CN107312296A - A kind of PLA composite titania material and preparation method thereof - Google Patents
A kind of PLA composite titania material and preparation method thereof Download PDFInfo
- Publication number
- CN107312296A CN107312296A CN201710676743.4A CN201710676743A CN107312296A CN 107312296 A CN107312296 A CN 107312296A CN 201710676743 A CN201710676743 A CN 201710676743A CN 107312296 A CN107312296 A CN 107312296A
- Authority
- CN
- China
- Prior art keywords
- pla
- titanium dioxide
- composite
- titania material
- composite titania
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
Abstract
The invention discloses a kind of preparation method of PLA composite titania material, including：(1) PLA is dissolved in organic solvent, at room temperature 20~30min of magnetic agitation, obtains PLA solution；(2) titanium dioxide that organic-treating is crossed is added into above-mentioned PLA solution, ultrasonic disperse handles 10~15min, adds the tetrahydrofuran solution containing stannous octoate, 30~45min of magnetic agitation obtains PLA tio_2 suspension；(3) under vacuum, by above-mentioned PLA tio_2 suspension in 130~160 DEG C of oil baths 24~36h of isothermal reaction, obtain solid sample, then wash solid sample, dry, obtain PLA composite titania material.Preparation technology of the present invention is simple, and in composite made from the titanium dioxide crossed using organic-treating, titanium dioxide is dispersed in PLA matrix with nano-scale, effectively improves the calorifics and mechanical property of the composite.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of PLA-composite titania material and its preparation
Method.
Background technology
PLA (PLA) has excellent biodegradability, and its final product degraded is carbon dioxide and water, will not
Environment is polluted, is a kind of Biodegradable material of complete natural circulation type all.Therefore, environment and to develop into main body
Today, PLA is naturally favored by people, to it in the research in each field, using also increasingly extensive.But it is due to depositing
Mechanical strength is low, the low shortcoming of restoring force, it is allowed to be difficult to apply on those medical articles higher to mechanical property requirements.
TiO2As inorganic addition phase, the high-strength mechanical properties with its inorganic material, and also there is good parent
Water, sterilization and photocatalysis performance etc..By titanium dioxide and the compound obtained TiO of PLA2/ PLA composites, can either be played
Pliability, the machining property of polymer, can embody the mechanical strength and hardness of inorganic matter again；If by the two in nanoscale
It is upper compound, moreover it is possible to make composite that there are some special performances of nano material, so that the combination property of composite is obtained
Effectively lifting.
At present, TiO2The preparation method of/PLA composite mainly has chemical method and Physical.Chemical method mainly with
Lactide is raw material, and composite is prepared in the ring-opening polymerisation on titanium dioxide granule surface by it.But, in the prior art
Preparation technology is complicated, and obtained TiO2TiO in/PLA composites2Disperse uneven in PLA matrix, easily hair
Raw agglomeration.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of PLA-composite titania material and preparation method thereof,
It can solve the problem that problems of the prior art.
The content of the invention
It is existing to overcome it is an object of the invention to provide a kind of PLA-composite titania material and preparation method thereof
There is the deficiency in technology.
To achieve the above object, the present invention provides following technical scheme：
A kind of preparation method of PLA-composite titania material, including：
(1) PLA is dissolved in organic solvent, at room temperature 20~30min of magnetic agitation, obtains PLA solution；
(2) titanium dioxide that addition organic-treating is crossed into above-mentioned PLA solution, ultrasonic disperse processing 10~
15min, adds the tetrahydrofuran solution containing stannous octoate, and 30~45min of magnetic agitation obtains PLA-titanium dioxide and hanged
Supernatant liquid；
(3) under vacuum, by above-mentioned PLA-tio_2 suspension isothermal reaction in 130~160 DEG C of oil baths
24~36h, obtains solid sample, then washs solid sample, drying, obtains PLA-composite titania material.
It is preferred that, in step (2), the organic-treating process of titanium dioxide is：1) by 2~6g titanium dioxide and 100~
300mL butanone is mixed, and 15~20min of ultrasonic disperse obtains tio_2 suspension；2) by 1~2.4g methyl acetoxyaluminums third
Base trimethoxy silane is added in 100~300mL butanone, is stirred, is obtained the silicon of propyl trimethoxy containing methyl acetoxyaluminum
The butanone solution of alkane；3) butanone solution of tio_2 suspension and the propyl trimethoxy silicane containing methyl acetoxyaluminum is mixed
Close, flowed back 1~3h at 70~80 DEG C, cools down, and centrifuges, and 12~24h is dried in 100 DEG C of baking oven, is organised
Treated titanium dioxide.
