100 DEG C~150 DEG C, and crystallization time is preferably 36h~72h.
In above-mentioned technical proposal, the Siliceous MCM-41 molecular screen primary powder is preferably prepared in the following manner:
(1) template, expanding agent are successively dissolved in deionized water, add pH adjusting agent, stirs evenly at room temperature
Solution A；
(2) under stirring condition, silicon source is added slowly in solution A, obtains white gels mixture, makes always rubbing for mixture
You become Na at group2O:SiO2:Q2:E:H2O=(0.05~0.5): 1:(0.1~0.5): (0.1-1.0): (60-150), wherein
Na2O represents basicity, Q2 represents template, E represents expanding agent；
(3) above-mentioned white gels are transferred in reaction kettle and carry out hydro-thermal reaction, 80 DEG C of -160 DEG C of dynamic crystallizations for 24 hours -
84h takes out washing after crystallization to pH=7~8, then drying, roasts to obtain MCM-41 molecular screen primary powder.
In the technical solution of above-mentioned Siliceous MCM-41 molecular screen primary powder, the template Q2 preferably is selected from cetyl triethyl group
Ammonium bromide, cetyl triethyl ammonium chloride, octadecyl triethylammonium bromide, at least one in octadecyl triethyl ammonium chloride
Kind.
In the technical solution of above-mentioned Siliceous MCM-41 molecular screen primary powder, the expanding agent E preferably is selected from 1,3,5- trimethylbenzenes
(TMB), lauryl amine, N, at least one of N- dimethyl hexadecyl base ammonium (DMHA).
The present invention also provides a kind of binder free total silicon molecule sieve adsorbants obtained according to above-mentioned preparation method.
The present invention still further provides a kind of above-mentioned Siliceous MCM-41 adsorbent of molecular sieve and inhales for SMB process selectivity
Method of the Fufen from cycloalkane, mononuclear aromatics and polycyclic aromatic hydrocarbon in diesel component.This method separates product and recycles by rectifying
Strippant respectively obtains the component rich in cycloalkane, mononuclear aromatics and polycyclic aromatic hydrocarbon.
The beneficial effects obtained by the present invention are as follows being:
1) present invention is greater than the large aperture MCM-41 molecular screen primary powder of 5nm using aperture, so that adsorbent is still after recrystallization
Possess sufficiently large main aperture road；Secondly property can be recrystallized using MCM-41 molecular sieve, increases original MCM-41 molecular sieve pores
Wall thickness improves the regenerated stability of adsorbent high-temperature roasting being prepared；
It 2) is effective absorbed component MCM-41 molecular sieve by the binder converted in-situ of forming process addition, increase is prepared into
The adsorbent surface silicone hydroxyl concentration arrived, improves adsorbent adsorption capacity, molecular diffusion rates and adsorbing separation effect；
3) the MCM-41 adsorbent of molecular sieve that the method for the present invention is prepared is applied in moving-bed adsorption separating technology
Cycloalkane, mononuclear aromatics, the multiring aromatic hydrocarbon substance in diesel component can be purified simultaneously, after strippant is recycled in rectifying, produced
For product purity up to 90% or more, it is high cetane number diesel oil that diesel oil, which obtains the paraffinic components of high-purity after absorption purification,
Component can also be used as the processes such as catalytic pyrolysis, catalytic cracking volume increase olefin feedstock.
Specific embodiment
Below with reference to embodiment, technical scheme of the present invention is further explained；
The raw materials used diesel component for removing alkane, composition are shown in Table 2 in embodiment, and Simulation moving bed evaluation result is shown in
Table 3；
Cycloalkane quality × 100% in cycloalkane yield=product cycloalkane quality/feedstock diesel；
Mononuclear aromatics quality × 100% in mononuclear aromatics yield=product mononuclear aromatics quality/feedstock diesel；
Polycyclic aromatic hydrocarbon quality × 100% in polycyclic aromatic hydrocarbon yield=product polycyclic aromatic hydrocarbon quality/feedstock diesel；
Cycloalkane quality/naphthenic components gross mass × 100% in cycloalkane purity=naphthenic components；
Mononuclear aromatics quality/mononuclear aromatics component gross mass × 100% in mononuclear aromatics purity=mononuclear aromatics component；
Polycyclic aromatic hydrocarbon quality/polycyclic aromatic hydrocarbon component gross mass × 100% in polycyclic aromatic hydrocarbon purity=polycyclic aromatic hydrocarbon component.
