CN107442156A - A kind of preparation method and applications of the catalyst of Pt Al/MCM 41 - Google Patents
A kind of preparation method and applications of the catalyst of Pt Al/MCM 41 Download PDFInfo
- Publication number
- CN107442156A CN107442156A CN201710570013.6A CN201710570013A CN107442156A CN 107442156 A CN107442156 A CN 107442156A CN 201710570013 A CN201710570013 A CN 201710570013A CN 107442156 A CN107442156 A CN 107442156A
- Authority
- CN
- China
- Prior art keywords
- mcm
- catalyst
- preparation
- ethanol
- ethanol solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 57
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 23
- 239000010703 silicon Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- SWGZAKPJNWCPRY-UHFFFAOYSA-N methyl-bis(trimethylsilyloxy)silicon Chemical compound C[Si](C)(C)O[Si](C)O[Si](C)(C)C SWGZAKPJNWCPRY-UHFFFAOYSA-N 0.000 claims abstract description 13
- NJGHBZYAEWVDMY-UHFFFAOYSA-K ethanol;trichloroalumane Chemical compound [Al+3].[Cl-].[Cl-].[Cl-].CCO NJGHBZYAEWVDMY-UHFFFAOYSA-K 0.000 claims abstract description 11
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 8
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 6
- 238000007259 addition reaction Methods 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 4
- 238000002425 crystallisation Methods 0.000 claims abstract description 4
- 230000008025 crystallization Effects 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000001257 hydrogen Substances 0.000 claims abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 43
- 239000000243 solution Substances 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 48
- 239000013078 crystal Substances 0.000 description 12
- 229910052697 platinum Inorganic materials 0.000 description 10
- 235000019441 ethanol Nutrition 0.000 description 9
- 239000011148 porous material Substances 0.000 description 6
- 239000000376 reactant Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000006459 hydrosilylation reaction Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 239000002815 homogeneous catalyst Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 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
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/394—Metal dispersion value, e.g. percentage or fraction
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
-
- 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
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Catalysts (AREA)
Abstract
The present invention provides a kind of preparation method and applications of the catalyst of Pt Al/MCM 41, 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 the catalyst of Pt Al/MCM 41：Lead to N by activated mesoporous silicon MCM 41 and after the ethanol of dewater treatment adds container2After conversion, chloroplatinic acid ethanol solution, stirring are added, then ethanol is evaporated；Then aluminium chloride ethanol solution and ethanol are added, stirring, is filtered with distilled water, then dried, the catalyst of Pt Al/MCM 41 is made；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 method of Pt-Al/MCM-41 catalyst
And its application.
Background technology
Most effective, the most frequently used platinum catalyst of hydrosilylation is Speier catalyst and Karstedt catalyst, this
Two kinds of catalyst have good catalytic activity to the hydrosilylation of unsaturated hydrocarbons, but it is anti-both to belong to homogeneous catalyst
Answer system, it is difficult to recycle, cause the waste of noble metal platinum.At present, people are directed to researching and developing heterogeneous catalysis, and platinum is born
It is loaded on carrier, forms macromolecule load catalyst, can recycle and reuse, reduce the loss of noble metal platinum, reduces production
Cost.However, easily reuniting between platinum metal particles on loaded catalyst, and then cause the activity reduction of catalyst.Cause
This, it is necessary to develop that a kind of stability is good, reusability is good, recovery is convenient, lower-cost platinum catalyst is to meet city
The needs of field.
The content of the invention
It is an object of the invention to provide a kind of preparation method and applications of Pt-Al/MCM-41 catalyst, anhydrous second is utilized
Alcohol is solvent, AlCl3For accelerator, mesoporous silicon MCM-41 is carrier, the support type Pt-Al/MCM-41 catalyst of preparation, is had
The advantages that stability is good, reusability is good, active high, recovery is convenient, cost is relatively low.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of preparation method of Pt-Al/MCM-41 catalyst, comprises the following steps：
1) mesoporous silicon MCM-41 preparation：
Cetyl trimethylammonium bromide (CTAB), distilled water and concentrated ammonia liquor are added in three-necked flask, it is permanent at 60 DEG C
Tetraethyl orthosilicate is added after temperature stirring 1h, continues to stop reaction after stirring 7h, is placed in crystallization in room temperature, filtering, washing, drying,
Cetyl trimethylammonium bromide is removed with acidic ethanol solution, and is washed to neutrality, 2h is calcined at 400 DEG C, is made and is situated between
Hole silicon MCM-41；
2) preparation of Pt-Al/MCM-41 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, 10h is stirred at 75 DEG C, then be evaporated ethanol with high pure nitrogen；Then aluminium chloride-ethanol is added
Solution and ethanol, 10h is stirred, is filtered with distilled water, is subsequently placed in 50 DEG C of vacuum desiccator and dries, Pt-Al/ is made
MCM-41 catalyst.
