CN107376979A - A kind of supporting Pts of MCM 41, the preparation method and applications of Al catalyst - Google Patents
A kind of supporting Pts of MCM 41, the preparation method and applications of Al catalyst Download PDFInfo
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- CN107376979A CN107376979A CN201710570012.1A CN201710570012A CN107376979A CN 107376979 A CN107376979 A CN 107376979A CN 201710570012 A CN201710570012 A CN 201710570012A CN 107376979 A CN107376979 A CN 107376979A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
- B01J29/0316—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41 containing iron group metals, noble metals or copper
- B01J29/0325—Noble metals
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/041—Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41
- B01J29/042—Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41 containing iron group metals, noble metals or copper
- B01J29/043—Noble metals
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/336—Polymers modified by chemical after-treatment with organic compounds containing silicon
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- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
- B01J2229/186—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself not in framework positions
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Abstract
The present invention provides a kind of supporting Pts of MCM 41, the preparation method and applications of Al catalyst, comprises the following steps：1) mesoporous silicon MCM 41 preparation：By cetyl trimethylammonium bromide, distilled water and concentrated ammonia liquor, tetraethyl orthosilicate is added after stirring, continues to stop reaction after stirring 7h, it is placed in crystallization in room temperature, filtering, washing, drying, cetyl trimethylammonium bromide is removed, and is washed, mesoporous silicon MCM 41 is made after roasting；2) preparation of MCM 41 supporting Pt, Al catalyst：Lead to N by activated mesoporous silicon MCM 41 and after the ethanol of dewater treatment adds container2After conversion, chloroplatinic acid ethanol solution and aluminium chloride ethanol solution are added, the supporting Pts of MCM 41, Al catalyst is made；Catalyst is used for heptamethyltrisiloxane and the catalyzing addition reaction of silicon with hydrogen of polyethylene glycol allyl.The product of the present invention has the advantages that stability is good, reusability is good, active high, recovery facilitates, cost is relatively low.
Description
Technical field
The present invention relates to catalyst manufacturing technology field, and in particular to a kind of preparation of MCM-41 supporting Pts, Al catalyst
Method and its application.
Background technology
In hydrosilylation, because heterogeneous catalysis is there is that can not reuse, separates etc. and to lack with product difficulty
Point, people are directed to researching and developing loaded catalyst, can recycled and reused, easily separated, reduce cost.But support type list
Easily reunite between metal in metallic catalyst, its catalytic activity can be reduced；In order to further improve noble metal catalyst
Catalytic capability, it is contemplated that have synergy between metal, it is to solve metal agglomeration to develop bi-component or multicomponent metallic catalyst
Effective way.Therefore, develop that a kind of stability is good, reusability is good, recovery is convenient, lower-cost load type platinum is urged
Agent is just into one of focus of research.
The content of the invention
It is an object of the invention to provide a kind of MCM-41 supporting Pts, the preparation method and applications of Al catalyst, nothing is utilized
Water-ethanol is solvent, AlCl3For accelerator, mesoporous silicon MCM-41 is carrier, by Pt, Al different orders of addition, is prepared
Pt, Al catalyst of MCM-41 loads, have stability is good, reusability is good, it is active it is high, recovery is convenient, cost is more low
Advantage.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of MCM-41 supporting Pts, the preparation method of Al catalyst, comprise the following steps：
1) mesoporous silicon MCM-41 preparation：
Cetyl trimethylammonium bromide, distilled water and concentrated ammonia liquor are added in three-necked flask, constant temperature stirs at 60 DEG C
Tetraethyl orthosilicate is added after 1h, continues to stop reaction after stirring 7h, crystallization in room temperature, filtering, washing, drying is placed in, with acidifying
Ethanol solution removes cetyl trimethylammonium bromide, and washs to neutrality, and 2h is calcined at 400 DEG C, and mesoporous silicon is made
MCM-41；
2) preparation of MCM-41 supporting Pts, Al catalyst：
Activated mesoporous silicon MCM-41 and the ethanol through dewater treatment are placed in three-necked flask, lead to N2After 0.5h, add
Enter chloroplatinic acid-ethanol solution and aluminium chloride-ethanol solution, MCM-41 supporting Pts, Al catalyst is made.
