CN109248707B - Preparation method of acidic mesoporous molecular sieve and application of acidic mesoporous molecular sieve in catalytic esterification reaction - Google Patents
Preparation method of acidic mesoporous molecular sieve and application of acidic mesoporous molecular sieve in catalytic esterification reaction Download PDFInfo
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- CN109248707B CN109248707B CN201810945921.3A CN201810945921A CN109248707B CN 109248707 B CN109248707 B CN 109248707B CN 201810945921 A CN201810945921 A CN 201810945921A CN 109248707 B CN109248707 B CN 109248707B
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 65
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 230000002378 acidificating effect Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000005886 esterification reaction Methods 0.000 title claims abstract description 13
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 12
- 238000003756 stirring Methods 0.000 claims description 31
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 20
- WUAXWQRULBZETB-UHFFFAOYSA-N homoveratric acid Chemical compound COC1=CC=C(CC(O)=O)C=C1OC WUAXWQRULBZETB-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000012295 chemical reaction liquid Substances 0.000 claims description 6
- 230000001678 irradiating effect Effects 0.000 claims description 6
- DILOFCBIBDMHAY-UHFFFAOYSA-N methyl 2-(3,4-dimethoxyphenyl)acetate Chemical compound COC(=O)CC1=CC=C(OC)C(OC)=C1 DILOFCBIBDMHAY-UHFFFAOYSA-N 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 229910020489 SiO3 Inorganic materials 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- 230000032050 esterification Effects 0.000 abstract description 2
- 125000005842 heteroatom Chemical group 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 13
- 229910021641 deionized water Inorganic materials 0.000 description 13
- 238000002425 crystallisation Methods 0.000 description 11
- 230000008025 crystallization Effects 0.000 description 11
- 239000004115 Sodium Silicate Substances 0.000 description 5
- -1 polytetrafluoroethylene Polymers 0.000 description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 238000003547 Friedel-Crafts alkylation reaction Methods 0.000 description 1
- 102220500397 Neutral and basic amino acid transport protein rBAT_M41T_mutation Human genes 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
Classifications
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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
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/345—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of ultraviolet wave energy
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Plasma & Fusion (AREA)
- Optics & Photonics (AREA)
- Electromagnetism (AREA)
- Dispersion Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention relates to preparation of a mesoporous molecular sieve, and discloses a preparation method of an acidic mesoporous molecular sieve and application of the acidic mesoporous molecular sieve in catalytic esterification. The preparation method provided by the invention is that in the preparation process of the mesoporous molecular sieve, ultraviolet light is added to improve the acidity of the mesoporous molecular sieve. The preparation method makes the mesoporous molecular sieve acidic, increases active sites, and can improve the catalytic activity of the mesoporous molecular sieve, and because metal heteroatoms are not introduced to modulate the acidity of the molecular sieve, the introduction of active components is not existed, the falling of the active components can not occur, the stability of the molecular sieve is increased, and the industrial production of the molecular sieve is realized.
Description
Technical Field
The invention relates to preparation of a mesoporous molecular sieve, in particular to a preparation method of an acidic mesoporous molecular sieve and application of the acidic mesoporous molecular sieve in catalytic esterification.
Background
The novel mesoporous molecular sieve M41S has been developed successfully, and has a large uniform pore channel structure, so that the mesoporous molecular sieve has a good application prospect when being used as a catalyst for macromolecular reaction. However, due to the complexity and uncontrollable nature of the synthetic chemistry, such as the type of template agent, the silica-alumina ratio, the system pH, the crystallization temperature and the crystallization time, the shape and the structure of the synthesized mesoporous molecular sieve can be influenced; except that the surface silicon hydroxyl has weak acidity, the mesoporous molecular sieve basically does not show any acidity, lacks active sites and has weak catalytic oxidation reaction capability, so the application of the mesoporous molecular sieve in catalysis is limited, and the insufficient acidity severely restricts the industrial application of the mesoporous molecular sieve.