It is preferred that, in step (1), the organic solvent is one kind in tetrahydrofuran or chloroform.
Technical solution of the present invention also provides a kind of PLA-titanium dioxide composite wood obtained according to above-mentioned preparation method
The mass ratio of titanium dioxide and PLA in material, the PLA-composite titania material is 1:5~20.
It is preferred that, the mass ratio of titanium dioxide and PLA in the PLA-composite titania material is 1:10.
Compared with prior art, the advantage of the invention is that：Preparation technology of the present invention is simple, is crossed using organic-treating
In composite made from titanium dioxide, titanium dioxide is dispersed in PLA matrix with nano-scale, is effectively improved
The calorifics and mechanical property of the composite.
Embodiment
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described by embodiment are only used
In the explanation present invention, without should be also without limitation on the present invention described in detail in claims.
The present invention discloses a kind of preparation method of PLA-composite titania material, including：
(1) PLA is dissolved in organic solvent, at room temperature 20~30min of magnetic agitation, obtains PLA solution；
(2) titanium dioxide that addition organic-treating is crossed into above-mentioned PLA solution, ultrasonic disperse processing 10~
15min, adds the tetrahydrofuran solution containing stannous octoate, and 30~45min of magnetic agitation obtains PLA-titanium dioxide and hanged
Supernatant liquid；
(3) under vacuum, by above-mentioned PLA-tio_2 suspension isothermal reaction in 130~160 DEG C of oil baths
24~36h, obtains solid sample, then washs solid sample, drying, obtains PLA-composite titania material.
In above-mentioned steps (1), the organic solvent is one kind in tetrahydrofuran or chloroform.
In one embodiment, the organic-treating process of titanium dioxide is：
1) 2~6g titanium dioxide is mixed with 100~300mL butanone, 15~20min of ultrasonic disperse obtains titanium dioxide
Suspension；
2) 1~2.4g methyl acetoxyaluminums propyl trimethoxy silicane is added in 100~300mL butanone, stirred,
Obtain the butanone solution of the propyl trimethoxy silicane containing methyl acetoxyaluminum；
3) tio_2 suspension is mixed with the butanone solution of the propyl trimethoxy silicane containing methyl acetoxyaluminum, 70
Flowed back 1~3h at~80 DEG C, cools down, and centrifuges, and 12~24h is dried in 100 DEG C of baking oven, obtains what organic-treating was crossed
Titanium dioxide.
Embodiment
1st, the organic-treating of titanium dioxide
1) 6g titanium dioxide is mixed with 300mL butanone, ultrasonic disperse 20min obtains tio_2 suspension；
2) 2.4g methyl acetoxyaluminums propyl trimethoxy silicane is added in 300mL butanone, stirred, obtain containing first
The butanone solution of base acetyloxypropyl trimethoxy silane；
3) tio_2 suspension is mixed with the butanone solution of the propyl trimethoxy silicane containing methyl acetoxyaluminum, 80
Flowed back 2h at DEG C, cools down, and centrifuges, and 20h is dried in 100 DEG C of baking oven, the titanium dioxide that organic-treating is crossed is obtained.
2nd, PLA-composite titania material is prepared
(1) PLA is dissolved in tetrahydrofuran, at room temperature magnetic agitation 30min, obtains PLA solution；
(2) titanium dioxide that organic-treating according to the method described above is crossed, ultrasonic disperse are added into above-mentioned PLA solution
15min is handled, the tetrahydrofuran solution containing stannous octoate is added, magnetic agitation 40min obtains PLA-titanium dioxide and hanged
Supernatant liquid；
(3) under vacuum, by above-mentioned PLA-tio_2 suspension in 150 DEG C of oil baths isothermal reaction 36h,
Solid sample is obtained, then solid sample is washed, dries, obtains PLA-composite titania material.
