CN109248707A - It is a kind of acidity mesopore molecular sieve preparation method and its application in catalytic esterification - Google Patents
It is a kind of acidity mesopore molecular sieve preparation method and its application in catalytic esterification Download PDFInfo
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- CN109248707A CN109248707A CN201810945921.3A CN201810945921A CN109248707A CN 109248707 A CN109248707 A CN 109248707A CN 201810945921 A CN201810945921 A CN 201810945921A CN 109248707 A CN109248707 A CN 109248707A
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 54
- 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 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 230000032050 esterification Effects 0.000 title claims abstract description 14
- 238000005886 esterification reaction Methods 0.000 title claims abstract description 14
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 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 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 238000001354 calcination Methods 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 9
- 238000002425 crystallisation Methods 0.000 claims description 9
- 230000008025 crystallization Effects 0.000 claims description 9
- -1 Veratric acid methyl esters Chemical class 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 8
- 230000003213 activating effect Effects 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- DILOFCBIBDMHAY-UHFFFAOYSA-N methyl 2-(3,4-dimethoxyphenyl)acetate Chemical class 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
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- 229910003243 Na2SiO3·9H2O Inorganic materials 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 2
- GPVDHNVGGIAOQT-UHFFFAOYSA-N Veratric acid Natural products COC1=CC=C(C(O)=O)C(OC)=C1 GPVDHNVGGIAOQT-UHFFFAOYSA-N 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 125000005842 heteroatom Chemical group 0.000 abstract description 3
- 238000005286 illumination Methods 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 13
- 229910021641 deionized water Inorganic materials 0.000 description 13
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 description 10
- 238000005352 clarification Methods 0.000 description 6
- 229910020489 SiO3 Inorganic materials 0.000 description 5
- 239000004115 Sodium Silicate Substances 0.000 description 5
- 230000002378 acidificating effect Effects 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000011734 sodium 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
- 238000000034 method Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000007795 chemical reaction product Substances 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
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 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
- 102220500397 Neutral and basic amino acid transport protein rBAT_M41T_mutation Human genes 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 241000489523 Veratrum Species 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 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
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 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
-
- 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)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Electromagnetism (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The preparation method that a kind of acid mesopore molecular sieve is disclosed the present invention relates to the preparation of mesopore molecular sieve and its application in catalytic esterification.Preparation method provided by the invention is by the way that the acidity that ultraviolet illumination improves mesopore molecular sieve in the preparation process of mesopore molecular sieve, is added.The preparation method makes mesopore molecular sieve in acidity, increase active site, so as to improve its catalytic activity, because not introducing the acidity that metal heteroatom carrys out modulation molecular sieve, there is no the introducings of active component, also falling off for active component would not occur, increase the stability of molecular sieve, to realize the industrialized production of molecular sieve.
Description
Technical field
The present invention relates to the preparation of mesopore molecular sieve, in particular to the preparation method of a kind of acid mesopore molecular sieve and its
Application in catalytic esterification.
Background technique
Since New Mesoporous Molecular Sieves M41S is developed to function, since it has big uniform cellular structure, as big
The catalyst of molecule reaction, shows preferable application prospect.But due to the complexity and uncontrollability of its synthesis chemistry, such as mould
Plate agent type, silica alumina ratio, system pH, crystallization temperature, crystallization time all can to we synthesize mesopore molecular sieve pattern with knot
Structure has an impact；Mesoporous molecular, which screens out surface silanol group, has faint acidity outer, does not show any acidity substantially, lacks active sites
Point, catalytic oxidation ability is weak, therefore limits its application in terms of catalysis, its acid deficiency is caused seriously to constrain it
Industrial application.
Currently, many researchs are by introducing metal heteroatom in framework of molecular sieve come the acid of modulation molecular sieve mostly
Property, acid catalyzed requirement is complied with, for example introduce the metal components catalysis of phenolization such as Al, Ti in pure silicon molecular sieve and pay gram alkyl
Change reaction and prepares alkylbenzene；Loaded metallocene catalysis acrylic acid and methanol obtain on hollow ball-shape mesoporous composite material for another example
To methyl acrylate；But dosing for metal, active component is likely to so that the stability of gained molecular sieve declines, and lives
Property component dose that itself is also unstable, be easy to fall off, it is difficult to realize the industrialized production of molecular sieve.Therefore it provides a kind of acid
Property mesopore molecular sieve preparation method, mesopore molecular sieve acidity can be made to improve to improve its catalytic activity, it is steady to reinforce molecular sieve
It is qualitative, it is of great significance.
