CN107903596A - A kind of high temperature resistant lactic acid composite material and preparation method thereof - Google Patents
A kind of high temperature resistant lactic acid composite material and preparation method thereof Download PDFInfo
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- CN107903596A CN107903596A CN201711244371.4A CN201711244371A CN107903596A CN 107903596 A CN107903596 A CN 107903596A CN 201711244371 A CN201711244371 A CN 201711244371A CN 107903596 A CN107903596 A CN 107903596A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses a kind of high temperature resistant lactic acid composite material and preparation method thereof, including following parts by weight raw material to be prepared：5 15 parts of nano-aluminum hydroxide, 5 10 parts of modifying agent, 20 35 parts of polyethyleneglycol diacrylate, 55 70 parts of polylactic acid, 0.3 0.8 parts of coupling agent, 25 parts of crosslinking agent, 5 10 parts of calcium succinate, 0.1 0.3 parts of zinc stearate；The present invention is for composite by the nano-aluminum hydroxide Jing Guo specific aim modification and polylactic acid, and nano-aluminum hydroxide is set to be dispersed in polylactic acid system, obtained lactic acid composite material resistance to elevated temperatures is excellent, is conducive to application of the polylactic acid in more areas.
Description
Technical field
The present invention relates to modified material field, and in particular to a kind of high temperature resistant lactic acid composite material and preparation method thereof.
Background technology
Polylactic acid（PLA）It is a kind of new biodegradation material, uses reproducible plant resources（Such as corn）Carried
The starch material gone out is made.Lactic acid is made via fermentation process in starch material, then is converted into polylactic acid by chemical synthesis.It has
There is good biodegradability, can be degradable by microorganism in nature after use, carbon dioxide and water are ultimately generated, no
Environment is polluted, this is highly beneficial to environmental protection, is generally acknowledged environment-friendly material.The mechanical performance and physics of poly-lactic acid material
Functional, compatibility is good, and many advantages, such as breathing freely, the every field in life and production has extensive application.
With the continuous improvement that people require material resistance to elevated temperatures, the polylactic acid without heat resist modification has been difficult to full
Sufficient demand, thus, heat resist modification is carried out to polylactic acid and is necessitated.Now to the heat resist modification processing method kind of polylactic acid
Class is various, and modified effect is also fine, especially with the appearance and application of nano material, the heat-resisting quantity increase effect of polylactic acid
Significantly, polylactic acid is enable largely to be used in more areas, but there is also deficiency.Although nano material has high temperature resistant enhancing effect
It is good, the advantages of additive amount is small, but there is also difficulties in dispersion, it is of high cost the defects of.During heat resist modification is carried out, nanometer material
The scattered inequality of material can influence its high-temperature resistant result, and obtained modified material heat-resisting quantity is relatively low, production to modified material and should
With adversely affecting.
The content of the invention
A kind of the defects of it is an object of the invention to overcome existing lactic acid composite material heat-resisting quantity poor, there is provided resistance to height
Warm lactic acid composite material and preparation method thereof；The present invention is by the nano-aluminum hydroxide and polylactic acid Jing Guo specific aim modification
It is for composite, and nano-aluminum hydroxide is dispersed in polylactic acid system, obtained lactic acid composite material heat-resisting quantity
Can be excellent, be conducive to application of the polylactic acid in more areas.
In order to realize foregoing invention purpose, the present invention provides a kind of high temperature resistant lactic acid composite material, including it is following heavy
Amount part raw material are prepared：5-15 parts of nano-aluminum hydroxide, 5-10 parts of modifying agent, 20-35 parts of polyethylene glycol dipropyl
Olefin(e) acid ester, 55-70 parts of polylactic acid, 0.3-0.8 parts of coupling agent, 2-5 parts of crosslinking agent, 5-10 parts of calcium succinate, 0.1-
0.3 part of zinc stearate.