At present, most of researches modulate the acidity of a molecular sieve by introducing metal heteroatoms into a molecular sieve framework to enable the molecular sieve to meet the requirement of acid catalysis, for example, introducing metal components such as Al, Ti and the like into a pure silicon molecular sieve to catalyze phenol friedel-crafts alkylation reaction to prepare alkylbenzene; then, for example, acrylic acid and methanol are catalyzed by load type metallocene on the hollow spherical mesoporous composite material to obtain methyl acrylate; however, the stability of the molecular sieve is reduced by adding the metal and the active component, and the addition of the active component is unstable and easy to fall off, so that the industrial production of the molecular sieve is difficult to realize. Therefore, the preparation method of the acidic mesoporous molecular sieve is provided, the acidity of the mesoporous molecular sieve can be improved, the catalytic activity of the mesoporous molecular sieve is improved, and the stability of the mesoporous molecular sieve is enhanced, so that the preparation method has important significance.
Disclosure of Invention
In order to solve the problems of weak acidity, low catalytic activity and weak stability of the mesoporous molecular sieve in the prior art, the invention provides a preparation method of an acidic mesoporous molecular sieve.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of an acidic mesoporous molecular sieve comprises the following steps:
(1.1) dissolving a CTAB surfactant in water, stirring until the solution is clear, and cooling to room temperature; preferably, the stirring temperature is 25-40 ℃, and the stirring time is 1 h;
(1.2) adding Na2SiO3·9H2Dissolving O in water, stirring to clarify, cooling to room temperature, adding Na2SiO3Dropwise adding the solution into the CTAB solution in the step (1.1) and mixing; preferably, the stirring temperature is 25-40 ℃, and the stirring time is 0.5-1 h;
(1.3) adjusting the pH value of the reaction liquid obtained in the step (1.2) by using hydrochloric acid, stirring at room temperature, and irradiating the reaction liquid by using ultraviolet light; preferably, the pH of the reaction solution is adjusted to 10.0 to 11.0; stirring for 2-3 h; the time of ultraviolet irradiation is 1-4 h;
(1.4) crystallizing, filtering, washing, drying and calcining the reaction liquid obtained in the step (1.3) to obtain an acidic mesoporous molecular sieve MCM-41; preferably, the drying temperature is 100-120 ℃, and the drying time is 12-24 h; the calcination is carried out in a muffle furnace, the calcination temperature is 550-600 ℃, and the calcination time is 8-10 h.
Preferably, the CTAB and the Na provided by the invention2SiO3·9H2The molar ratio of O is 0.1:1 to 0.3: 1.
The invention improves the acidity of the mesoporous molecular sieve by adding ultraviolet light for illumination in the preparation process of the mesoporous molecular sieve, and the possible reason is that the amount of hydroxyl free radicals in the system is increased by ultraviolet light, the hydroxyl free radicals can excite silicon-oxygen bonds to break, the content of the hydroxyl on the surface of the molecular sieve is increased, the mesoporous molecular sieve is acidic, and active sites are increased, so that the catalytic activity of the mesoporous molecular sieve can be improved.
Meanwhile, the invention also provides an application of the acidic mesoporous molecular sieve in catalytic esterification reaction; the method can be applied to various esterification reactions, and preferably, the method takes the acidic mesoporous molecular sieve prepared by the preparation method as a catalyst, and the homoveratric acid and the methanol are subjected to esterification reaction to generate the homoveratric methyl ester.
The esterification reaction is carried out in a high-pressure reaction kettle, magnetons are added in the reaction process, nitrogen is replaced for 3 times, the reaction is carried out for 4 hours at the temperature of 100 ℃, and after the reaction is finished, the supernatant is removed by centrifugation, (the filter residue after centrifugation is the product) to obtain the product methyl homoverate.
Compared with the traditional hydrothermal method for preparing the homoveratric methyl ester, the acidic mesoporous molecular sieve MCM-41 prepared by the preparation method provided by the invention catalyzes the homoveratric acid and methanol to carry out esterification reaction, the conversion rate of the reaction is greatly improved, and test results prove that the preparation process of the acidic mesoporous molecular sieve provided by the invention has the advantages that the conversion rate of the homoveratric acid can reach more than 15%, and meanwhile, the prepared acidic mesoporous molecular sieve MCM-41 has stronger stability and can realize the industrial production of the molecular sieve.
Detailed Description
The invention discloses a preparation method of an acidic mesoporous molecular sieve and application of the acidic mesoporous molecular sieve in catalytic esterification reaction. Those skilled in the art can modify the process parameters appropriately to achieve the desired results with reference to the disclosure herein. It is expressly intended that all such similar substitutes and modifications which would be obvious to those skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The following detailed description of the invention refers to specific embodiments thereof for better understanding by those skilled in the art.