It is cetyl trimethylammonium bromide, distilled water, dense during the preparation of the mesoporous silicon MCM-41 according to above scheme
Ammoniacal liquor, the mass ratio of tetraethyl orthosilicate are 1~2:100~110:60~65:4~6.
According to above scheme, the acidic ethanol solution is that volume ratio is 1:20 hydrochloric acid and the mixed solution of ethanol.
According to above scheme, chloroplatinic acid concentration is 0.05mol/L in the chloroplatinic acid-ethanol solution, the aluminium chloride-second
Concentration of aluminum chloride is 0.05mol/L, the chloroplatinic acid-ethanol solution and aluminium chloride-ethanol solution dosage volume in alcoholic solution
Than for 2:5~4:3.
According to above scheme, the preparation of the MCM-41 supporting Pts, Al catalyst includes following method：
Activated mesoporous silicon MCM-41 and the ethanol through dewater treatment are placed in three-necked flask, lead to N2After 0.5h, add
Enter chloroplatinic acid-ethanol solution, 10h is stirred at 75 DEG C, then be evaporated ethanol with nitrogen of the purity more than or equal to 99.999%；
Then aluminium chloride-ethanol solution and ethanol are added, 10h is stirred, is filtered with distilled water, be subsequently placed in 50 DEG C of vacuum drying
Dried in device, MCM-41 elder generations supporting Pt is made, loads Al catalyst again, is designated as Al/Pt-MCM；
Activated mesoporous silicon MCM-41 and the ethanol through dewater treatment are placed in three-necked flask, lead to N2After 0.5h, add
Enter aluminium chloride-ethanol solution, 10h is stirred at 75 DEG C, then be evaporated ethanol with nitrogen of the purity more than or equal to 99.999%；
Then chloroplatinic acid-ethanol solution and ethanol are added, 10h is stirred, is filtered with distilled water, be subsequently placed in 50 DEG C of vacuum drying
Dried in device, MCM-41 is made and first loads Al, the catalyst of supporting Pt again, is designated as Pt/Al-MCM；
Activated mesoporous silicon MCM-41 and the ethanol through dewater treatment are placed in three-necked flask, lead to N2After 0.5h, add
Enter chloroplatinic acid-ethanol solution and aluminium chloride-ethanol solution, stir 10h at 75 DEG C, filtered with distilled water, is subsequently placed in
Dried in 50 DEG C of vacuum desiccator, MCM-41 supporting Pt, Al catalyst simultaneously is made, is designated as Pt+Al-MCM.
According to above scheme, the MCM-41 supporting Pts, Al catalyst are used for heptamethyltrisiloxane and polyethylene glycol alkene
The catalyzing addition reaction of silicon with hydrogen of propyl ether.
According to above scheme, during the hydrosilylation, MCM-41 supporting Pts, the dosage of Al catalyst are that reactant is total
The 0.3% of quality.
The beneficial effects of the invention are as follows：
1) prepared mesoporous silicon MCM-41 of the invention has bigger serface, orderly pore passage structure, preferableization
Stability and resistance to acids and bases are learned, is good carrier；
2) present invention is using mesoporous silicon MCM-41 as carrier, and absolute ethyl alcohol is solvent, AlCl3For accelerator, the load of preparation
Type MCM-41 supporting Pts, Al catalyst, effectively improve platinum agglomeration, improve the decentralization of platinum active body, from
And improve the catalytic activity of catalyst；Al addition makes the Pt of Pt metals formation electron deficientα+, the sulfur resistive with catalyst can be improved
Property, so as to have good stability, reusability and catalytic activity, and recycle conveniently, greatly reduce and be produced into
This；
3) MCM-41 supporting Pts of the invention, Al catalyst are used for heptamethyltrisiloxane and polyethylene glycol allyl
During catalyzing addition reaction of silicon with hydrogen, the conversion ratio of heptamethyltrisiloxane is more than Pt/MCM-41 single-metal reforming catalyst.