A kind of above-mentioned high temperature resistant lactic acid composite material, can increase the resistance to height of resin material according to nano-aluminum hydroxide and crosslinking
The basic principle of warm nature, not only by targetedly screening modifying agent, coupling agent and the species of crosslinking agent, to improve a nanometer hydrogen-oxygen
Change the compatibility between aluminium and polylactic acid, and make nano-aluminum hydroxide disperse evenly, to make nano-aluminum hydroxide in polylactic acid
It is more preferable to the heat-resisting quantity humidification of polylactic acid, also make modified polylactic acid compound by controlling the degree of polymerization of polylactic acid
Material reaches optimum balance relation between heat-resisting quantity and processability, so that the lactic acid composite material made is with excellent
Under conditions of different heat-resisting quantity, it may have excellent processability, allows it to be applied in more areas.
A kind of above-mentioned high temperature resistant lactic acid composite material, wherein, the nano-aluminum hydroxide particle diameter is 10-80nm；Receive
Rice aluminium hydroxide particle diameter is smaller, and dispersiveness is poorer, and nano-aluminum hydroxide particle diameter is bigger, and the high temperature resistant humidification of polylactic acid is got over
Difference；Preferably, the nano-aluminum hydroxide particle diameter is 30-50nm；Most preferably, the nano-aluminum hydroxide particle diameter is
40nm。
A kind of above-mentioned high temperature resistant lactic acid composite material, wherein, the modifying agent is butyl titanate and tripotassium phosphate
The mixture of ester composition；The modifying agent can improve the compatibility of nano-aluminum hydroxide and polylactic acid and in nanometer hydrogen
Aoxidize aluminium surface and form polar group, beneficial to scattered；Preferably, butyl titanate and trimethyl phosphate in the modifying agent
The ratio between amount of material is 1 ︰ 1.
A kind of above-mentioned high temperature resistant lactic acid composite material, wherein, the degree of polymerization of polyethyleneglycol diacrylate is bigger, then hands over
The heat-resisting quantity of lactic acid composite material is poorer after connection, and processability is better, and the polymer of polyethyleneglycol diacrylate is smaller, then
The heat-resisting quantity of lactic acid composite material is better after crosslinking, and processability is poorer, therefore, selects rational polyethylene glycol diacrylate
Polyisocyanate polyaddition degree, is the important means for balancing heat-resisting quantity and processability.The degree of polymerization of the polyethyleneglycol diacrylate is
180-250；Preferably, the degree of polymerization of the polyethyleneglycol diacrylate is 200-230；Optimal, described poly- second two
The degree of polymerization of alcohol diacrylate is 210；By preferred, obtained lactic acid composite material both has excellent heat-resisting quantity,
Also there is preferable processability, be adapted to the application in more areas.
Wherein, the polymerisation degree of poly-lactic acid is 600-1000；Preferably, the degree of polymerization of the polylactic acid is 700-900；
Most preferably, the degree of polymerization of the polylactic acid is 800；By preferred, obtained lactic acid composite material had both had excellent
Heat-resisting quantity, it may have preferable processability.
A kind of above-mentioned high temperature resistant lactic acid composite material, wherein, the coupling agent is aluminate coupling agent；Aluminate energy
Increase the compatibility between nano-aluminum hydroxide and polylactic acid and modifying agent, improve the performance of lactic acid composite material.
Wherein, the crosslinking agent is methacrylic acid, which can be by the polymer former material of two kinds of different polymerization degrees
The appropriate crosslinking of material, improves the heat-resisting quantity of lactic acid composite material.
A kind of above-mentioned high temperature resistant lactic acid composite material, wherein, its raw material further includes dispersant, plasticizer, antistatic
One or more auxiliary agents in agent, coloring agent, brightener；Above-mentioned auxiliary agent can improve the processability of lactic acid composite material, increase
Its feature etc. is added to act on, so as to increase its applicability.