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 purity of the high pure nitrogen is more than or equal to 99.999%.
According to above scheme, Pt/Al mol ratio is 1 in the Pt-Al/MCM-41 catalyst:0.1~1:8.
According to above scheme, Pt/Al mol ratio is 1 in the Pt-Al/MCM-41 catalyst:2.
According to above scheme, the Pt-Al/MCM-41 catalyst is used for heptamethyltrisiloxane and polyethylene glycol pi-allyl
The catalyzing addition reaction of silicon with hydrogen of ether.
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 Pt-Al/MCM-41 catalyst, effectively improve platinum agglomeration, the decentralization of platinum active body is improved, so as to carry
The catalytic activity and resistance to SO_2 of high catalyst, so as to have good stability, reusability and catalytic activity, and reclaim profit
With conveniently, production cost is greatly reduced；
3) Pt-Al/MCM-41 catalyst of the invention is used for urging for heptamethyltrisiloxane and polyethylene glycol allyl
During SiClx addition reaction of hydrogen, the conversion ratio of heptamethyltrisiloxane is up to more than 90%.
Brief description of the drawings
Fig. 1 is the TEM figures of the Pt-Al/MCM-41 catalyst of the different Pt/Al mol ratios of the present invention；
Fig. 2 is the BET characterization result figures of the Pt-Al/MCM-41 catalyst of the different Pt/Al mol ratios of the present invention；
Fig. 3 is the XRD of the Pt-Al/MCM-41 catalyst of the different Pt/Al mol ratios 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 preparation method of Pt-Al/MCM-41 catalyst, comprises the following steps：
1) mesoporous silicon MCM-41 preparation：
1.0gCTAB, 10mL distilled water and 70mL concentrated ammonia liquors are added in three-necked flask, at 60 DEG C after constant temperature stirring 1h
5g tetraethyl orthosilicates are added, continues to stop reaction after stirring 7h, is placed in crystallization in room temperature, filtering, washing, drying, with acidifying second
Alcoholic 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。
2) preparation of Pt-Al/MCM-41 catalyst：
Weigh activated ethanol of the mesoporous silicon MCM-41 and 35mL through dewater treatment of 2.0g to be placed in three-necked flask, lead to N2
After 0.5h, 15mL 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 10mL 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, Pt-Al/MCM-41 catalyst is made, is designated as Pt1Al1-MCM。
Embodiment 2, see Fig. 1-Fig. 3：
Substantially with embodiment 1, difference is the preparation process of the present embodiment：The addition of aluminium chloride-ethanol solution
For 20mL, Pt is designated as1Al2-MCM。
Embodiment 3, see Fig. 1-Fig. 3：
Substantially with embodiment 1, difference is the preparation process of the present embodiment：The addition of aluminium chloride-ethanol solution
For 40mL, Pt is designated as1Al4-MCM。
Embodiment 4, see Fig. 1-Fig. 3：
Substantially with embodiment 1, difference is the preparation process of the present embodiment：The addition of aluminium chloride-ethanol solution
For 80mL, Pt is designated as1Al8-MCM。
Embodiment 5, see Fig. 1-Fig. 3：
Substantially with embodiment 1, difference is the preparation process of the present embodiment：The addition of aluminium chloride-ethanol solution
For 0mL, Pt is designated as1Al0-MCM。
TEM, BET, XRD sign have been carried out to the product for implementing 1 to 5, has as a result divided and sees Fig. 1 to Fig. 3.
Fig. 1 (A)-(E) is respectively Pt1Al0-MCM、Pt1Al1-MCM、Pt1Al2-MCM、Pt1Al4-MCM、Pt1Al8- MCM's
TEM schemes, and Fig. 1 (F) is the grain size distribution of Pt crystal grain in catalyst.As seen from Figure 1：Platinum can be improved by adding appropriate aluminium
Belong to the decentralization of crystal grain, platinum is smaller.
Fig. 2 (A), (B) and table 1 are the BET characterization results of each catalyst, from chart as can be seen that the pore-size distribution of sample
Comparing concentration, introduce Al Pt-MCM-41 catalyst, its specific surface area and pore volume have declined, and with Al dosages
Increase, the specific surface area and pore volume of Pt/Al-MCM catalyst all progressively decline, because Al occupies the duct of mesoporous silicon
And the pore structure of catalyst is set to change.
