CN117801181B - Method for preparing organic-inorganic nanocomposite material by UV photopolymerization - Google Patents
Method for preparing organic-inorganic nanocomposite material by UV photopolymerization Download PDFInfo
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- CN117801181B CN117801181B CN202410211320.5A CN202410211320A CN117801181B CN 117801181 B CN117801181 B CN 117801181B CN 202410211320 A CN202410211320 A CN 202410211320A CN 117801181 B CN117801181 B CN 117801181B
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims description 18
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 28
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 26
- GAURFLBIDLSLQU-UHFFFAOYSA-N diethoxy(methyl)silicon Chemical compound CCO[Si](C)OCC GAURFLBIDLSLQU-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 24
- -1 sulfonyl modified montmorillonite Chemical class 0.000 claims abstract description 24
- 239000004593 Epoxy Substances 0.000 claims abstract description 13
- 238000012663 cationic photopolymerization Methods 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- NZEDMAWEJPYWCD-UHFFFAOYSA-N 3-prop-2-enylsulfonylprop-1-ene Chemical compound C=CCS(=O)(=O)CC=C NZEDMAWEJPYWCD-UHFFFAOYSA-N 0.000 claims abstract description 9
- QQRDLIWKSDAFLZ-UHFFFAOYSA-M dibutyl-chloro-prop-2-enylstannane Chemical compound CCCC[Sn](Cl)(CC=C)CCCC QQRDLIWKSDAFLZ-UHFFFAOYSA-M 0.000 claims abstract description 8
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 43
- 238000003756 stirring Methods 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 11
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- DQEUYIQDSMINEY-UHFFFAOYSA-M magnesium;prop-1-ene;bromide Chemical compound [Mg+2].[Br-].[CH2-]C=C DQEUYIQDSMINEY-UHFFFAOYSA-M 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 4
- GUCYFKSBFREPBC-UHFFFAOYSA-N [phenyl-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C)C=C(C)C=C1C GUCYFKSBFREPBC-UHFFFAOYSA-N 0.000 claims description 3
- 125000005520 diaryliodonium group Chemical group 0.000 claims description 3
- FDPIMTJIUBPUKL-UHFFFAOYSA-N dimethylacetone Natural products CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 abstract description 2
- 125000003700 epoxy group Chemical group 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 2
- 238000006459 hydrosilylation reaction Methods 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 230000002687 intercalation Effects 0.000 abstract description 2
- 238000009830 intercalation Methods 0.000 abstract description 2
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 abstract description 2
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 229910003471 inorganic composite material Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000003993 interaction Effects 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920000767 polyaniline Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 108010074506 Transfer Factor Proteins 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/10—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention relates to the technical field of organic-inorganic nanocomposite preparation, in particular to a method for preparing an organic-inorganic nanocomposite by UV photopolymerization. The invention carries out hydrolytic condensation on methyl diethoxy silane and hydroxyl of montmorillonite to obtain methyl diethoxy silane/montmorillonite; performing hydrosilylation reaction on diallyl sulfone and silicon-hydrogen bond of methyldiethoxysilane/montmorillonite to obtain modified montmorillonite containing glycidyl ether and sulfonyl; intercalation is carried out on the sulfonyl modified montmorillonite and bisphenol A epoxy cationic photopolymerization resin; the epoxy group and propylene carbonate and allyl dibutyl tin chloride are subjected to UV photopolymerization to obtain an organic-inorganic nanocomposite; the organic-inorganic nanocomposite prepared by the UV photopolymerization has excellent ultraviolet absorption property and excellent dispersity.
Description
Technical Field
The invention relates to the technical field of organic-inorganic nanocomposite material preparation, in particular to a method for preparing an organic-inorganic nanocomposite material by UV photopolymerization.
Background
The nanometer organic-inorganic composite material is a composite material formed by the interaction of organic components and inorganic components under the nanometer scale, generally has the advantages of the two materials, and is one of the most economical and practical methods for preparing high-performance materials. The two components of the organic-inorganic composite material are different from the traditional composite material in many aspects of preparation method, treatment process, performance of the obtained material and the like due to the interaction on the nanometer scale, so that the relationship between the structure and the performance of the nanometer organic-inorganic composite material is required to be studied more widely and intensively. For preparing the high-performance nano organic-inorganic composite material, the excellent adjustment of the interaction between the organic component and the inorganic component is the key for improving the performance of the nano organic-inorganic composite material.
