CN105778446A - Preparation method of high strength and high buffer POSS hybrid polylactic acid foaming material - Google Patents
Preparation method of high strength and high buffer POSS hybrid polylactic acid foaming material Download PDFInfo
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- CN105778446A CN105778446A CN201410822967.8A CN201410822967A CN105778446A CN 105778446 A CN105778446 A CN 105778446A CN 201410822967 A CN201410822967 A CN 201410822967A CN 105778446 A CN105778446 A CN 105778446A
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Abstract
The invention relates to a preparation method of a high strength and high buffer POSS hybrid polylactic acid foaming material. The main ingredients of the foaming material comprises hydroxyl-terminated polylactic acid, thermoplastic elastomer polyurethane and polylactic acid, and the auxiliary ingredients include a compatilizer eight-armed maleamic acid based polyhedral oligomeric silsesquioxane, a polycondensation catalyst tetrabutyl titanate, and an antioxidant, a plasticizer, and an anti-ultraviolet agent. In the main ingredients, the mass ratio of hydroxyl-terminated polylactic acid is 45-65%, the mass ratio of the thermoplastic polyurethane elastomer is 25-45%, and the mass ratio of polylactic acid is 10-20%. In the auxiliary ingredients, the dosage of eight-armed maleamic acid based polyhedral oligomeric silsesquioxane accounts for 3.5-6% of the mass of the hydroxyl-terminated polylactic acid in the main ingredients, the dosage of the polycondensation catalyst tetrabutyl titanate accounts for 0.5-1.5% of the mass of the hydroxyl-terminated polylactic acid in the main ingredients, and the mass fraction of the antioxidant, the plasticizer, and the anti-ultraviolet agent accounts for 1-2% of the mass of the main ingredients. The foaming material adopts vapor extrusion foaming moulding, and the process is simple. The material has good strength and buffering performance, and is applicable to the packaging and industrial field with high strength and high buffering requirements.
Description
Technical field
The preparation method that the present invention relates to a kind of polylactic acid foam material, the preparation method particularly relating to a kind of expanded material with high intensity and high resiliency prepared by polycondensation reaction and POSS capacity increasing modifying.
Background technology
Although plastic material has more excellent performance and wide applicability; but it derives from oil product and cannot degrade; in today that crisis of resource and environmental pollution are serious all the more, find function admirable and reproducible substitution material then becomes the most important thing that current Material Field is studied.In buffering package field, polystyrol foam material (EPS) is because of its excellent forming ability, and coefficient of foaming and shock-absorbing capacity occupy most of share of amortizing packaging material.And polyethylene foam-material (EPE) is although its resiliency is general, but with low cost, it is also widely used for the packaging field that resiliency requirement is low.But the enhancing along with people's environmental consciousness, " white pollution " that brought by the Nondegradable of plastics has become as increasingly serious problem, because of the not perishable decomposition of foamed plastic such as polystyrene, harmful gas can be distributed during burning, cause environmental pollution and the CFCs (CFC8) for foamed polystyrene agent can destroy atmospheric ozone layer, harm biology, in Europe and Some Areas of USA, prohibite use EPS.Finding a kind of preparation technology simple, function admirable, the method for eco-friendly foamed plastic substitution material and foaming capable of being industrialized thereof then becomes a big problem of material science.At home and abroad, some researcheres have carried out exploratory development in this field, but realize and the aspect of performance of material still suffers from bigger defect in technique, as adopted part degradation material to prepare foamed plastic only, still suffer from the plastic grain crushed after degraded；Degradable expanded material expansion ratio is not enough, and in high foamability aftershaping ability, resiliency is poor, and difficult forming etc..And general degradable foam materials is due to the use of much starch, also resulting in hygroscopic, namely easily causing goes mouldy also is easily caused declining to a great extent of mechanical property.As one can be found to have an excellent mechanical performances, and there is the environmental-protecting foam material of excellent barrier and water proofing property, will have huge market potential undoubtedly.
