CN107739437A - A kind of nanometer silicon dioxide composite material preparation method - Google Patents
A kind of nanometer silicon dioxide composite material preparation method Download PDFInfo
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- CN107739437A CN107739437A CN201711056511.5A CN201711056511A CN107739437A CN 107739437 A CN107739437 A CN 107739437A CN 201711056511 A CN201711056511 A CN 201711056511A CN 107739437 A CN107739437 A CN 107739437A
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- material preparation
- silicon dioxide
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- 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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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- Silicon Compounds (AREA)
Abstract
A kind of nanometer silicon dioxide composite material preparation method, belongs to field of material preparation.It is characterized in that comprise the following steps：RNS A and methyl acrylate are added in flask, using methanol as solvent, magnetic agitation reaction is filtered after being washed after terminating with methanol, and half is obtained after drying for SiO2Dendritic macromole；Half is added in flask for SiO2And ethylenediamine, reacted by solvent magnetic agitation of methanol, synthesize SiO2Dendritic macromole；By lauric lactam, poplar bundles SiO2, water and phosphoric acid mixing add in polymeric kettle, with air in carbon dioxide replacement kettle, increasing temperature and pressure, discharged after then reacting pressurising at ambient pressure, material it is water cooled but after pelletizing, obtain Nano-meter SiO_22Composite.Pass through the improvement for original preparation technology, using the Michael addition reaction for repeating amido and methyl acrylate, be made amine type dendritic macromole, this law described nanometer silicon dioxide composite material preparation method technique it is simple, it is easily operated, there is great application value.
Description
Technical field
The invention belongs to field of material preparation, more particularly to a kind of nanometer silicon dioxide composite material preparation method.
Background technology
With the continuous development of science and technology, new material technology has also obtained large range of popularization and application, wherein nanometer skill
Art has been applied to the multiple fields such as space flight, living electric apparatus, clothes.Nano material is due to small-size effect, quantum effect
Should, interfacial effect and quantum tunneling effect etc., make it have many strange characteristics.But nano particle diameter is small, surface energy
Greatly, it is easy to reunite, influence its in the polymer scattered.
The content of the invention
A kind of present invention seek to address that above mentioned problem, there is provided nanometer silicon dioxide composite material preparation method.
A kind of nanometer silicon dioxide composite material preparation method, it is characterised in that comprise the following steps：
（1）15gRNS-A and 15mL methyl acrylates, using 100mL methanol as solvent, magnetic agitation are added in 250mL flask
Reaction, reaction are filtered after being washed after terminating with methanol, and half is obtained after drying for SiO2Anchor closes PAMAM type dendritic macromoles；
（2）10g half is added in 250mL flasks for SiO2With 10mL ethylenediamines, using 100mL methanol as solvent, magnetic agitation is anti-
Should, synthesize SiO2 Anchor closes PAMAM type dendritic macromoles；
（3）By lauric lactam, poplar bundles SiO2, water and phosphoric acid mixing add polymeric kettle in, use CO2Air in kettle is replaced, is risen
Temperature rise pressure keeps 2h, and normal pressure is then slowly deflated in 1.5h, and 270 DEG C of reaction 1.5h, discharge after pressurising at ambient pressure, material warp
Pelletizing after water cooling, obtain PA12/ Nano-meter SiO_2s2Composite.
A kind of nanometer silicon dioxide composite material preparation method of the present invention, it is characterised in that step（1）Described in
The temperature of magnetic agitation is 50 DEG C, time 24h.
A kind of nanometer silicon dioxide composite material preparation method of the present invention, it is characterised in that step（2）Described in
The temperature of magnetic agitation is 50 DEG C, time 24h.
A kind of nanometer silicon dioxide composite material preparation method of the present invention, it is characterised in that step（3）Described in
Increasing temperature and pressure process temperature is 260 DEG C, pressure 1.6MPa.
A kind of nanometer silicon dioxide composite material preparation method of the present invention, passes through changing for original preparation technology
Enter, using the Michael addition reaction for repeating amido and methyl acrylate, be made amine type dendritic macromole, this law it is described
Nanometer silicon dioxide composite material preparation method technique is simple, easily operated, has great application value.
Embodiment
A kind of nanometer silicon dioxide composite material preparation method, it is characterised in that comprise the following steps：
（1）15gRNS-A and 15mL methyl acrylates, using 100mL methanol as solvent, magnetic agitation are added in 250mL flask
Reaction, reaction are filtered after being washed after terminating with methanol, and half is obtained after drying for SiO2Anchor closes PAMAM type dendritic macromoles；
（2）10g half is added in 250mL flasks for SiO2With 10mL ethylenediamines, using 100mL methanol as solvent, magnetic agitation is anti-
Should, synthesize SiO2 Anchor closes PAMAM type dendritic macromoles；
（3）By lauric lactam, poplar bundles SiO2, water and phosphoric acid mixing add polymeric kettle in, use CO2Air in kettle is replaced, is risen
Temperature rise pressure keeps 2h, and normal pressure is then slowly deflated in 1.5h, and 270 DEG C of reaction 1.5h, discharge after pressurising at ambient pressure, material warp
Pelletizing after water cooling, obtain PA12/ Nano-meter SiO_2s2Composite.