The invention discloses a polyaniline-Fe 3O4 nanocomposite and a preparation method thereof, and provides a conductive ferromagnetic organic polymer-inorganic nanocomposite and a preparation technology thereof. The method is that polyaniline particles are soaked in a mixed ferric salt solution containing Fe 2+ and Fe 3+ for a certain time, then the polyaniline particles are dripped into an alkaline solution to a proper pH value under stirring, and then the polyaniline-Fe 3O4 nano composite particles are prepared under stirring for a certain time. The nano composite particles can form an electromagnetic rheological fluid if mixed with dielectric oil; if the nano composite film is doped with organic acid, the nano composite film with giant magnetoresistance can be prepared.
The Chinese patent application with publication number of CN1563176A provides a method for preparing high heat-resistant organic-inorganic composite material. Specifically, a polyvalent inorganic substance or a precursor thereof is added to the monomer or prepolymer, and if necessary, a silane coupling agent is also added. The monomer or prepolymer system is polymerized under certain condition, or the multi-element inorganic matter is directly mixed with the polymer, finally the polymer-inorganic matter composite material is prepared. Such materials have excellent thermal stability, and their thermal decomposition temperatures can be raised by tens or even hundreds of degrees, generally compared to the polymer bulk.
Chinese patent publication No. CN1277846C discloses an organic-inorganic nanocomposite and a method for preparing the same, and more particularly, to a method for preparing an organic-inorganic nanocomposite capable of uniformly dispersing silicate compounds in a multimeric medium by adding monomers, initiators, and emulsifiers to an ion-exchanged layered silicate prepared by adding a cationic initiator and a cationic chain transfer factor to the layered silicate compound to cause polymerization.
The organic-inorganic nanocomposite prepared by the above patent and the prior art has low transparency and poor ultraviolet absorption performance; the dispersity is not ideal; the interlayer spacing is small and the barrier property is poor.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing an organic-inorganic nanocomposite material by UV photopolymerization, which comprises the following operation steps:
S1: weighing 5-10 parts by weight of sulfonyl modified montmorillonite, 7-15 parts by weight of bisphenol A epoxy cationic photopolymerization resin and 80-100 parts by weight of solvent, stirring and mixing uniformly, and carrying out ultrasonic treatment;
S2: adding 0.1-0.5 part of photoinitiator, 0.1-0.5 part of propylene carbonate and 0.001-0.05 part of allyl dibutyl tin chloride, stirring and reacting to obtain the UV photopolymerization preparation organic-inorganic nanocomposite.
Preferably, the bisphenol A epoxy cationic photopolymerization resin is commercially available from Changxing chemical Co., ltd. EM828.
Preferably, the solvent is one of N, N-dimethylformamide, dimethyl sulfoxide and acetone.
Preferably, the ultrasonic treatment time is 10-30min.
Preferably, the reaction temperature of S2 is 40-60 ℃ for 1-3h.
Preferably, the photoinitiator is one of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, diaryl iodonium salt, triaryliodonium salt and aryl ferrocenium salt.
Preferably, the preparation method of the sulfonyl modified montmorillonite comprises the following steps:
b1: weighing 3-7 parts by weight of methyldiethoxysilane, 10-15 parts by weight of montmorillonite and 100-120 parts by weight of water, adding into a reaction kettle, heating for reaction, filtering and drying; obtaining methyldiethoxysilane/montmorillonite;
b2: adding 20-40 parts of diallyl sulfone, 0.002-0.05 part of allyl magnesium bromide, 0.001-0.005 part of platinum-carbon catalyst, 12-16 parts of methyldiethoxysilane/montmorillonite and 100-120 parts of ethanol into a reaction kettle, introducing nitrogen to replace air, controlling the temperature for reaction, centrifuging, and drying in vacuum to obtain the sulfonyl modified montmorillonite.
Preferably, the reaction temperature of the B1 is 40-50 ℃ and the reaction time is 60-120min.
Preferably, the reaction temperature of the B2 is 60-70 ℃ and the time is 4-5h.
Preferably, the vacuum drying time of the B2 is 1-3h.