Brief description of the drawings
Fig. 1 is the TEM figures of MCM-41 load different order Pt, the Al catalyst of the present invention；
Fig. 2 is the BET characterization result figures of MCM-41 load different order Pt, the Al catalyst of the present invention；
Fig. 3 is the XRD of MCM-41 load different order Pt, the Al catalyst of the present invention.
Embodiment
Technical scheme is illustrated with embodiment below in conjunction with the accompanying drawings.
Embodiment 1, see Fig. 1-Fig. 3：
The present invention provides a kind of MCM-41 supporting Pts, the preparation method of Al catalyst, comprises the following steps：
1) mesoporous silicon MCM-41 preparation：
1.5gCTAB, 120mL distilled water and 80mL concentrated ammonia liquors are added in three-necked flask, at 60 DEG C after constant temperature stirring 1h
4.5g tetraethyl orthosilicates are added, continues to stop reaction after stirring 7h, crystallization in room temperature, filtering, washing, drying is placed in, with acidifying
Ethanol solution (VHydrochloric acid:VEthanol=1:20) CTAB is removed, and is washed to neutrality, 2h is calcined at 400 DEG C, mesoporous silicon MCM- is made
41, it is designated as MCM；
2) preparation of MCM-41 supporting Pts, Al catalyst：
Weigh activated ethanol of the mesoporous silicon MCM-41 and 35mL through dewater treatment of 1.0g to be placed in three-necked flask, lead to N2
After 0.5h, 10mL chloroplatinic acids-ethanol solution is added, 10h is stirred at 75 DEG C, then will with high pure nitrogen (purity 99.999%)
Ethanol is evaporated；Then 15mL aluminium chloride-ethanol solution and 30mL ethanol are added, 10h is stirred, is filtered with distilled water, then
It is placed in 50 DEG C of vacuum desiccator and dries, MCM-41 elder generations supporting Pt is made, loads Al catalyst again, is designated as Al/Pt-MCM.
Embodiment 2, see Fig. 1-Fig. 3：
Substantially with embodiment 1, difference is the preparation process of the present embodiment：Aluminium chloride-ethanol solution is first added, so
Aluminium chloride-ethanol solution is added afterwards, and MCM-41 is made and first loads Al, the catalyst of supporting Pt again, is designated as Pt/Al-MCM.
Embodiment 3, see Fig. 1-Fig. 3：
For the preparation process of the present embodiment substantially with embodiment 1, difference is MCM-41 supporting Pts, the system of Al catalyst
It is standby：
Weigh activated ethanol of the mesoporous silicon MCM-41 and 65mL through dewater treatment of 1.0g to be placed in three-necked flask, lead to N2
After 0.5h, 10mL chloroplatinic acids-ethanol solution and 15mL aluminium chloride-ethanol solution are added, 10h is stirred at 75 DEG C, uses distilled water
Filtered, be subsequently placed in 50 DEG C of vacuum desiccator and dry, MCM-41 supporting Pt, Al catalyst simultaneously is made, is designated as
Pt+Al-MCM。
Embodiment 4, see Fig. 1-Fig. 3：
The preparation process of the present embodiment substantially with embodiment 3, difference be difference be MCM-41 supporting Pts,
The preparation of Al catalyst：
Weigh activated ethanol of the mesoporous silicon MCM-41 and 35mL through dewater treatment of 1.0g to be placed in three-necked flask, lead to N2
After 0.5h, 10mL chloroplatinic acids-ethanol solution is added, 10h is stirred at 75 DEG C, is filtered with distilled water, be subsequently placed in 50 DEG C
Vacuum desiccator in dry, the catalyst of MCM-41 supporting Pts is made, is designated as Pt/MCM.
TEM, BET, XRD sign have been carried out to the product for implementing 1 to 4, has as a result divided and sees Fig. 1 to Fig. 3.
Fig. 1 (A)-(D) be respectively Pt/MCM, Pt/Al-MCM, Pt+Al-MCM, Al/Pt-MCM, TEM figures, Fig. 1 (E) is
The grain size distribution of Pt crystal grain in catalyst.As seen from Figure 1：Platinum crystal grain is successfully supported on mesoporous silicon MCM-41, Fig. 1
(A) Pt-MCM catalyst distributions have part to reunite than comparatively dense between particle in, and other load Al catalyst decentralization
Preferably, illustrate that the decentralization of platinum crystal grain can be improved by adding appropriate aluminium, and platinum is smaller.