Example 1
0.3mol CTAB surfactant in deionized water at 40 deg.C for 1h to clear, 1mol Na2SiO3·9H2Dissolving O in deionized water, stirring at 40 deg.C for 1h to clarify, and cooling to room temperature; slowly dropwise adding a sodium silicate solution into a CTAB solution for mixing, stirring for 15min, then adjusting the pH to 10.5 by using 2mol/L hydrochloric acid, continuously stirring for 3h at 25 ℃, irradiating the obtained uniform gel for 3h under room temperature ultraviolet light, transferring the obtained uniform gel into a polytetrafluoroethylene crystallization kettle for crystallization at 105 ℃, then performing suction filtration and washing by using deionized water, drying in an oven at 105 ℃ for 24h, and finally calcining for 8h at 550 ℃ by using a muffle furnace to obtain the acid molecular sieve MCM-41.
Example 2
0.3mol CTAB surfactant in deionized water at 40 deg.C for 1h to clear, 1mol Na2SiO3·9H2Dissolving O in deionized water, stirring at 40 deg.C for 1h to clarify, and cooling to room temperature; slowly dropwise adding sodium silicate solution into CTAB solution, mixing, stirring for 15min, adjusting pH to 10.5 with 2mol/L hydrochloric acid, stirring at 25 deg.C for 3 hr, irradiating the obtained uniform gel with ultraviolet light at room temperature for 3 hr to obtain uniform gelTransferring the obtained product to a polytetrafluoroethylene crystallization kettle for crystallization at 105 ℃, then performing suction filtration and washing by using deionized water, drying in a drying oven at 100 ℃ for 24 hours, and finally calcining in a muffle furnace at 550 ℃ for 8 hours to obtain the acidic molecular sieve MCM-41.
Example 3
0.3mol CTAB surfactant is stirred in deionized water at 25 ℃ for 1h until clear, 3mol Na2SiO3·9H2Dissolving O in deionized water, stirring at 25 deg.C to clarify, and cooling to room temperature; slowly and dropwise adding a sodium silicate solution into a CTAB solution for mixing, stirring for 30min, then adjusting the pH to 11 by using 2mol/L hydrochloric acid, continuously stirring for 2h at 25 ℃, irradiating the obtained uniform gel for 1h under room-temperature ultraviolet light, transferring the obtained uniform gel into a polytetrafluoroethylene crystallization kettle for crystallization at 105 ℃, then performing suction filtration and washing by using deionized water, drying for 18h in a 110 ℃ oven, and finally calcining for 10h at 600 ℃ by using a muffle furnace to obtain the acid molecular sieve MCM-41.
Example 4
0.3mol CTAB surfactant is stirred in deionized water at 33 ℃ for 1h until clear, 2mol Na2SiO3·9H2Dissolving O in deionized water, and stirring at 32 ℃ until the solution is clear; and cooling the two solutions to room temperature, slowly dropwise adding the sodium silicate solution into the CTAB solution for mixing, stirring for 30min, then adjusting the pH to 11 by using 2mol/L hydrochloric acid, continuously stirring for 3h at 25 ℃, irradiating the obtained uniform gel for 4h under room-temperature ultraviolet light, transferring the obtained uniform gel into a polytetrafluoroethylene crystallization kettle for crystallization at 105 ℃, then performing suction filtration and washing by using deionized water, drying in an oven at 120 ℃ for 24h, and finally calcining for 9h at 580 ℃ by using a muffle furnace to obtain the acid molecular sieve MCM-41.
Example 5
Weighing 2g (0.01mol) homoveratric acid, weighing a certain amount of methanol (0.3mol), adding into a 75ml high-pressure reaction kettle, adding 0.05g of the molecular sieve MCM-41 catalyst of example 1, adding magnetons, performing nitrogen replacement for 3 times, charging 2.5Mpa nitrogen, rotating at a speed of 630/min, reacting for 4h at 100 ℃, centrifuging the reaction product to remove supernatant, and obtaining homoveratric methyl ester, wherein the conversion rate of homoveratric acid is 15.32%.