Embodiment 1
Synthesis: weighing 81.3g cetyltriethylammonium bromide, 48.1gTMB, successively dissolve in 3600g deionized water,
9.6gNaOH is added, at room temperature after mixing evenly, 416.7g ethyl orthosilicate is slowly added dropwise, obtains flat-white gel, is turned
It moves in reaction kettle, 100 DEG C of stirring crystallization 72h, washing is taken out after crystallization to pH=7~8, then drying, roast greatly
Aperture MCM-41 molecular screen primary powder.
Molding: above-mentioned large aperture MCM-41 molecular sieve powder is weighed on sugar coating machine inner rotary table, sprays in rotation plus silicon is molten
Glue solution, silica aqueous solution additive amount are 5wt%-15wt%, and it is 0.3~0.8mm's that partial size is screened out after molding
Particle, then drying, roasting obtain spheric granules.
Recrystallization: 37.6g dodecyl trimethyl ammonium bromide is weighed, 2.0gNaOH, 50.9g ethyl orthosilicate are successively dissolved in
It in 1100g deionized water, stirs evenly at room temperature, above-mentioned 110g molding spheric granules, 100 DEG C of static crystallization 60h, crystallization is added
After take out washing to pH=7~8, then drying, roast to obtain MCM-41 adsorbent of molecular sieve.
Performance evaluation: diesel oil adsorbing separation uses 5th areas, 16 column SMB device, and mononuclear aromatics parses agent and uses methyl cyclohexane
Alkane, polycyclic aromatic hydrocarbon strippant use toluene, and adsorption bed subregion is 4-2-3-5-2, and absorption column temperature is 80-100 DEG C, adsorbent bed
Stressor layer is 0.5~0.8MPa, and switching time is 700~900s, and raw material diesel oil and parsing agent mass velocity ratio are 1:2~1:3,
The volume flow rate ratio of raw material diesel oil and internal circulating load is 1:4~1:5.
Embodiment 2
Synthesis: 180.3g cetyl triethyl ammonium chloride, 136.3g dodecane are weighed, 2160g deionization is successively dissolved in
In water, 16.3gNaOH is added, at room temperature after mixing evenly, 568.4g sodium metasilicate is slowly added, obtains flat-white gel,
It is transferred in reaction kettle, 120 DEG C of stirring crystallization 60h, washing is taken out after crystallization to pH=7~8, then drying, roast
Large aperture MCM-41 molecular screen primary powder.
Molding: above-mentioned large aperture MCM-41 molecular sieve powder is weighed on sugar coating machine inner rotary table, sprays in rotation plus silicon is molten
Glue solution, sodium silicate solution additive amount are 5wt%-15wt%, and it is 0.3~0.8mm's that partial size is screened out after molding
Particle, then drying, roasting obtain spheric granules.
Recrystallization: 89.3g decyl trimethyl ammonium chloride, 4.9gNaOH, 86.9 sodium metasilicate are weighed and is successively dissolved in 2200g and goes
It in ionized water, stirs evenly at room temperature, is added above-mentioned 110g molding spheric granules, 120 DEG C of static crystallization 48h, after crystallization
Washing is taken out to pH=7~8, then drying, roasts to obtain MCM-41 adsorbent of molecular sieve.
Performance evaluation: identical as 1 the method condition of embodiment.
Embodiment 3
Synthesis: 260.6g octadecyl triethylammonium bromide, 144.2gTMB are weighed, 5040g deionized water is successively dissolved in
In, 32gNaOH is added, at room temperature after mixing evenly, is slowly added 122.4g white carbon black, obtains flat-white gel, is shifted
Into reaction kettle, 150 DEG C of stirring crystallization 36h take out washing after crystallization to pH=7~8, then drying, roast to obtain macropore
Diameter MCM-41 molecular screen primary powder.
Molding: above-mentioned large aperture MCM-41 molecular sieve powder is weighed on sugar coating machine inner rotary table, sprays in rotation and adds water glass
Glass aqueous solution, silica aqueous solution additive amount are 5wt%-15wt%, and it is 0.3~0.8mm's that partial size is screened out after molding
Particle, then drying, roasting obtain spheric granules.
Recrystallization: ten alkyl trimethyl ammonium bromide of 51.4g is weighed, 6.3gNaOH, 54.62g ethyl orthosilicate are successively dissolved in
It in 1650g deionized water, stirs evenly at room temperature, above-mentioned 110g molding spheric granules, 150 DEG C of static crystallization 36h, crystallization is added
After take out washing to pH=7~8, then drying, roast to obtain MCM-41 adsorbent of molecular sieve.
Performance evaluation: identical as 1 the method condition of embodiment.
Embodiment 4
Synthesis: 325.1g cetyltriethylammonium bromide, 431.2gDMHA are weighed, 4320g deionized water is successively dissolved in
In, 48gKOH is added, at room temperature after mixing evenly, 416.7g ethyl orthosilicate is slowly added, obtains flat-white gel, is turned
It moves in reaction kettle, 120 DEG C of stirring crystallization 60h, washing is taken out after crystallization to pH=7~8, then drying, roast greatly
Aperture MCM-41 molecular screen primary powder.