Reaction principle: hydrolyzing and condensing methyl diethoxy silane and the hydroxyl of montmorillonite to obtain methyl diethoxy silane/montmorillonite; performing hydrosilylation reaction on diallyl sulfone and silicon-hydrogen bond of methyldiethoxysilane/montmorillonite to obtain modified montmorillonite containing glycidyl ether and sulfonyl; intercalation is carried out on the sulfonyl modified montmorillonite and bisphenol A epoxy cationic photopolymerization resin; and (3) performing UV photopolymerization on the epoxy group, propylene carbonate and allyl dibutyl tin chloride to obtain the organic-inorganic nanocomposite.
The beneficial effects are that: 1. the organic-inorganic nanocomposite prepared by the UV photopolymerization has the transparency as high as 93 at the wavelength of 680nm and has the characteristic of excellent ultraviolet absorption;
2. The organic-inorganic nanocomposite prepared by the UV photopolymerization has excellent dispersity;
3. the UV photopolymerization prepared by the invention prepares the organic-inorganic nanocomposite, and the molecular chain of the polymeric resin enters between the modified montmorillonite nano material sheets, so that the movement of the molecular chain segments is limited, the interlayer spacing of the composite is obviously improved, and the organic-inorganic nanocomposite can resist the permeation of various gases in two-dimensional directions, thereby achieving good heat resistance and air tightness.
Detailed Description
In order to further describe the technical means and effects adopted by the present invention for achieving the intended purpose, the following detailed description of the specific embodiments according to the present invention is given in conjunction with the preferred embodiments.
1. Degree of dispersion: observing by using a transmission electron microscope;
2. Transparency: detecting by an ultraviolet-visible light spectroscope;
3. interlayer spacing: and detecting by adopting an X-ray diffractometer.
Example 1: the UV photopolymerization method for preparing the organic-inorganic nanocomposite comprises the following operation steps:
S1: weighing 5g of sulfonyl modified montmorillonite, 7g of bisphenol A epoxy cationic photopolymerization resin and 80g of solvent, stirring and mixing uniformly, and carrying out ultrasonic treatment;
S2: adding 0.1g of photoinitiator, 0.1g of propylene carbonate and 0.001g of allyl dibutyl tin chloride, stirring and reacting to obtain the UV photopolymerization to prepare the organic-inorganic nanocomposite.
The bisphenol A epoxy cationic photopolymerization resin is commercially available from Changxing chemical Co Ltd EM828.
The solvent is N, N-dimethylformamide.
The ultrasonic treatment time is 10min.
The reaction temperature of S2 is 40 ℃ and the time is 1h.
The photoinitiator is phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide.
The preparation method of the sulfonyl modified montmorillonite comprises the following steps:
B1: weighing 3g of methyldiethoxysilane, 10g of montmorillonite and 100g of water, adding into a reaction kettle, heating for reaction, filtering and drying; obtaining methyldiethoxysilane/montmorillonite;
b2: 20g of diallyl sulfone, 0.002g of allyl magnesium bromide, 0.001g of platinum carbon catalyst, 12g of methyldiethoxysilane/montmorillonite and 100g of ethanol are added into a reaction kettle, nitrogen is introduced to replace air, the temperature is controlled for reaction, and after centrifugal separation, the sulfonyl modified montmorillonite is obtained by vacuum drying.
The reaction temperature of the B1 is 40 ℃ and the reaction time is 60min.
The reaction temperature of the B2 is 60 ℃ and the reaction time is 4 hours.
The vacuum drying time of the B2 is 1h.
Example 2: the UV photopolymerization method for preparing the organic-inorganic nanocomposite comprises the following operation steps:
S1: weighing 6g of sulfonyl modified montmorillonite, 9g of bisphenol A epoxy cationic photopolymerization resin and 85g of solvent, stirring and mixing uniformly, and carrying out ultrasonic treatment;
S2: adding 0.2g of photoinitiator, 0.2g of propylene carbonate and 0.02g of allyl dibutyl tin chloride, stirring and reacting to obtain the UV photopolymerization to prepare the organic-inorganic nanocomposite.
The bisphenol A epoxy cationic photopolymerization resin is commercially available from Changxing chemical Co Ltd EM828.
The solvent is dimethyl sulfoxide.
The ultrasonic treatment time is 15min.