In order to realize foregoing invention purpose, further, present invention also offers a kind of high temperature resistant lactic acid composite material
Preparation method, comprise the following steps：
（1）Nano-aluminum hydroxide is handled with coupling agent；
（2）Nano-aluminum hydroxide Jing Guo coupling agent treatment is subjected to cladding processing with modifying agent；
（3）By the nano-aluminum hydroxide after cladding and polylactic acid processing for composite in the electric field after mixing, mixed
Material；
（4）Mixture is being carried out after mixing with polyethyleneglycol diacrylate, crosslinking agent, zinc stearate, calcium succinate
Combined processing, obtains high temperature resistant lactic acid composite material.
A kind of preparation method of high temperature resistant lactic acid composite material, first carries out at coupling nano-aluminum hydroxide with coupling agent
Reason, increase nano-aluminum hydroxide and modifying agent, the compatibility of polylactic acid；Place is modified to nano-aluminum hydroxide with modifying agent again
Reason, and form polar group on its surface；Finally make the polarity in nano-aluminum hydroxide surface and polylactic acid chain using external electric field
Group polarizes, powered, by repelling each other between electric charge or attracting principle, while making nano-aluminum hydroxide dispersed, also can
It is bonded with the polar group in polylactic acid chain, so that the high temperature resistant enhancing effect of nano-aluminum hydroxide obtains maximum body
It is existing, so as to get polydactyl acid heat-resisting quantity significantly improve；The preparation method is simple and reliable, is suitable for high temperature resistant polylactic acid
Extensive, the industrialized production of composite material.
A kind of preparation method of above-mentioned high temperature resistant lactic acid composite material, wherein, it is preferred that step 1 carries out coupling processing
During can use ultrasonic wave aid in；Shaken by the high speed of ultrasonic wave, make nano-aluminum hydroxide dispersiveness more preferable, and to coupling
Processing has facilitation.
A kind of preparation method of above-mentioned high temperature resistant lactic acid composite material, wherein, the electric field energy described in step 3 is to group
Polarization is produced, makes group powered, so as to promote the scattered and bonded effect of nano-aluminum hydroxide, improves polydactyl acid
Heat-resisting quantity.
Preferably, the electric field strength is 1.5-2.5kv/m；Electric field strength is too small, and polarization effect is weak, to nanometer hydrogen-oxygen
The dispersion effect for changing aluminium is poor；Electric field strength is excessive, and polarization effect is too strong, and intermolecular force is too big, and strand produces orientation and moves
It is dynamic, arrangement and the bonded performance for having an impact, may be decreased lactic acid composite material to strand；Most preferably, it is described
Electric field strength is 1.8-2.0kv/m.
Wherein, it is preferred that the electric field is the constant parallel electric field of direction of an electric field；The constant parallel electric field of direction of an electric field
Best to the polarization effect of polar group, group intermolecular forces are stablized, and the scattered and bonded promotion to nano-aluminum hydroxide is made
Use best results.
Compared with prior art, beneficial effects of the present invention：
1st, lactic acid composite material of the present invention targetedly screens the species of modifying agent, coupling agent and crosslinking agent, makes a nanometer hydrogen-oxygen
The compatibility changed between aluminium and polylactic acid is more preferable, and the dispersiveness in polylactic acid is more preferable, and nano-aluminum hydroxide is to the resistance to of polylactic acid
High temperatures humidification is more preferable.
2nd, lactic acid composite material of the present invention is made by controlling the degree of polymerization of polylactic acid and polyethyleneglycol diacrylate
Modified lactic acid composite material reaches optimum balance relation between heat-resisting quantity and processability, so as to get polylactic acid answer
Condensation material is under conditions of with excellent heat-resisting quantity, it may have excellent processability.
3rd, the preparation method of lactic acid composite material of the present invention, using the polarization of external electric field, can promote nanometer hydrogen-oxygen
It is scattered and bonded in polylactic acid system to change aluminium, the high temperature resistant enhancing effect of nano-aluminum hydroxide is more preferable, obtained polylactic acid
The heat-resisting quantity higher of composite material.
4th, the preparation method of lactic acid composite material of the present invention is simple, reliable, is adapted to high temperature resistant lactic acid composite material
On a large scale, industrialized production.