Summary of the invention
In order to solve the problems, such as that the acidity of mesopore molecular sieve in the prior art is weak, catalytic activity is low and stability is weak, this
Invention provides a kind of preparation method of acid mesopore molecular sieve.
In order to solve the above-mentioned technical problem, the invention adopts the following technical scheme:
A kind of preparation method of acidity mesopore molecular sieve comprising following steps:
(1.1) it stirs to clarify ctab surface activating agent is soluble in water, is cooled to room temperature；Preferably, the temperature of stirring
It is 25~40 DEG C, the time of stirring is 1h；
(1.2) by Na2SiO3·9H2O is soluble in water to be stirred to clarify, and is cooled to room temperature, by Na2SiO3Solution is added drop-wise to step
Suddenly it in the CTAB solution in (1.1) and mixes；Preferably, the temperature of stirring is 25~40 DEG C, the time of stirring is 0.5~
1h；
(1.3) pH of the reaction solution obtained using hydrochloric acid regulating step (1.2), is stirred at room temperature, and using purple
Outer light is irradiated reaction solution；Preferably, the pH of reaction solution is adjusted to 10.0-11.0；The time of stirring is 2~3h；It is ultraviolet
The time of light irradiation is 1-4h；
(1.4) reaction solution for obtaining step (1.3) carries out crystallization, filtering and washing, drying and calcination, obtains acid mesoporous
Molecular sieve MCM-41；Preferably, dry temperature is 100-120 DEG C, and the dry time is 12-24h；Calcining in Muffle furnace into
Row, the temperature of calcining are 550-600 DEG C, and the time of calcining is 8-10h.
Preferably, CTAB provided by the invention and Na2SiO3·9H2The molar ratio of O is 0.1:1~0.3:1.
The present invention is by the preparation process of mesopore molecular sieve, being added the acid that ultraviolet illumination improves mesopore molecular sieve
Property, the possible reason is, by the amount of hydroxyl radical free radical in ultraviolet care increase system, hydroxyl radical free radical can excite silicon oxygen bond disconnected
It splits, increases the content of the hydroxyl of molecular sieve surface, make mesopore molecular sieve in acidity, active site is increased, so as to improve
Its catalytic activity, because not introducing the acidity that metal heteroatom carrys out modulation molecular sieve, there is no the introducings of active component, also
Be not in falling off for active component, increase the stability of molecular sieve, to realize the industrialized production of molecular sieve.
Simultaneously, the application the present invention also provides a kind of above-mentioned acid mesopore molecular sieve in catalytic esterification；
It can be applied in various esterification class reactions, it is preferable that the present invention is to be with the acid mesopore molecular sieve of above-mentioned preparation method preparation
Catalyst, homoveratric acid and methanol carry out esterification, generate homoveratric acid methyl esters.
Above-mentioned esterification is to carry out in a high pressure reaction kettle, magneton is added in reaction process, nitrogen is replaced 3 times, 100
4h is reacted at DEG C, carries out centrifugation removal supernatant after reaction, (filter residue after centrifugation is product) obtains the high black false hellebore of product
Sour methyl esters.
Compared with traditional hydrothermal method prepares homoveratric acid methyl esters, using the acid of preparation method provided by the invention preparation
Property mesostructured material, be catalyzed homoveratric acid and methanol and carry out esterification, the conversion ratio of reaction has obtained largely
Raising, experiment results proved, it is provided by the invention acidity mesopore molecular sieve preparation process, the conversion ratio energy of homoveratric acid
The stability for the acid mesostructured material for enough reaching 15% or more, while being prepared is stronger, can be realized molecular sieve
Industrialized production.
Specific embodiment
The invention discloses a kind of preparation method of acid mesopore molecular sieve and its applications in catalytic esterification.This
Field technical staff can use for reference present disclosure, be suitably modified realization of process parameters.In particular, it should be pointed out that all similar
Replace and change apparent to those skilled in the art, they are considered as including in the present invention.This hair
Bright method and application are described by preferred embodiment, related personnel obviously can not depart from the content of present invention,
To method described herein and application is modified or appropriate changes and combinations in spirit and scope, carry out the implementation and application present invention
Technology.
In order to enable those skilled in the art to better understand the present invention, With reference to embodiment to the present invention
It is described in further detail.