In current degradation material, starch is furtherd investigate because of its cheap price and originating widely and is prepared for multiple life and industrial goods by modified with compound, such as starch basement membrane, starch dishware etc..But starch has the defect that it is natural, its poor mechanical property, unstable properties, the field that mechanical property requirements is low can only be applied to.And the appearance of polylactic acid changes this present situation.Polylactic acid (PLA) is aliphatic polyester, with lactic acid (2 hydroxy propanoic acid) for basic structural unit.PLA can pass through the natural materials such as fermented maize and prepare, it is possible to adopt lactic acid polycondensation to prepare.PLA and end product thereof can become CO in natural decomposition under composting conditions2And water, reduce solid waste discharge amount, be the biogenic material of a kind of environmental protection.It is better that PLA has the mechanical characteristic being similar to polystyrene, bending modulus and hot strength, but heat stability and shock resistance are poor, there is the defect that melt viscosity is low in the thermoforming course of processing, limit its application.After improving these shortcomings, the best substitute can being expected to as plastic material can be employed for industry, civil area by PLA.In the application of PLA, generally to substitute common plastics after adopting different material such as starch, polycaprolactone, EVA etc. toughness reinforcing.And polylactic acid is due to its characteristic, as can as expanded material also great prospect.In this type of research, CN1544525 discloses a kind of biodegradable polylactic acid foam plastic preparation method, namely in foaming process, add peroxide crosslinking polylactic acid, CN103642185A discloses a kind of Polylactic acid foam material and preparation method thereof, this patent adopts water as foaming agent, add a small amount of nucleator, realized the feature of environmental protection of material by Water blown.CN103242632A also discloses employing and adds cross-linking agent, nucleator to realize the technology of expanded polylactic acid.CN1600814 discloses a kind of polylactic acid, the copolymer of aliphatic-aromatic polyester, nucleator, interior lubrication prescription and the mixed foaming technique of outer lubrication prescription.But in general, for polylactic acid foam material, the how intensity of aggregate balancing material and toughness, and ensure the uniform of foaming process, remain the problem needing to solve.
Summary of the invention
The fragility that the invention aims to overcome polylactic acid foam material is big, and resiliency is poor, not the defect of easy-formation, it is provided that the preparation method of a kind of polylactic acid foam material with excellent in strength and damping characteristics.
It is an object of the invention to be achieved through the following technical solutions:
A kind of preparation method of high intensity high buffering POSS hydridization polylactic acid foam material.This expanded material is made up of major ingredient and adjuvant, major ingredient includes hydroxyl-terminated polylactic acid, thermoplastic polyurethanes, polylactic acid, adjuvant includes compatilizer eight arm maleic amide acidic group caged silsesquioxane, polycondensation catalyst butyl titanate and auxiliary agent antioxidant, plasticiser, ultraviolet (UV) resistant agent.In major ingredient, the mass ratio of hydroxyl-terminated polylactic acid is between 45-65%, and the mass ratio of Polyurethane Thermoplastic Elastomer is between 25-45%, and the mass ratio of polylactic acid is between 10-20%.In adjuvant, the consumption of eight arm maleic amide acidic group caged silsesquioxanes is the 3.5-6% of hydroxyl-terminated polylactic acid quality in major ingredient, the consumption of polycondensation catalyst butyl titanate is the 0.5-1.5% of hydroxyl-terminated polylactic acid quality in major ingredient, antioxidant, plasticizer, ultraviolet (UV) resistant agent mass fraction between the 1-2% of major ingredient quality.
Further, described hydroxyl-terminated polylactic acid is end group is-OH(hydroxyl) copolymer of poly lactic acid, can there is the monomer of hydroxyl carry out copolymerization end-blocking and obtain by introducing in polylactic acid building-up process.Such as poly-(lactic acid/Isosorbide-5-Nitrae butanediol) copolymer, poly-(lactic acid/diethanolamine) copolymer, poly-(lactic acid/6-caprolactone) copolymer.Its preparation can be prepared by temperature gradient method with double; two carboxylic monomer such as 1,4 butanediols, diethanolamine, 6-caprolactones by lactic acid.Existing commercial product can also be bought.
Further, the molecular weight of described hydroxyl-terminated polylactic acid is between 50000-300000g/mol, and in end group, hydroxyl ratio accounts between the 70-90% of total end group ratio.
Further, described Polyurethane Thermoplastic Elastomer is Polyether-type thermoplastic polyurethane elastomer.This type of Polyurethane Thermoplastic Elastomer has less glass transition temperature and better hydrolytic stability.