The pore structure parameter of the catalyst of table 1
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 catalyst, the grain of the Pt crystal grain on crystal face (111)/(200)
Footpath size is as shown in Table 1 above.As shown in Fig. 3 (A), contrast does not add Al Pt1Al0- MCM catalyst, introduce Al catalyst
Diffraction peak intensity in (100), (110) and (200) three crystal faces has weakened, and illustrates that its pore passage structure is varied from, and reduces
Its degree of order.Thus can determine whether, Al has been carried in mesoporous silicon MCM.As shown in Fig. 3 (B), catalyst is in 2 θ=30~90 °
There are four stronger diffraction maximums, 2 θ are 39.7 °, 46.3 °, 67.4 ° and 81.3 °, be belonging respectively to metal platinum (111),
(200), the diffraction maximum of (220) and (311) crystal face, illustrates that Pt metals are successfully loaded on mesoporous silicon, and point on duct
Divergence is preferable.
Comprehensive BET, TEM, XRD analysis result are understood, when Pt/Al mol ratio is 1:When 2, crystal face (111) in XRD/
(200) particle diameter of the Pt crystal grain on is minimum, and the average grain diameter of Pt crystal grain is also minimum in TEM figures, and decentralization is relatively best, because
And the resultant effect of catalyst is best.
Embodiment 6：
Take Pt1Al2- MCM catalyst is used for heptamethyltrisiloxane and the catalysis Si―H addition reaction of polyethylene glycol allyl is anti-
Should：Reaction temperature be 95 DEG C, catalyst amount be the total dosage of reactant 0.4wt.%, reactant molar ratio n (polyethylene glycol alkene
Propyl ether)/n (heptamethyltrisiloxane) be 0.9:1.After 4h is reacted, the conversion ratio of heptamethyltrisiloxane reaches 90%.
When reaction temperature is 95 DEG C, reactant molar ratio n (polyethylene glycol allyl)/n (heptamethyltrisiloxane) is
1:When 1.1, the conversion ratio of heptamethyltrisiloxane can reach 94%；As reactant molar ratio n (polyethylene glycol allyl)/n
(heptamethyltrisiloxane) is 0.9:1, when reaction temperature brings up to 100 DEG C, after 4h is reacted, the conversion of heptamethyltrisiloxane
Rate reaches 94%, and after circulating 6 uses, its conversion ratio to heptamethyltrisiloxane is still up to 90%.
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 (8)
1. a kind of preparation method of Pt-Al/MCM-41 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 Pt-Al/MCM-41 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, 10h is stirred at 75 DEG C, then be evaporated ethanol with high pure nitrogen；Then aluminium chloride-ethanol solution is added
And ethanol, 10h is stirred, is filtered with distilled water, is subsequently placed in 50 DEG C of vacuum desiccator and dries, Pt-Al/MCM- is made
41 catalyst.
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. the preparation method of Pt-Al/MCM-41 catalyst according to claim 1, it is characterised in that the high pure nitrogen
Purity be more than or equal to 99.999%.
6. the preparation method of Pt-Al/MCM-41 catalyst according to claim 1, it is characterised in that the Pt-Al/
Pt/Al mol ratio is 1 in MCM-41 catalyst:0.1~1:8.
7. the preparation method of Pt-Al/MCM-41 catalyst according to claim 1, it is characterised in that the Pt-Al/
Pt/Al mol ratio is 1 in MCM-41 catalyst:2.