Fig. 2 (A), (B) and table 1 are each catalyst and mesoporous silicon MCM-41 BET characterization results, from chart as can be seen that
The pore-size distribution of sample compares concentration, introduces Al Pt-MCM-41 catalyst, and its specific surface area and pore volume have declined,
And with the increase of Al dosages, the specific surface area and pore volume of Pt/Al-MCM catalyst all progressively decline, because Al is occupied
The duct of mesoporous silicon and the pore structure of catalyst is changed.
The mesoporous silicon MCM-41 of table 1 and each catalyst pore structure parameter
Note：dPt,XRDFor the particle size of Pt crystal grain on crystal face (111)/(200)；dPt,TEMAverage grain diameter for Pt crystal grain is big
It is small.
Fig. 3 (A), (B) are respectively the small angle and big angle XRD of mesoporous silicon MCM-41 and each catalyst, and crystal face (111)/
(200) particle size of the Pt crystal grain on is as shown in Table 1 above.From Fig. 3 (A), when loading a certain amount of Pt metals, urge
Agent has subtracted in the diffraction peak intensity of (100), (110) and (200) three crystal faces that 2 θ are at 2.19 °, 3.80 ° and 4.39 °
It is weak, but it still has orderly hexagonal phase pore passage structure.However, the catalyst for adding Al metals, the diffraction maximum of three
Intensity has weakened, but does not have a significant impact the order in its duct.Observe Fig. 3 (B) understand, catalyst 2 θ=30~
90 ° there are four stronger diffraction maximums, and it is that this is belonging respectively to metal at 39.7 °, 46.3 °, 67.4 ° and 81.3 ° in 2 θ
Platinum illustrates that Pt metals are successfully carried on mesoporous silicon in the characteristic diffraction peak of (111), (200), (220) and (311) crystal face
On, and its decentralization on duct is preferable.
Embodiment 5：
Take Pt/Al-MCM catalyst anti-for the catalysis Si―H addition reaction of heptamethyltrisiloxane and polyethylene glycol allyl
Should：Reaction temperature be 95 DEG C, catalyst amount be the total dosage of reactant 0.3wt.%, reactant molar ratio n (polyethylene glycol alkene
Propyl ether)/n (heptamethyltrisiloxane) be 0.9:1.After 6h is reacted, the conversion ratio of heptamethyltrisiloxane reaches 87%.
Above example is only to illustrative and not limiting technical scheme, although above-described embodiment enters to the present invention
Detailed description is gone, the person skilled of this area should be understood：The present invention can be modified or replaced on an equal basis, but
Any modification and local replacement for not departing from spirit and scope of the invention all should be covered in scope of the presently claimed invention.
Claims (7)
1. a kind of MCM-41 supporting Pts, the preparation method of Al catalyst, it is characterised in that comprise the following steps：
1) mesoporous silicon MCM-41 preparation：
Cetyl trimethylammonium bromide, distilled water and concentrated ammonia liquor are added in three-necked flask, at 60 DEG C after constant temperature stirring 1h
Tetraethyl orthosilicate is added, continues to stop reaction after stirring 7h, is placed in crystallization in room temperature, filtering, washing, drying, uses acidic ethanol
Solution removes cetyl trimethylammonium bromide, and washs to neutrality, and 2h is calcined at 400 DEG C, and mesoporous silicon MCM-41 is made；
2) preparation of MCM-41 supporting Pts, Al catalyst：
Activated mesoporous silicon MCM-41 and the ethanol through dewater treatment are placed in three-necked flask, lead to N2After 0.5h, chlorine is added
Platinic acid-ethanol solution and aluminium chloride-ethanol solution, MCM-41 supporting Pts, Al catalyst is made.
2. the preparation method of Pt-Al/MCM-41 catalyst according to claim 1, it is characterised in that the mesoporous silicon
During MCM-41 preparation, cetyl trimethylammonium bromide, distilled water, concentrated ammonia liquor, the mass ratio of tetraethyl orthosilicate are 1~2:
100~110:60~65:4~6.