Further, described butyl titanate is polycondensation catalyst, can effectively polycondensation reaction between catalysis hydroxyl.In body series, catalyst can effectively polycondensation reaction between terminal hydroxy group between catalysis hydroxyl-terminated polylactic acid and in hydroxyl-terminated polylactic acid and eight arm maleic amide acidic group caged silsesquioxanes.Thus forming attachment structure so that POSS and polylactic acid stable bond, and thermoplastic shape polyurethane elastomer is wrapped up wherein uniformly.
Further, compatilizer eight arm maleic amide acidic group caged silsesquioxane involved in the present invention is the derivant of caged silsesquioxane (POSS).Caged silsesquioxane is a kind of silica structure with octahedra cage structure, and it exists 8 group R that can be modified on the corner of cage structure.When R is hydrophilic molecules chain, because molecular structure and the hydrophilic-hydrophobic structure of its nanoscale are employed for the compatible modified of both sexes blend.R in the POSS adopted in the present invention is maleic amide acidic group, and its molecular structure is as follows:
Wherein the caged silicon-oxide structure of POSS has hydrophobicity, can be combined with the oleophylic segment in polylactic acid and Polyurethane Thermoplastic Elastomer, and the maleamic acid group of end group has good hydrophilic, can be combined with the hydrophilic segment in polylactic acid and thermoplastic polyurethane molecule.Be conducive to the raising of the compatibility.The more important thing is, wherein the hydroxyl of maleamic acid group end with the end group generation polycondensation reaction of hydroxyl-terminated polylactic acid, can be connected with System forming, so that POSS compatilizer better plays the effect improving the compatibility closely.
Further, the abscess of described high intensity high buffering POSS hydridization polylactic acid foam material is hole-closing structure, and pore size is between 20-200 micron.
Further, described polylactic acid is poly (l-lactic acid), gathers D-ALPHA-Hydroxypropionic acid or poly-L, poly-D-ALPHA-Hydroxypropionic acid compositions, and the molecular weight of this polylactic acid is 80000g/mol-600000g/mol.
Further, described antioxidant is antioxidant 264, one or more in BHT, 168,1010.
Further, described plasticiser is aliphatic dibasic acid ester or Phthalates plasticiser.
Further, described ultraviolet (UV) resistant agent is the one or more combination in UV531, UV-2908, UV477.
Further, the preparation method of a kind of high intensity high buffering POSS hydridization polylactic acid foam material is as follows:
(1): drying of material: hydroxyl-terminated polylactic acid, polylactic acid, Polyurethane Thermoplastic Elastomer, eight arm maleic amide acidic group caged silsesquioxanes, butyl titanate being dried 6-8 hour under 60 degree in vacuum drying oven, pressure is lower than 0.01MPa, standby；
(2) extrusion foaming:
(I) by hydroxyl-terminated polylactic acid, thermoplastic shape elastomer polyurethane, eight arm maleic amide acidic group caged silsesquioxanes, butyl titanate in proportion in blended 5-8 minute of 50 degree of lower high speeds of high speed blender, rear vacuum extruding pelletize in extruder is put into.Extrusion temperature is between 170-180 degree, and vacuum, lower than 0.01MPa, finds time as 3-4 minute.Obtain masterbatch A；
(II) by masterbatch A, polylactic acid, other auxiliary agents in blended 5-8 minute of 50 degree of lower high speeds of high speed blender, in rear input extruder, extrusion temperature is between 170-190 degree, extrusion passes into water vapour, steam temperature is between 120-140 degree, and Stress control is between 1-1.5MPa, and the extrusion time of staying is 2-3 minute, decompression rate is between 20-50MPa/s, and extrusion obtains expanded material.
Further, adopting the extrusion being added without polylactic acid and auxiliary agent that two-step method extrusion is because the first step to be conducive to reaction and elastomer effective dispersion wherein of hydroxyl-terminated polylactic acid and POSS compatilizer, second step adds polylactic acid and various auxiliary agent is then conducive to auxiliary agent dispersion wherein.In second step extrusion, being added with of polylactic acid is beneficial to processability, and ensures the uniformity of foaming.
The beneficial effects of the present invention is, by the polycondensation reaction of hydroxyl-terminated polylactic acid and POSS terminal hydroxy group by dispersed for POSS and be connected to system, uniformly wrap up thermoplastic elastomer (TPE) simultaneously.This key connect be conducive to foam time material dimensionally stable, meanwhile, the compatibility being greatly improved in system between each component so that elastomer can be dispersed in polylactic acid, and in foaming body more effective raising toughness of material.In system, polylactic acid provides intensity, Polyurethane Thermoplastic Elastomer to provide toughness.The expressing technique of two-step method, advantageously ensures that the dispersion in system of the first polycondensation walked and various auxiliary agent and foaming, passes through Stress control, it may be achieved effective control of cell size.