8. the preparation method of Pt-Al/MCM-41 catalyst according to claim 1, it is characterised in that the Pt-Al/
MCM-41 catalyst is used for heptamethyltrisiloxane and the catalyzing addition reaction of silicon with hydrogen of polyethylene glycol allyl.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710570013.6A CN107442156A (en) | 2017-07-13 | 2017-07-13 | A kind of preparation method and applications of the catalyst of Pt Al/MCM 41 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710570013.6A CN107442156A (en) | 2017-07-13 | 2017-07-13 | A kind of preparation method and applications of the catalyst of Pt Al/MCM 41 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107442156A true CN107442156A (en) | 2017-12-08 |
Family
ID=60488047
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710570013.6A Pending CN107442156A (en) | 2017-07-13 | 2017-07-13 | A kind of preparation method and applications of the catalyst of Pt Al/MCM 41 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107442156A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101703929A (en) * | 2009-07-15 | 2010-05-12 | 李浩贤 | Synthesis and characterization of MCM loaded Pt catalyst and microwave catalytic hydrosilylation of octene |
| CN103100415A (en) * | 2012-12-03 | 2013-05-15 | 北京化工大学 | Catalyst with active component nano particles embedded in molecular sieve to crystallize, method and application |
| CN104689841A (en) * | 2013-12-05 | 2015-06-10 | 青岛惠城石化科技有限公司 | Synthesis and characterization of MCM loaded Pt catalyst and microwave catalytic hydrosilylation of octene |
-
2017
- 2017-07-13 CN CN201710570013.6A patent/CN107442156A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101703929A (en) * | 2009-07-15 | 2010-05-12 | 李浩贤 | Synthesis and characterization of MCM loaded Pt catalyst and microwave catalytic hydrosilylation of octene |
| CN103100415A (en) * | 2012-12-03 | 2013-05-15 | 北京化工大学 | Catalyst with active component nano particles embedded in molecular sieve to crystallize, method and application |
| CN104689841A (en) * | 2013-12-05 | 2015-06-10 | 青岛惠城石化科技有限公司 | Synthesis and characterization of MCM loaded Pt catalyst and microwave catalytic hydrosilylation of octene |
Non-Patent Citations (1)
| Title |
|---|
| 罗明检: "Pt-Al/MCM-41催化剂制备及其芳烃加氢性能研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104248985B (en) | The preparation method of the composite mesoporous carrier of spherical montmorillonite and loaded catalyst and its preparation method and application and ethyl acetate | |
| CN104248981B (en) | The spherical complex carrier in three-dimensional cubic duct and catalyst and its preparation method and application and the preparation method of ethyl acetate | |
| CN109999915B (en) | For CO2Porphyrin-based metal organic framework material for cyclization catalytic reaction and preparation method thereof | |
| CN104248979B (en) | The preparation method of sphericity mesoporous silicon dioxide complex carrier and Catalysts and its preparation method and application and ethyl acetate | |
| CN104248986B (en) | The preparation method of the composite mesoporous carrier of spherical attapulgite and loaded catalyst and its preparation method and application and ethyl acetate | |
| CN104069882B (en) | A kind of method of the metallic catalyst preparing carbon-nitrogen material load | |
| CN103920534A (en) | Catalyst of basic ionic liquid immobilized on metal-organic frameworks and preparation method thereof | |
| CN102276642A (en) | Ionic liquid precursor and mesoporous material for supporting ionic liquid precursor, synthesis and application | |
| CN106622377B (en) | It is a kind of spherical shape mesoporous composite material containing aluminium and loaded catalyst and its preparation method and application and ethyl acetate preparation method | |
| CN104448381A (en) | Preparation and application of imidazole functionalized ordered mesoporous phenolic resin material | |
| CN112121853A (en) | Mesoporous hollow silica nanosphere loaded with prolinol catalyst and preparation method and application thereof | |
| CN107199052A (en) | A kind of silver-colored titanium dioxide metal-organic framework composite and its preparation method and application | |
| CN113289688A (en) | Amino-functionalized zirconium-based MOFs nanosheet synthesized by microwave-assisted method and preparation method thereof | |
| CN106622378B (en) | It is a kind of spherical shape mesoporous composite material containing aluminium and loaded catalyst and its preparation method and application and cyclohexanone glycerol ketal method | |
| CN105585035B (en) | A kind of preparation method of hollow aluminum oxide microspheres | |
| CN102895986A (en) | Palladium-supported mesoporous carbon nitride catalyst for bromate reduction and preparation | |
| CN107442156A (en) | A kind of preparation method and applications of the catalyst of Pt Al/MCM 41 | |
| CN107376979A (en) | A kind of supporting Pts of MCM 41, the preparation method and applications of Al catalyst | |
| CN104437474A (en) | Ordered mesoporous carbon material loaded platinum catalyst and application thereof to catalytic hydrogenation of aromatic nitro compound | |
| CN108017740B (en) | Spherical porous mesoporous composite material, supported catalyst and preparation method thereof | |
| CN101229517A (en) | Method of preparing nanometer magnetic heteropoly acid | |
| CN108003261B (en) | Method for polymerizing ethylene and polyethylene | |
| CN103464200A (en) | Supported perrhenate ionic liquid as well as preparation method thereof | |
| CN107096567B (en) | The composite catalyst and preparation method of synthesis of propylene glycol | |
| CN111054384A (en) | Catalyst for organic liquid hydrogen storage material dehydrogenation and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171208 |
|
| RJ01 | Rejection of invention patent application after publication |