3. the preparation method of Pt-Al/MCM-41 catalyst according to claim 1, it is characterised in that the acidic ethanol
Solution is that volume ratio is 1:20 hydrochloric acid and the mixed solution of ethanol.
4. the preparation method of Pt-Al/MCM-41 catalyst according to claim 1, it is characterised in that the chloroplatinic acid-
Chloroplatinic acid concentration is 0.05mol/L in ethanol solution, and concentration of aluminum chloride is 0.05mol/L in the aluminium chloride-ethanol solution, institute
The dosage volume ratio for stating chloroplatinic acid-ethanol solution and aluminium chloride-ethanol solution is 2:5~4:3.
5. MCM-41 supporting Pts according to claim 1, the preparation method of Al catalyst, it is characterised in that the MCM-
The preparation of 41 supporting Pts, Al catalyst includes following method：
Activated mesoporous silicon MCM-41 and the ethanol through dewater treatment are placed in three-necked flask, lead to N2After 0.5h, chlorine is added
Platinic acid-ethanol solution, 10h is stirred at 75 DEG C, then be evaporated ethanol with nitrogen of the purity more than or equal to 99.999%；Then
Aluminium chloride-ethanol solution and ethanol are added, 10h is stirred, is filtered, be subsequently placed in 50 DEG C of vacuum desiccator with distilled water
Drying, MCM-41 elder generations supporting Pt is made, loads Al catalyst again, is designated as Al/Pt-MCM；
Activated mesoporous silicon MCM-41 and the ethanol through dewater treatment are placed in three-necked flask, lead to N2After 0.5h, chlorine is added
Change aluminium-ethanol solution, 10h is stirred at 75 DEG C, then be evaporated ethanol with nitrogen of the purity more than or equal to 99.999%；Then
Chloroplatinic acid-ethanol solution and ethanol are added, 10h is stirred, is filtered, be subsequently placed in 50 DEG C of vacuum desiccator with distilled water
Drying, MCM-41 is made and first loads Al, the catalyst of supporting Pt again, is designated as Pt/Al-MCM；
Activated mesoporous silicon MCM-41 and the ethanol through dewater treatment are placed in three-necked flask, lead to N2After 0.5h, chlorine is added
Platinic acid-ethanol solution and aluminium chloride-ethanol solution, stir 10h at 75 DEG C, are filtered with distilled water, are subsequently placed in 50 DEG C
Vacuum desiccator in dry, be made MCM-41 simultaneously supporting Pt, Al catalyst, be designated as Pt+Al-MCM.
6. MCM-41 supporting Pts according to claim 1, the preparation method of Al catalyst, it is characterised in that the MCM-
41 supporting Pts, Al catalyst are used for heptamethyltrisiloxane and the catalyzing addition reaction of silicon with hydrogen of polyethylene glycol allyl.
7. MCM-41 supporting Pts according to claim 4, the preparation method of Al catalyst, it is characterised in that the silicon hydrogen
During addition reaction, MCM-41 supporting Pts, 0.3% that the dosage of Al catalyst is reactant gross mass.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108767270A (en) * | 2018-06-11 | 2018-11-06 | 佛山腾鲤新能源科技有限公司 | A kind of preparation method of fuel-cell catalyst |
| CN110201706A (en) * | 2019-06-18 | 2019-09-06 | 仲恺农业工程学院 | A kind of Pt/NH2- MCM-41 catalyst and the preparation method and application thereof |
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| CN108767270A (en) * | 2018-06-11 | 2018-11-06 | 佛山腾鲤新能源科技有限公司 | A kind of preparation method of fuel-cell catalyst |
| CN108767270B (en) * | 2018-06-11 | 2021-01-29 | 山东岱擎新能源科技有限公司 | Preparation method of fuel cell catalyst |
| CN110201706A (en) * | 2019-06-18 | 2019-09-06 | 仲恺农业工程学院 | A kind of Pt/NH2- MCM-41 catalyst and the preparation method and application thereof |
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