Embodiment
With reference to test example and embodiment, the present invention is described in further detail.But this should not be understood
Following embodiment is only limitted to for the scope of the above-mentioned theme of the present invention, it is all that this is belonged to based on the technology that present invention is realized
The scope of invention.
Embodiment 1
（1）10 parts of nano-aluminum hydroxide is handled with 0.6 part of Aluminate；
（2）By the nano-aluminum hydroxide Jing Guo coupling agent treatment with 3.5 parts of butyl titanate and 3.5 parts of trimethyl phosphate into
The processing of row cladding；
（3）By polylactic acid that the nano-aluminum hydroxide after cladding and 60 parts of the degree of polymerization are 800 after mixing in electric field strength
To be extruded in the constant parallel electric field of the direction of an electric field of 2.0kv/m, mixture is obtained；
（4）Polyethyleneglycol diacrylate, the 4 parts of metering systems of the mixture that step 3 is obtained and 28 parts of the degree of polymerization for 210
Acid, 8 parts of calcium succinate, 0.2 part of zinc stearate are extruded after mixing, obtain high temperature resistant lactic acid composite material.
Embodiment 2
（1）5 parts of nano-aluminum hydroxide is handled with 0.3 part of Aluminate；
（2）By the nano-aluminum hydroxide Jing Guo coupling agent treatment with 2.5 parts of butyl titanate and 2.5 parts of trimethyl phosphate into
The processing of row cladding；
（3）By polylactic acid that the nano-aluminum hydroxide after cladding and 55 parts of the degree of polymerization are 1000 after mixing in electric-field strength
Spend in the electric field for 2.5kv/m and extruded, obtain mixture；
（4）Polyethyleneglycol diacrylate, the 2 parts of metering systems of the mixture that step 3 is obtained and 20 parts of the degree of polymerization for 180
Acid, 5 parts of calcium succinate, 0.3 part of zinc stearate are extruded after mixing, obtain high temperature resistant lactic acid composite material.
Embodiment 3
（1）15 parts of nano-aluminum hydroxide is handled with 0.8 part of Aluminate；
（2）Nano-aluminum hydroxide Jing Guo coupling agent treatment is wrapped with 5 parts of butyl titanate and 4 parts of trimethyl phosphate
Cover processing；
（3）By polylactic acid that the nano-aluminum hydroxide after cladding and 70 parts of the degree of polymerization are 600 after mixing in electric-field strength
Spend to be extruded in the constant parallel electric field of the direction of an electric field of 1.5kv/m, obtain mixture；
（4）Polyethyleneglycol diacrylate, the 5 parts of metering systems of the mixture that step 3 is obtained and 35 parts of the degree of polymerization for 250
Acid, 10 parts of calcium succinate, 0.1 part of zinc stearate are extruded after mixing, obtain high temperature resistant lactic acid composite material.
Comparative example 1
（1）10 parts of nano-aluminum hydroxide is handled with 0.6 part of Aluminate；
（2）By the nano-aluminum hydroxide Jing Guo coupling agent treatment and 7 parts of dispersant, the polylactic acid that 60 parts of the degree of polymerization is 800
Extruded after mixing in the constant parallel electric field of the direction of an electric field that electric field strength is 1.2kv/m, obtain mixture；
（3）Polyethyleneglycol diacrylate, the 4 parts of metering systems of the mixture that step 2 is obtained and 28 parts of the degree of polymerization for 210
Acid, 8 parts of calcium succinate, 0.2 part of zinc stearate are extruded after mixing, obtain lactic acid composite material.
Comparative example 2
（1）10 parts of nano-aluminum hydroxide is handled with 0.6 part of Aluminate；
（2）By the nano-aluminum hydroxide Jing Guo coupling agent treatment with 3.5 parts of butyl titanate and 3.5 parts of trimethyl phosphate into
The processing of row cladding；
（3）It is 210 by polylactic acid that the nano-aluminum hydroxide after cladding and 60 parts of the degree of polymerization are 800,28 parts of the degree of polymerization
Polyethyleneglycol diacrylate, 4 parts of methacrylic acids, 8 parts of calcium succinate, 0.2 part of zinc stearate carry out after mixing
Extrusion, obtains lactic acid composite material.