The reaction temperature of S2 is 45 ℃ and the time is 2h.
The photoinitiator is diaryl iodonium salt.
The preparation method of the sulfonyl modified montmorillonite comprises the following steps:
B1: weighing 4g of methyldiethoxysilane, 12g of montmorillonite and 105g of water, adding into a reaction kettle, heating for reaction, filtering and drying; obtaining methyldiethoxysilane/montmorillonite;
B2: 25g of diallyl sulfone, 0.01g of allyl magnesium bromide, 0.002g of platinum carbon catalyst, 13g of methyldiethoxysilane/montmorillonite and 105g of ethanol are added into a reaction kettle, nitrogen is introduced to replace air, the temperature is controlled for reaction, and after centrifugal separation, the sulfonyl modified montmorillonite is obtained by vacuum drying.
The reaction temperature of the B1 is 45 ℃ and the reaction time is 80min.
The reaction temperature of the B2 is 65 ℃ and the reaction time is 4.5h.
The vacuum drying time of the B2 is 2h.
Example 3: the UV photopolymerization method for preparing the organic-inorganic nanocomposite comprises the following operation steps:
s1: weighing 8g of sulfonyl modified montmorillonite, 13g of bisphenol A epoxy cationic photopolymerization resin and 95g of solvent, stirring and mixing uniformly, and carrying out ultrasonic treatment;
S2: adding 0.4g of photoinitiator, 0.4g of propylene carbonate and 0.04g of allyl dibutyl tin chloride, stirring and reacting to obtain the UV photopolymerization to prepare the organic-inorganic nanocomposite.
The bisphenol A epoxy cationic photopolymerization resin is commercially available from Changxing chemical Co Ltd EM828.
The solvent is dimethyl sulfoxide.
The ultrasonic treatment time is 25min.
The reaction temperature of S2 is 55 ℃ and the time is 2h.
The photoinitiator is triaryliodonium salt.
The preparation method of the sulfonyl modified montmorillonite comprises the following steps:
B1: weighing 6g of methyldiethoxysilane, 14g of montmorillonite and 115g of water, adding into a reaction kettle, heating for reaction, filtering and drying; obtaining methyldiethoxysilane/montmorillonite;
B2: 35g of diallyl sulfone, 0.03g of allyl magnesium bromide, 0.004g of platinum-carbon catalyst, 15g of methyldiethoxysilane/montmorillonite and 115g of ethanol are added into a reaction kettle, nitrogen is introduced to replace air, the temperature is controlled for reaction, and after centrifugal separation, the sulfonyl modified montmorillonite is obtained by vacuum drying.
The reaction temperature of the B1 is 45 ℃ and the reaction time is 100min.
The reaction temperature of the B2 is 65 ℃ and the reaction time is 4.5h.
The vacuum drying time of the B2 is 2h.
Example 4: the UV photopolymerization method for preparing the organic-inorganic nanocomposite comprises the following operation steps:
s1: weighing 10g of sulfonyl modified montmorillonite, 15g of bisphenol A epoxy cationic photopolymerization resin and 100g of solvent, stirring and mixing uniformly, and carrying out ultrasonic treatment;
s2: adding 0.5g of photoinitiator, 0.5g of propylene carbonate and 0.05g of allyl dibutyl tin chloride, stirring and reacting to obtain the UV photopolymerization to prepare the organic-inorganic nanocomposite.
The bisphenol A epoxy cationic photopolymerization resin is commercially available from Changxing chemical Co Ltd EM828.
The solvent is acetone.
The ultrasonic treatment time is 30min.
The reaction temperature of S2 is 60 ℃ and the time is 3h.
The photoinitiator is aryl ferric salt.
The preparation method of the sulfonyl modified montmorillonite comprises the following steps:
B1: 7g of methyldiethoxysilane, 15g of montmorillonite and 120g of water are weighed, added into a reaction kettle, heated for reaction, filtered and dried; obtaining methyldiethoxysilane/montmorillonite;
B2: adding 40g of diallyl sulfone, 0.05g of allyl magnesium bromide, 0.005g of platinum carbon catalyst, 16g of methyldiethoxysilane/montmorillonite and 120g of ethanol into a reaction kettle, introducing nitrogen to replace air, controlling the temperature for reaction, centrifuging, and drying in vacuum to obtain the sulfonyl modified montmorillonite.