Molding: above-mentioned large aperture MCM-41 molecular sieve powder is weighed on sugar coating machine inner rotary table, sprays in rotation and adds water glass
Glass aqueous solution, silica aqueous solution additive amount are 5wt%-15wt%, and it is 0.3~0.8mm's that partial size is screened out after molding
Particle, then drying, roasting obtain spheric granules.
Recrystallization: 154.0g dodecyl trimethyl ammonium chloride is weighed, 9.8gKOH, 52.4g silica solution are successively dissolved in
It in 2750g deionized water, stirs evenly at room temperature, above-mentioned 110g molding spheric granules, 120 DEG C of static crystallization 48h, crystallization is added
After take out washing to pH=7~8, then drying, roast to obtain MCM-41 adsorbent of molecular sieve.
Performance evaluation: identical as 1 the method condition of embodiment.
Embodiment 5
Synthesis: 287.3g octadecyl triethyl ammonium chloride, 102.2g dodecane are weighed, 2880g deionization is successively dissolved in
In water, 11.7gKOH is added, at room temperature after mixing evenly, 568.4g sodium metasilicate is slowly added, obtains flat-white gel, is turned
It moves in reaction kettle, 100 DEG C of stirring crystallization 60h, washing is taken out after crystallization to pH=7~8, then drying, roast greatly
Aperture MCM-41 molecular screen primary powder.
Molding: above-mentioned MCM-41 molecular sieve powder is weighed on sugar coating machine inner rotary table, sprays in rotation plus silica solution is water-soluble
Liquid, sodium silicate solution additive amount are 5wt%-15wt%, and the particle that partial size is 0.3~0.8mm is screened out after molding, then
Drying, roasting obtain spheric granules.
Recrystallization: ten alkyl trimethyl ammonium bromide of 85.8g is weighed, 5.8gNaOH, 144.74g sodium metasilicate are successively dissolved in
It in 2750g deionized water, stirs evenly at room temperature, above-mentioned 110g molding spheric granules, 100 DEG C of static crystallization 48h, crystallization is added
After take out washing to pH=7~8, then drying, roast to obtain MCM-41 adsorbent of molecular sieve.
Performance evaluation: identical as 1 the method condition of embodiment.
Embodiment 6
MCM-41 adsorbent of molecular sieve after performance evaluation in embodiment 1 is subjected to high-temperature roasting, tests adsorbent reactivation
Thermal stability, roasting condition are as follows: air atmosphere, 2 DEG C/min rise to 300 DEG C of holdings 2h, 2 DEG C/min and rise to 550 DEG C of holding 6h, from
So cooling, adsorbent carries out performance evaluation using method condition same as Example 1 after roasting.
Embodiment 7
MCM-41 adsorbent of molecular sieve after performance evaluation in embodiment 2 is subjected to high-temperature roasting, tests adsorbent reactivation
Thermal stability, roasting condition are as follows: air atmosphere, 2 DEG C/min rise to 300 DEG C of holdings 2h, 2 DEG C/min and rise to 550 DEG C of holding 6h, from
So cooling, adsorbent carries out performance evaluation using method condition same as Example 1 after roasting.
Comparative example 1
MCM-41 sieve synthesis procedure, forming process are same as Example 1, without recrystallization process, obtain containing viscous
Tie the MCM-41 adsorbent of agent.
Performance evaluation: identical as 1 the method condition of embodiment.
Comparative example 2
MCM-41 sieve synthesis procedure, forming process are same as Example 2, without recrystallization process, obtain containing viscous
Tie the MCM-41 adsorbent of agent.
Performance evaluation: identical as 1 the method condition of embodiment.
1 MCM-41 adsorbent of molecular sieve physical property of table
2 diesel raw material of table composition
3 embodiment of table and the adsorbent adsorbing separation evaluation result of comparative example preparation
Claims (6)
1. a kind of preparation method of binder free Siliceous MCM-41 adsorbent of molecular sieve, which comprises the following steps:
(1) it forms: using Siliceous MCM-41 molecular screen primary powder as activated adoption component, binder, roller forming, drying, roasting is added
It burns, obtains the spheric granules of particle size range 0.3-0.8mm；Wherein in spheric granules MCM-41 molecular sieve content be 85wt%~
95wt%；
(2) it recrystallizes: template, pH adjusting agent, silicon source being sequentially added in deionized water, stirred evenly at room temperature, mixture
Total moles group become Na2O:SiO2:Q1:H2O=(0.05~0.6): 1:(0.2~1.2): (200~500), wherein Na2O generation
Table basicity, Q1 represent template, spheric granules made from step (1) are added, liquid-solid ratio=(10~30): 1,80 DEG C -160 DEG C quiet
State crystallization -84h for 24 hours takes out washing after crystallization to pH=7~8, then drying, roasts to obtain MCM-41 adsorbent of molecular sieve；
The Siliceous MCM-41 molecular screen primary powder is greater than 5nm with the calculated aperture of BJH model；
The molding is at least one of waterglass, silica solution with binder.