Comparative example 3
（1）10 parts of nano-aluminum hydroxide is handled with 0.6 part of Aluminate；
（2）Nano-aluminum hydroxide Jing Guo coupling agent treatment is carried out with 3.5 parts of polystyrene and 3.5 parts of trimethyl phosphate
Cladding processing；
（3）By polylactic acid that the nano-aluminum hydroxide after cladding and 60 parts of the degree of polymerization are 800 after mixing in electric field strength
To be extruded in the constant parallel electric field of the direction of an electric field of 2.0kv/m, mixture is obtained；
（4）Polyethyleneglycol diacrylate, the 4 parts of metering systems of the mixture that step 3 is obtained and 28 parts of the degree of polymerization for 210
Acid, 8 parts of calcium succinate, 0.2 part of zinc stearate are extruded after mixing, obtain lactic acid composite material.
Comparative example 4
（1）10 parts of nano-aluminum hydroxide is handled with 0.6 part of Aluminate；
（2）By the nano-aluminum hydroxide Jing Guo coupling agent treatment with 3.5 parts of butyl titanate and 3.5 parts of trimethyl phosphate into
The processing of row cladding；
（3）By the polyethyleneglycol diacrylate of the nano-aluminum hydroxide after cladding and 28 parts of the degree of polymerization for 210,4 parts of methyl
Acrylic acid, 8 parts of calcium succinate, 0.2 part of zinc stearate, 60 parts of the degree of polymerization be 800 polylactic acid after mixing in electricity
Field intensity is to be extruded in the constant parallel electric field of the direction of an electric field of 2.0kv/m, obtains lactic acid composite material.
Comparative example 5
（1）10 parts of nano-aluminum hydroxide is handled with 0.6 part of Aluminate；
（2）By the nano-aluminum hydroxide Jing Guo coupling agent treatment with 3.5 parts of butyl titanate and 3.5 parts of trimethyl phosphate into
The processing of row cladding；
（3）By polylactic acid that the nano-aluminum hydroxide after cladding and 60 parts of the degree of polymerization are 500 after mixing in electric field strength
To be extruded in the constant parallel electric field of the direction of an electric field of 2.0kv/m, mixture is obtained；
（4）Polyethyleneglycol diacrylate, 4 parts of the butanedioic acid of the mixture that step 3 is obtained and 28 parts of the degree of polymerization for 150
Calcium, 0.2 part of zinc stearate, 8 parts of methacrylic acids are extruded after mixing, obtain lactic acid composite material.
By the lactic acid composite material in above-described embodiment 1-3 and comparative example 1-5, performance detection is carried out, record data are such as
Under：
| Performance | Heat distortion temperature（℃） | Processability |
| Embodiment 1 | 142 | ++++ |
| Embodiment 2 | 141 | ++++ |
| Embodiment 3 | 141 | ++++ |
| Comparative example 1 | 131 | ++++ |
| Comparative example 2 | 133 | ++++ |
| Comparative example 3 | 137 | ++++ |
| Comparative example 4 | 138 | ++++ |
| Comparative example 5 | 142 | ++ |
| Polylactic acid | 120 | +++ |
Note："+" is more, illustrates that performance is better.