Technical scheme also provides a kind of PLA-titanium dioxide obtained according to above-mentioned preparation method and is combined
The mass ratio of titanium dioxide and PLA in material, the PLA-composite titania material is 1:5~20, further
The mass ratio of titanium dioxide and PLA in ground, the PLA-composite titania material is 1:10.
In PLA-composite titania material made from method in the present invention, organised because titanium dioxide is used
Process is handled so that the absorption of methyl acetoxyaluminum propyl trimethoxy silicane forms protective layer in titanium dioxide surface,
Its space steric effect enhances the repulsive interaction between TiO 2 particles, improves the scattered stability of particle, so that
Titanium dioxide can be dispersed in PLA matrix with nano-scale, effectively improve the calorifics and mechanics of the composite
Performance.
Mechanics is carried out to the composite in the present invention at 20 DEG C using Instrong-4466 type universal material experimental machines
Performance test understands that the tensile strength and modulus of elasticity of the composite are greatly improved；Using TA2100-SDT2960 instruments
Thermogravimetic analysis (TGA) is carried out to the composite in the present invention and understands that the heat decomposition temperature of the composite increases.
Finally, in addition it is also necessary to explanation, term " comprising ", "comprising" or its any other variant are intended to non-exclusive
Property include so that process, method, article or equipment including a series of key elements not only include those key elements, and
Also include other key elements for being not expressly set out, or also include for this process, method, article or equipment inherently
Key element.
Claims (5)
1. a kind of preparation method of PLA-composite titania material, it is characterised in that including：
(1) PLA is dissolved in organic solvent, at room temperature 20~30min of magnetic agitation, obtains PLA solution；
(2) titanium dioxide that organic-treating is crossed is added into above-mentioned PLA solution, ultrasonic disperse handles 10~15min, then
The tetrahydrofuran solution containing stannous octoate is added, 30~45min of magnetic agitation obtains PLA-tio_2 suspension；
(3) under vacuum, by above-mentioned PLA-tio_2 suspension in 130~160 DEG C of oil baths isothermal reaction 24~
36h, obtains solid sample, then washs solid sample, drying, obtains PLA-composite titania material.
2. the preparation method of PLA-composite titania material according to claim 1, it is characterised in that step (2)
In, the organic-treating process of titanium dioxide is：1) 2~6g titanium dioxide is mixed with 100~300mL butanone, ultrasonic disperse
15~20min, obtains tio_2 suspension；2) by 1~2.4g methyl acetoxyaluminums propyl trimethoxy silicane add 100~
In 300mL butanone, stir, obtain the butanone solution of the propyl trimethoxy silicane containing methyl acetoxyaluminum；3) by titanium dioxide
Titanium suspension is mixed with the butanone solution of the propyl trimethoxy silicane containing methyl acetoxyaluminum, and flow back 1~3h at 70~80 DEG C,
Cooling, is centrifuged, and 12~24h is dried in 100 DEG C of baking oven, the titanium dioxide that organic-treating is crossed is obtained.
3. the preparation method of PLA-composite titania material according to claim 1, it is characterised in that step (1)
In, the organic solvent is one kind in tetrahydrofuran or chloroform.
4. a kind of PLA-composite titania material that preparation method according to claim 1 is obtained, it is characterised in that institute
The mass ratio for stating the titanium dioxide in PLA-composite titania material and PLA is 1:5~20.