Embodiment 1
The ctab surface activating agent of 0.3mol stirs 1h to clarification, the Na of 1mol in deionized water at 40 DEG C2SiO3·
9H2O, which is dissolved in deionized water at 40 DEG C, stirs 1h to clarifying, and the two is cooled to room temperature；Sodium silicate solution is slowly dropped to
It is mixed in CTAB solution, stirs 15min, then with 2mol/L salt acid for adjusting pH to 10.5, continue to stir 3h at 25 DEG C, will
3h is irradiated under room temperature ultraviolet light to homogeneous gel, homogeneous gel will be obtained and be transferred in polytetrafluoroethylene (PTFE) crystallizing kettle in 105 DEG C
Lower crystallization uses deionized water filtering and washing later, and drying for 24 hours, is finally used 550 DEG C of calcining 8h of Muffle furnace, obtained in 105 DEG C of baking ovens
To acidic molecular sieve MCM-41.
Embodiment 2
The ctab surface activating agent of 0.3mol stirs 1h to clarification, the Na of 1mol in deionized water at 40 DEG C2SiO3·
9H2O, which is dissolved in deionized water at 40 DEG C, stirs 1h to clarifying, and the two is cooled to room temperature；Sodium silicate solution is slowly dropped to
It is mixed in CTAB solution, stirs 15min, then with 2mol/L salt acid for adjusting pH to 10.5, continue to stir 3h at 25 DEG C, will
3h is irradiated under room temperature ultraviolet light to homogeneous gel, homogeneous gel will be obtained and be transferred in polytetrafluoroethylene (PTFE) crystallizing kettle in 105 DEG C
Lower crystallization uses deionized water filtering and washing later, and drying for 24 hours, is finally used 550 DEG C of calcining 8h of Muffle furnace, obtained in 100 DEG C of baking ovens
To acidic molecular sieve MCM-41.
Embodiment 3
0.3mol ctab surface activating agent stirs 1h to clarification, 3mol Na in deionized water at 25 DEG C2SiO3·
9H2O is dissolved in deionized water to be stirred to clarify at 25 DEG C, and the two is cooled to room temperature；Sodium silicate solution is slowly dropped to
It is mixed in CTAB solution, stirs 30min, then with 2mol/L salt acid for adjusting pH to 11, continued to stir 2h at 25 DEG C, will obtain
Homogeneous gel irradiates 1h under room temperature ultraviolet light, will obtain homogeneous gel and is transferred in polytetrafluoroethylene (PTFE) crystallizing kettle at 105 DEG C
Crystallization uses deionized water filtering and washing later, and dry 18h, finally uses 600 DEG C of calcining 10h of Muffle furnace, obtain in 110 DEG C of baking ovens
To acidic molecular sieve MCM-41.
Embodiment 4
0.3mol ctab surface activating agent stirs 1h to clarification, 2mol Na in deionized water water at 33 DEG C2SiO3·
9H2O is dissolved in deionized water to be stirred to clarify at 32 DEG C；The two is cooled to room temperature, and sodium silicate solution is slowly dropped to
It is mixed in CTAB solution, stirs 30min, then with 2mol/L salt acid for adjusting pH to 11, continued to stir 3h at 25 DEG C, will obtain
Homogeneous gel irradiates 4h under room temperature ultraviolet light, will obtain homogeneous gel and is transferred in polytetrafluoroethylene (PTFE) crystallizing kettle at 105 DEG C
Crystallization uses deionized water filtering and washing later, and drying for 24 hours, is finally used 580 DEG C of calcining 9h of Muffle furnace, obtained in 120 DEG C of baking ovens
Acidic molecular sieve MCM-41.
Embodiment 5
2g (0.01mol) homoveratric acid is weighed, certain methanol (0.3mol) is measured and is added in 75ml autoclave, add
The molecular sieve MCM-41 catalyst 0.05g for entering embodiment 1 is put into magneton, and nitrogen is replaced 3 times, is filled with 2.5Mpa nitrogen, revolving speed
630/min reacts 4h at 100 DEG C, and supernatant liquor is removed in reaction product centrifugation, obtains homoveratric acid methyl esters, homoveratric acid conversion
Rate is 15.32%.