2. the preparation method of Siliceous MCM-41 adsorbent of molecular sieve according to claim 1, which is characterized in that described is complete
Silicon MCM-41 molecular screen primary powder is prepared by the following method:
(1) template, expanding agent are successively dissolved in deionized water, add pH adjusting agent, stir evenly to obtain solution at room temperature
A；
(2) under stirring condition, silicon source is slowly added dropwise into solution A, obtains white gels mixture, makes the total moles group of mixture
As Na2O:SiO2:Q2:E:H2O=(0.02~0.6): 1:(0.05~0.8): (0.05~1.5): (40~200), wherein
Na2O represents basicity, Q2 represents template, E represents expanding agent；
(3) above-mentioned white gels mixture is transferred in reaction kettle and carries out hydro-thermal reaction, 80 DEG C~160 DEG C dynamic crystallizations are for 24 hours
~84h takes out washing after crystallization to pH=7~8, then drying, roasts to obtain Siliceous MCM-41 molecular screen primary powder.
3. the preparation method of Siliceous MCM-41 adsorbent of molecular sieve described in accordance with the claim 1, it is characterised in that:
The template is at least one of the salt of ten alkyl trimethyl ammoniums, the salt of dodecyl trimethyl ammonium；
The silicon source is at least one of ethyl orthosilicate, sodium metasilicate, silica solution.
4. the preparation method of Siliceous MCM-41 adsorbent of molecular sieve according to claim 2, it is characterised in that: the mould
Plate agent Q2 is the salt of cetyl triethyl ammonium, at least one of the salt of octadecyl triethyl ammonium；The expanding agent is
1,3,5- trimethylbenzene, lauryl amine, N, at least one of N- dimethyl hexadecyl base ammonium.
5. a kind of Siliceous MCM-41 adsorbent of molecular sieve made of any one of Claims 1 to 4 the method.
6. Siliceous MCM-41 adsorbent of molecular sieve described in a kind of claim 5 is in diesel component cycloalkane, mononuclear aromatics, polycyclic
Application in the three components separation of aromatic hydrocarbons.
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| CN114210301A (en) * | 2021-10-29 | 2022-03-22 | 中国人民解放军63919部队 | Mesoporous solid amine adsorbent and preparation method and application thereof |
| CN114433037A (en) * | 2020-10-20 | 2022-05-06 | 中国石油化工股份有限公司 | Preparation method of M41S mesoporous material adsorbent, M41S mesoporous material adsorbent and application |
| CN114768748A (en) * | 2022-04-22 | 2022-07-22 | 山东亮剑环保新材料有限公司 | Preparation method of all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent |
| CN114917865A (en) * | 2022-06-06 | 2022-08-19 | 中海油天津化工研究设计院有限公司 | Aromatic hydrocarbon adsorbent and application thereof in increasing yield of ethylene cracking raw material |
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| CN114433037A (en) * | 2020-10-20 | 2022-05-06 | 中国石油化工股份有限公司 | Preparation method of M41S mesoporous material adsorbent, M41S mesoporous material adsorbent and application |
| CN114433037B (en) * | 2020-10-20 | 2024-01-26 | 中国石油化工股份有限公司 | Preparation method of M41S mesoporous material adsorbent, M41S mesoporous material adsorbent and application |
| CN114210301A (en) * | 2021-10-29 | 2022-03-22 | 中国人民解放军63919部队 | Mesoporous solid amine adsorbent and preparation method and application thereof |
| CN114768748A (en) * | 2022-04-22 | 2022-07-22 | 山东亮剑环保新材料有限公司 | Preparation method of all-silicon micro-mesoporous composite molecular sieve VOCs adsorbent |
| CN114917865A (en) * | 2022-06-06 | 2022-08-19 | 中海油天津化工研究设计院有限公司 | Aromatic hydrocarbon adsorbent and application thereof in increasing yield of ethylene cracking raw material |
| CN114917865B (en) * | 2022-06-06 | 2023-08-22 | 中海油天津化工研究设计院有限公司 | Aromatic hydrocarbon adsorbent and application thereof in yield-increasing ethylene cracking raw material |
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