5. PLA-composite titania material according to claim 4, it is characterised in that the PLA-titanium dioxide
The mass ratio of titanium dioxide and PLA in titanium composite material is 1:10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710676743.4A CN107312296A (en) | 2017-08-09 | 2017-08-09 | A kind of PLA composite titania material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710676743.4A CN107312296A (en) | 2017-08-09 | 2017-08-09 | A kind of PLA composite titania material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107312296A true CN107312296A (en) | 2017-11-03 |
Family
ID=60175251
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710676743.4A Pending CN107312296A (en) | 2017-08-09 | 2017-08-09 | A kind of PLA composite titania material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107312296A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112375356A (en) * | 2020-11-27 | 2021-02-19 | 东莞全球环保科技有限公司 | Biodegradable soft shell forming process and mobile phone soft shell prepared by same |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215411A (en) * | 2008-01-21 | 2008-07-09 | 南京大学 | Light degradation antibiotic polylactic acid material and preparation method thereof |
| CN102964572A (en) * | 2012-12-06 | 2013-03-13 | 西北师范大学 | Preparation method of titanium dioxide/polylactic acid nanocomposite |
| CN103254410A (en) * | 2013-06-03 | 2013-08-21 | 北京理工大学 | Preparation method of high-molecular-weight polylactic acid based on metal powder dehydrating agent |
-
2017
- 2017-08-09 CN CN201710676743.4A patent/CN107312296A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215411A (en) * | 2008-01-21 | 2008-07-09 | 南京大学 | Light degradation antibiotic polylactic acid material and preparation method thereof |
| CN102964572A (en) * | 2012-12-06 | 2013-03-13 | 西北师范大学 | Preparation method of titanium dioxide/polylactic acid nanocomposite |
| CN103254410A (en) * | 2013-06-03 | 2013-08-21 | 北京理工大学 | Preparation method of high-molecular-weight polylactic acid based on metal powder dehydrating agent |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112375356A (en) * | 2020-11-27 | 2021-02-19 | 东莞全球环保科技有限公司 | Biodegradable soft shell forming process and mobile phone soft shell prepared by same |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Dong et al. | Highly transparent and toughened poly (methyl methacrylate) nanocomposite films containing networks of cellulose nanofibrils | |
| Kumar et al. | Improving mechanical and thermal properties of TiO2-epoxy nanocomposite | |
| Zhu et al. | High-adsorption, self-extinguishing, thermal, and acoustic-resistance aerogels based on organic and inorganic waste valorization from cellulose nanocrystals and red mud | |
| Sui et al. | Nanocomposite hydrogels based on carbon dots and polymers | |
| Maeda et al. | Pickering-type water-in-oil-in-water multiple emulsions toward multihollow nanocomposite microspheres | |
| Goyat et al. | Innovative application of ultrasonic mixing to produce homogeneously mixed nanoparticulate-epoxy composite of improved physical properties | |
| Aliakbari et al. | Multi-nationality epoxy adhesives on trial for future nanocomposite developments | |
| Li et al. | Natural rubber-based elastomer reinforced by chemically modified multiscale leather collagen fibers with excellent toughness | |
| CN104558664B (en) | The method that strong hydrophilicity PET film is prepared using graphene oxide and nano silicon dioxide | |
| CN107324296A (en) | The method of modifying and hydroxyl modification boron nitride of hexagonal boron nitride | |
| CN105907042B (en) | A kind of functionalized carbon nano-tube epoxy resin nano composites and preparation method thereof | |
| CN103962074B (en) | A kind of hollow sub-micron, its preparation method and application | |
| Ghasemi et al. | Effects of multi‐walled carbon nanotube functionalization on the morphological and mechanical properties of nanocomposite foams based on poly (vinyl chloride)/(wood flour)/(multi‐walled carbon nanotubes) | |
| Wang et al. | Castor oil‐based polyurethane/silica nanocomposites: Morphology, thermal and mechanical properties | |
| Mathur et al. | Dynamic mechanical analysis of PVC/TiO 2 nanocomposites | |
| CN110105483A (en) | A kind of hydrotalcite dual network Nanometer composite hydrogel and preparation method thereof | |
| Xu et al. | Heat-resistant and microwaveable poly (lactic acid) by quantum-dot-promoted stereocomplexation | |
| CN107312296A (en) | A kind of PLA composite titania material and preparation method thereof | |
| Gong et al. | An enhancement on the dielectric performance of poly (vinylidene fluoride)-based composite with graphene oxide-BaTiO3 hybrid | |
| Hu et al. | Interfacial engineering with rigid nanoplatelets in immiscible polymer blends: interface strengthening and interfacial curvature controlling | |
| CN107880460A (en) | A kind of cellulose nano-fibrous enhancing composite membrane of UV resistance and preparation method thereof | |
| Mallakpour et al. | Green route for the synthesis of alanine-based poly (amide-imide) nanocomposites reinforced with the modified ZnO by poly (vinyl alcohol) as a biocompatible coupling agent | |
| Parushuram et al. | Facile fabrication of silk fibroin microparticles: their characterization and potential adsorption study | |
| Nguyen et al. | Elaboration and dielectric property of modified PZT/epoxy nanocomposites | |
| CN106947291A (en) | A kind of preparation method of modified manometer silicon dioxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171103 |
|
| RJ01 | Rejection of invention patent application after publication |