Above-mentioned analysis of experimental data is understood, the high temperature resistant polylactic acid composite wood of the present invention being prepared in embodiment 1-3
Material, nano-aluminum hydroxide are uniformly dispersed, and good with the compatibility of polylactic acid, lactic acid composite material heat-resisting quantity is good, and processability is good；
And in comparative example 1, modifying agent is not used processing is modified to nano-aluminum hydroxide, although adding dispersant, nanometer hydrogen
Alumina dispersion effect is poor, and the poor compatibility with polylactic acid, the heat-resisting quantity of lactic acid composite material significantly reduces；Comparative example 2
In not processing for composite in the electric field, nano-aluminum hydroxide dispersion effect is poor, and the heat-resisting quantity of lactic acid composite material is notable
Reduce；Modifying agent is not the application defined in comparative example 3, and nano-aluminum hydroxide dispersion effect is poor, lactic acid composite material
Heat-resisting quantity significantly reduce；Cross-linking reaction equally carries out in the electric field in comparative example 4, and electric field produces unfavorable shadow to cross-linking reaction
Ring, so as to get lactic acid composite material heat-resisting quantity reduce；Two propylene of polylactic acid and polyethylene glycol used in comparative example 5
The acid esters degree of polymerization is too small, although heat-resisting quantity increased after compound, its processability significantly reduces, and it is compound to be unfavorable for polylactic acid
The application of material.
Claims (10)
1. a kind of high temperature resistant lactic acid composite material, it is characterised in that be prepared including following parts by weight raw material：5-15 parts
Nano-aluminum hydroxide, 5-10 parts of modifying agent, 20-35 parts of polyethyleneglycol diacrylate, 55-70 parts of polylactic acid,
0.3-0.8 parts of coupling agent, 2-5 parts of crosslinking agent, 5-10 parts of calcium succinate, 0.1-0.3 parts of zinc stearate；The modification
The mixture that agent forms for butyl titanate with trimethyl phosphate；The coupling agent is aluminate coupling agent, and the crosslinking agent is
Methacrylic acid；The degree of polymerization of the polyethyleneglycol diacrylate is 180-250；The polymerisation degree of poly-lactic acid is 600-
1000。
2. lactic acid composite material according to claim 1, it is characterised in that butyl titanate and phosphorus in the modifying agent
The ratio between amount of material of sour trimethyl is 1 ︰ 1.
3. lactic acid composite material according to claim 1, it is characterised in that the polyethyleneglycol diacrylate gathers
Right is 200-230.
4. lactic acid composite material according to claim 3, it is characterised in that the polyethyleneglycol diacrylate gathers
Right is 210.
5. lactic acid composite material according to claim 1, it is characterised in that the polymerisation degree of poly-lactic acid is 700-900.
6. lactic acid composite material according to claim 5, it is characterised in that the polymerisation degree of poly-lactic acid is 800.
7. a kind of preparation method of the lactic acid composite material as described in claim 1-6, it is characterised in that comprise the following steps：
（1）Nano-aluminum hydroxide is handled with coupling agent；
（2）Nano-aluminum hydroxide Jing Guo coupling agent treatment is subjected to cladding processing with modifying agent；
（3）By the nano-aluminum hydroxide after cladding and polylactic acid processing for composite in the electric field after mixing, mixed
Material；（4）Mixture and polyethyleneglycol diacrylate, crosslinking agent, zinc stearate, calcium succinate are being answered after mixing
Conjunction is handled, and obtains high temperature resistant lactic acid composite material.
8. preparation method according to claim 7, it is characterised in that step（3）Middle electric field strength is 1.5-2.5kv/m.
9. preparation method according to claim 8, it is characterised in that step（3）Middle electric field strength is 1.8-2.0kv/m.
10. preparation method according to claim 7, it is characterised in that step（3）Middle electric field is put down for direction of an electric field is constant
Row electric field.
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| CN201711244371.4A CN107903596A (en) | 2017-11-30 | 2017-11-30 | A kind of high temperature resistant lactic acid composite material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110408039A (en) * | 2019-08-19 | 2019-11-05 | 陕西理工大学 | A kind of preparation method of the miniature product of high-intensity and high-tenacity polylactic acid |
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2017
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110408039A (en) * | 2019-08-19 | 2019-11-05 | 陕西理工大学 | A kind of preparation method of the miniature product of high-intensity and high-tenacity polylactic acid |
| CN110408039B (en) * | 2019-08-19 | 2021-12-03 | 陕西理工大学 | Preparation method of high-strength high-toughness polylactic acid miniature product |
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