Comparative example 1
0.3mol CTAB surfactant in 20ml water at 40 deg.C for 1h to clear, 1mol Na2SiO3·9H2Dissolving O in 10ml of water, and stirring for 1h at 40 ℃ until the solution is clear; and cooling the two solutions to room temperature, slowly dropwise adding the sodium silicate solution into the CTAB solution, mixing, stirring for 15min, then adjusting the pH to 10.5 by using 2mol/L hydrochloric acid, continuously stirring for 3h at 25 ℃, transferring the obtained uniform gel into a polytetrafluoroethylene crystallization kettle, crystallizing at 105 ℃, then performing suction filtration and washing by using deionized water, drying for 24h in a 105 ℃ oven, and finally calcining for 8h at 550 ℃ by using a muffle furnace to obtain the traditional hydrothermal acidic molecular sieve MCM-41.
Weighing 2g (0.01mol) homoveratric acid, measuring a certain amount of methanol (0.3mol), adding into a 75ml high-pressure reaction kettle, adding the traditional hydrothermal molecular sieve MCM-410.05 g, adding magnetons, performing nitrogen replacement for 3 times, charging 2.5Mpa nitrogen, performing reaction at the rotating speed of 630/min at 100 ℃ for 4h, centrifuging the reaction product, collecting supernatant to obtain homoveratric methyl ester, and performing comparison to obtain the homoveratric acid with the conversion rate of 8.28%.
Comparative example 2
Weighing 2g (0.01mol) homoveratric acid, measuring certain methanol (0.3mol), adding into a 75ml high-pressure reaction kettle, adding magnetons, replacing with nitrogen for 3 times, charging 2.5Mpa nitrogen, rotating at 630/min, reacting at 100 ℃ for 4h, centrifuging reaction products, collecting supernatant to obtain homoveratric methyl ester, and making blank group to obtain homoveratric acid with the conversion rate of 5.05%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The preparation method of the acidic mesoporous molecular sieve is characterized by comprising the following steps:
(1.1) dissolving a CTAB surfactant in water, stirring until the solution is clear, and cooling to room temperature;
(1.2) adding Na2SiO3·9H2Dissolving O in water, stirring to clarify, and coolingAt room temperature, adding Na2SiO3Dropwise adding the solution into the CTAB solution in the step (1.1) and mixing;
(1.3) adjusting the pH value of the reaction liquid obtained in the step (1.2) by using hydrochloric acid, stirring at room temperature, and irradiating the reaction liquid by using ultraviolet light;
and (1.4) crystallizing, filtering, washing, drying and calcining the reaction liquid obtained in the step (1.3) to obtain the acidic mesoporous molecular sieve MCM-41.
2. The method of claim 1, wherein CTAB and Na are present in the molecular sieve2SiO3·9H2The molar ratio of O is 0.1:1 to 0.3: 1.
3. The method for preparing an acidic mesoporous molecular sieve according to claim 1, wherein the stirring temperature in the step (1.1) is 25 to 40 ℃, and the stirring time is 1 h; the stirring temperature in the step (1.2) is 25-40 ℃, and the stirring time is 0.5-1 h.
4. The method of claim 1, wherein the pH of the reaction solution in step (1.3) is adjusted to 10.0 to 11.0; the stirring time is 2-3 h.
5. The method for preparing an acidic mesoporous molecular sieve according to claim 1, wherein in the step (1.3), the ultraviolet irradiation is performed for 1 to 4 hours.
6. The method for preparing an acidic mesoporous molecular sieve according to claim 1, wherein in the step (1.4), the drying temperature is 100-120 ℃, and the drying time is 12-24 h; in the step (1.4), the calcination is carried out in a muffle furnace, the calcination temperature is 550-600 ℃, and the calcination time is 8-10 h.
7. The use of an acidic mesoporous molecular sieve prepared by the preparation method of any one of claims 1 to 6 in catalytic esterification reactions; and (3) carrying out esterification reaction on homoveratric acid and methanol by using the acidic mesoporous molecular sieve as a catalyst to generate homoveratric methyl ester.
8. The use of claim 7, wherein the esterification reaction is carried out in a high pressure reactor, magnetons are added during the reaction, nitrogen is used for replacement for 3 times, the reaction is carried out for 4 hours at 100 ℃, centrifugation is carried out after the reaction is finished, and supernatant is collected to obtain the product methyl homoveralate.
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