The reaction temperature of the B1 is 50 ℃ and the reaction time is 120min.
The reaction temperature of the B2 is 70 ℃ and the reaction time is 5 hours.
The vacuum drying time of the B2 is 3 hours.
Comparative example 1: this example was conducted in the same manner as in example 1 except that the sulfone group-modified montmorillonite was not added and unmodified montmorillonite was added.
Comparative example 2: this example was conducted in the same manner as in example 1 except that methyldiethoxysilane was not added.
Comparative example 3: this example was conducted in the same manner as in example 1 except that diallyl sulfone was not added.
Table 1: test results for each example and comparative example:
Through data analysis of each example and comparative example in table 1, the organic-inorganic nanocomposite material prepared by the present invention has a transparency of up to 93 at a wavelength of 680nm, and has excellent ultraviolet light absorption characteristics; has excellent dispersity; the organic-inorganic nano composite material has high interlayer spacing, and has good heat resistance and airtight effect.
The present invention is not limited to the above embodiments, but is capable of modification and variation in detail, and other modifications and variations can be made by those skilled in the art without departing from the scope of the present invention.
Claims (8)
- A method for preparing an organic-inorganic nanocomposite material by uv photopolymerization, characterized by: the operation steps are as follows:S1: weighing 5-10 parts by weight of sulfonyl modified montmorillonite, 7-15 parts by weight of bisphenol A epoxy cationic photopolymerization resin and 80-100 parts by weight of solvent, stirring and mixing uniformly, and carrying out ultrasonic treatment;s2: adding 0.1-0.5 part of photoinitiator, 0.1-0.5 part of propylene carbonate and 0.001-0.05 part of allyl dibutyl tin chloride, stirring, and reacting to obtain the UV photopolymerization to prepare the organic-inorganic nanocomposite;The preparation method of the sulfonyl modified montmorillonite comprises the following steps:b1: weighing 3-7 parts by weight of methyldiethoxysilane, 10-15 parts by weight of montmorillonite and 100-120 parts by weight of water, adding into a reaction kettle, heating for reaction, filtering and drying; obtaining methyldiethoxysilane/montmorillonite;B2: adding 20-40 parts of diallyl sulfone, 0.002-0.05 part of allyl magnesium bromide, 0.001-0.005 part of platinum-carbon catalyst, 12-16 parts of methyldiethoxysilane/montmorillonite and 100-120 parts of ethanol into a reaction kettle, introducing nitrogen to replace air, controlling the temperature for reaction, centrifuging, and drying in vacuum to obtain the sulfonyl modified montmorillonite.
- 2. The method of preparing an organic-inorganic nanocomposite material by UV photopolymerization according to claim 1, wherein: the solvent is one of N, N-dimethylformamide, dimethyl sulfoxide and acetone.
- 3. The method of preparing an organic-inorganic nanocomposite material by UV photopolymerization according to claim 1, wherein: the ultrasonic treatment time is 10-30min.
- 4. The method of preparing an organic-inorganic nanocomposite material by UV photopolymerization according to claim 1, wherein: the reaction temperature of the S2 is 40-60 ℃ and the reaction time is 1-3h.
- 5. The method of preparing an organic-inorganic nanocomposite material by UV photopolymerization according to claim 1, wherein: the photoinitiator is one of phenyl bis (2, 4, 6-trimethyl benzoyl) phosphine oxide, diaryl iodonium salt, triaryliodonium salt and aryl ferrocenium salt.
- 6. The method of preparing an organic-inorganic nanocomposite material by UV photopolymerization according to claim 1, wherein: the reaction temperature of the B1 is 40-50 ℃ and the reaction time is 60-120min.
- 7. The method of preparing an organic-inorganic nanocomposite material by UV photopolymerization according to claim 1, wherein: the reaction temperature of the B2 is 60-70 ℃ and the reaction time is 4-5h.
- 8. The method of preparing an organic-inorganic nanocomposite material by UV photopolymerization according to claim 1, wherein: the vacuum drying time of the B2 is 1-3h.
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| CN202410211320.5A CN117801181B (en) | 2024-02-27 | 2024-02-27 | Method for preparing organic-inorganic nanocomposite material by UV photopolymerization |
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