A kind of nanometer silicon dioxide composite material preparation method of the present invention, step（1）Described in magnetic agitation
Temperature is 50 DEG C, time 24h.Step（2）Described in magnetic agitation temperature be 50 DEG C, time 24h.Step（3）Middle institute
It is 260 DEG C to state increasing temperature and pressure process temperature, pressure 1.6MPa.It is anti-by repeating Michael addition reaction and the amidatioon of ester group
Should, PAMAM type dendritic macromoles are successfully grafted to SiO2Surface, due to the growth of amine dendrimer algebraically, sky
Between steric hindrance also gradually increase, hinder in next step reaction progress.Meanwhile using carbomethoxy is end group half for product acid amides
Change in course of reaction, an amido in ethylenediamine molecule in addition to amidation process occurs with a carbomethoxy, meanwhile, the other end
Amido is also possible to react with intramolecular or another intermolecular carbomethoxy, obtains cross-linking products, so that algebraically increases
Terminate, this can equally reduce the amine groups content in product.The purer PA12 of notch impact strength of composite height.Tensile strength
Change is little, and bending strength and elongation at break are all on a declining curve.The increase of strand cladodification degree, can make between molecule away from
From increase, intermolecular active force reduces, thus the tensile strength of high polymer can reduce, but impact strength can improve.SiO2Table
Face is grafted with the structure of poplar bundles, with the increase of algebraically, the amido amount increase on surface, lauric lactam ring-opening polymerisation, molecule
It is linked on surface amine groups, the side chain of formation increases, and arrangement of the end of the chain in space is more closer than linear molecule, makes branching molecule
Size in the solution is less than the linear molecule of close molecular weight, so that relative viscosity reduces.The addition pair of nano-particle
Heterogeneous nucleating effect is played in PA12 crystallization, can quickly form a large amount of nucleus, completes crystallization quickly；SiO2The amine on surface
Base is connected with PA12 matrixes by chemical bond or hydrogen bond, adds SiO2Interaction between PA12, PA12 molecules are arranged
Enter lattice and play inhibition so that be difficult to be formed the spherocrystal of structural integrity., Nano-meter SiO_22The addition of particulate makes PA12 crystallization
Temperature improves, as the increase of algebraically has the trend gradually risen.Nano-meter SiO_22As nucleator, PA12 heterogeneous nucleation knots are induced
Crystalline substance, make crystallization more easy, can occur at relatively high temperatures.The degree of supercooling of composite has reduced compared with PA12, is advantageous to
Composite rapid crystallization during machine-shaping, improve material property.
Claims (4)
1. a kind of nanometer silicon dioxide composite material preparation method, it is characterised in that comprise the following steps：
（1）15gRNS-A and 15mL methyl acrylates, using 100mL methanol as solvent, magnetic agitation are added in 250mL flask
Reaction, reaction are filtered after being washed after terminating with methanol, and half is obtained after drying for SiO2Anchor closes PAMAM type dendritic macromoles；
（2）10g half is added in 250mL flasks for SiO2With 10mL ethylenediamines, using 100mL methanol as solvent, magnetic agitation is anti-
Should, synthesize SiO2 Anchor closes PAMAM type dendritic macromoles；
（3）By lauric lactam, poplar bundles SiO2, water and phosphoric acid mixing add polymeric kettle in, use CO2Replace air in kettle, heating
Boosting keeps 2h, and normal pressure is then slowly deflated in 1.5h, and 270 DEG C of reaction 1.5h, discharge, material is through water after pressurising at ambient pressure
Pelletizing after cooling, obtain PA12/ Nano-meter SiO_2s2Composite.
A kind of 2. nanometer silicon dioxide composite material preparation method as claimed in claim 1, it is characterised in that step（1）Middle institute
The temperature for stating magnetic agitation is 50 DEG C, time 24h.
A kind of 3. nanometer silicon dioxide composite material preparation method as claimed in claim 1, it is characterised in that step（2）Middle institute
The temperature for stating magnetic agitation is 50 DEG C, time 24h.
A kind of 4. nanometer silicon dioxide composite material preparation method as claimed in claim 1, it is characterised in that step（3）Middle institute
It is 260 DEG C to state increasing temperature and pressure process temperature, pressure 1.6MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711056511.5A CN107739437A (en) | 2017-10-23 | 2017-10-23 | A kind of nanometer silicon dioxide composite material preparation method |
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| CN201711056511.5A CN107739437A (en) | 2017-10-23 | 2017-10-23 | A kind of nanometer silicon dioxide composite material preparation method |
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| CN107739437A true CN107739437A (en) | 2018-02-27 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108852858A (en) * | 2018-07-12 | 2018-11-23 | 东华大学 | A kind of rambutan shape SiO2Base gear division compound resin and preparation method thereof |
| CN113264535A (en) * | 2021-06-28 | 2021-08-17 | 上海千溯生物科技有限公司 | Silicon dioxide nano particle with bent spikes and preparation method thereof |
| CN115044173A (en) * | 2022-07-11 | 2022-09-13 | 中山超分子新材料有限公司 | Corrosion-resistant high-elasticity composite fiber and preparation method thereof |
-
2017
- 2017-10-23 CN CN201711056511.5A patent/CN107739437A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108852858A (en) * | 2018-07-12 | 2018-11-23 | 东华大学 | A kind of rambutan shape SiO2Base gear division compound resin and preparation method thereof |
| CN113264535A (en) * | 2021-06-28 | 2021-08-17 | 上海千溯生物科技有限公司 | Silicon dioxide nano particle with bent spikes and preparation method thereof |
| CN115044173A (en) * | 2022-07-11 | 2022-09-13 | 中山超分子新材料有限公司 | Corrosion-resistant high-elasticity composite fiber and preparation method thereof |
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| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180227 |
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| WW01 | Invention patent application withdrawn after publication |