Comparative example 1
0.3mol ctab surface activating agent stirs 1h to clarification, 1mol Na in 20ml water at 40 DEG C2SiO3·9H2O
1h is stirred in molten 10ml water at 40 DEG C to clarification；The two is cooled to room temperature, and sodium silicate solution is slowly dropped to CTAB solution
15min is stirred in middle mixing, then with 2mol/L salt acid for adjusting pH to 10.5, is continued to stir 3h at 25 DEG C, will uniformly be coagulated
Glue is transferred in polytetrafluoroethylene (PTFE) crystallizing kettle the crystallization at 105 DEG C, deionized water filtering and washing is used later, in 105 DEG C of baking ovens
Drying for 24 hours, finally uses 550 DEG C of calcining 8h of Muffle furnace, obtains conventional hydrothermal method acidic molecular sieve MCM-41.
2g (0.01mol) homoveratric acid is weighed, certain methanol (0.3mol) is measured and is added in 75ml autoclave, add
Enter above-mentioned conventional hydrothermal molecular sieve MCM-41 0.05g, be put into magneton, nitrogen is replaced 3 times, and 2.5Mpa nitrogen, revolving speed 630/ are filled with
Min reacts 4h at 100 DEG C, and supernatant liquor is collected by centrifugation in reaction product, obtains homoveratric acid methyl esters, does contrast groups, obtains
Homoveratric acid conversion ratio is 8.28%.
Comparative example 2
2g (0.01mol) homoveratric acid is weighed, certain methanol (0.3mol) is measured and is added in 75ml autoclave, put
Enter magneton, nitrogen is replaced 3 times, and 2.5Mpa nitrogen is filled with, and revolving speed 630/min reacts 4h at 100 DEG C, and reaction product centrifugation is received
Collect supernatant liquor, obtain homoveratric acid methyl esters, do blank group, obtained homoveratric acid conversion ratio is 5.05%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of acidity mesopore molecular sieve, which is characterized in that it includes the following steps:
(1.1) it stirs to clarify ctab surface activating agent is soluble in water, is cooled to room temperature；
(1.2) by Na2SiO3·9H2O is soluble in water to be stirred to clarify, and is cooled to room temperature, by Na2SiO3Solution is added drop-wise to step
(1.1) it in the CTAB solution in and mixes；
(1.3) pH of the reaction solution obtained using hydrochloric acid regulating step (1.2), is stirred at room temperature, and uses ultraviolet light
Reaction solution is irradiated；
(1.4) reaction solution for obtaining step (1.3) carries out crystallization, filtering and washing, drying and calcination, obtains acid mesoporous molecular
Sieve MCM-41.
2. the preparation method of acidity mesopore molecular sieve as described in claim 1, which is characterized in that CTAB and Na2SiO3·9H2O
Molar ratio be 0.1:1~0.3:1.
3. the preparation method of acidity mesopore molecular sieve as described in claim 1, which is characterized in that stirred in step (1.1)
Temperature is 25~40 DEG C, and the time of stirring is 1h；The temperature of stirring in step (1.2) is 25~40 DEG C, the time of stirring
It is 0.5~1h.
4. the preparation method of acidity mesopore molecular sieve as described in claim 1, which is characterized in that reaction solution in step (1.3)
PH adjust to 10.0~11.0；The time of stirring is 2~3h.
5. the preparation method of acidity mesopore molecular sieve as described in claim 1, which is characterized in that in step (1.3), ultraviolet light
The time of irradiation is 1~4h.
6. the preparation method of acidity mesopore molecular sieve as described in claim 1, which is characterized in that in step (1.4), dry
Temperature be 100~120 DEG C, the dry time be 12~for 24 hours；In step (1.4), calcining carries out in Muffle furnace, the temperature of calcining
Degree is 550~600 DEG C, and the time of calcining is 8~10h.
7. a kind of acid mesopore molecular sieve of the preparation method preparation as described in claim 1~6 is any is in catalytic esterification
In application.
8. the use as claimed in claim 7, which is characterized in that the condition of esterification are as follows: in being applied described in claim 7
Acid mesopore molecular sieve be catalyst, homoveratric acid and methanol carry out esterification, generate homoveratric acid methyl esters.
9. application as claimed in claim 8, which is characterized in that esterification carries out in a high pressure reaction kettle, in reaction process
Magneton is added, nitrogen replaces 3 times, 4h is reacted at 100 DEG C, is centrifuged after reaction, collects supernatant, obtains product height
Veratric acid methyl esters.
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| CN113912499A (en) * | 2021-11-29 | 2022-01-11 | 八叶草健康产业研究院(厦门)有限公司 | 4-fluoro-5-hydroxy-2-nitrobenzoic acid methyl ester |
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