Specific embodiment 1
Weigh 80.4g hydroxyl-terminated polylactic acid, the moulding elastomer polyurethane of 43.9g, 21.9g polylactic acid, 4g eight arm maleic amide acidic group caged silsesquioxane, 0.8g butyl titanate, 1.75 antioxidant BHTs, 2g plasticiser DOP and 2.3g ultraviolet (UV) resistant agent UV531.
Being dried 7 hours under 60 degree in vacuum drying oven by each raw material of above mass ratio, pressure is lower than 0.01MPa, standby.
By hydroxyl-terminated polylactic acid, thermoplastic shape elastomer polyurethane, eight arm maleic amide acidic group caged silsesquioxanes, butyl titanate in proportion in blended 6 minutes of 50 degree of lower high speeds of high speed blender, rear put into vacuum extruding pelletize in extruder.Extrusion temperature is between 170-180 degree, and wherein 1 section of temperature of extrusion is set as 170 degree, and 2 sections are set to 175 degree, and 3 sections are set to 175 degree, and 4 sections are set to 180 degree, and 5 sections are set to 175 degree, and vacuum, lower than 0.01MPa, finds time as 3-4 minute.Obtain masterbatch A.
By masterbatch A, polylactic acid, other auxiliary agents in blended 5-8 minute of 50 degree of lower high speeds of high speed blender, rear putting in extruder, extrusion temperature is between 170-190 degree, wherein 1 section of temperature of extrusion is set as 170 degree, and 2 sections are set to 175 degree, and 3 sections are set to 180 degree, four sections are set to 190 degree, 5 sections are set to 185 degree, pass into water vapour in extrusion 2 sections, and steam temperature is 130 degree, Stress control is between 1-1.5MPa, the extrusion time of staying is 2-3 minute, and decompression rate is 45MPa/s, and extrusion obtains expanded material.
Described polylactic acid is poly (l-lactic acid), and the weight average molecular weight of this polylactic acid is 200000g/mol-600000g/mol.
The molecular weight of described hydroxyl-terminated polylactic acid is between 100000-200000g/mol, and in end group, hydroxyl ratio accounts for the 85% of total end group ratio.
Specific performance is table 1 such as:
Specific embodiment 2
Weigh 100.2g hydroxyl-terminated polylactic acid, the moulding elastomer polyurethane of 64.1g, 36g polylactic acid, 4.5g eight arm maleic amide acidic group caged silsesquioxane, 1.2g butyl titanate, 3.2 antioxidant BHTs, 3g plasticiser DOP and 2.8g ultraviolet (UV) resistant agent UV531.
Being dried 7 hours under 60 degree in vacuum drying oven by each raw material of above mass ratio, pressure is lower than 0.01MPa, standby.
By hydroxyl-terminated polylactic acid, thermoplastic shape elastomer polyurethane, eight arm maleic amide acidic group caged silsesquioxanes, butyl titanate in proportion in blended 6 minutes of 50 degree of lower high speeds of high speed blender, rear put into vacuum extruding pelletize in extruder.Extrusion temperature is between 170-180 degree, and wherein 1 section of temperature of extrusion is set as 170 degree, and 2 sections are set to 175 degree, and 3 sections are set to 175 degree, and four sections are set to 180 degree, and 5 sections are set to 175 degree, and vacuum, lower than 0.01MPa, finds time as 3-4 minute.Obtain masterbatch A.
By masterbatch A, polylactic acid, other auxiliary agents in blended 5-8 minute of 50 degree of lower high speeds of high speed blender, rear putting in extruder, extrusion temperature is between 170-190 degree, wherein 1 section of temperature of extrusion is set as 170 degree, and 2 sections are set to 175 degree, and 3 sections are set to 180 degree, four sections are set to 190 degree, 5 sections are set to 185 degree, pass into water vapour in extrusion 2 sections, and steam temperature is 130 degree, Stress control is between 1-1.5MPa, the extrusion time of staying is 2-3 minute, and decompression rate is 40MPa/s, and extrusion obtains expanded material.
Described polylactic acid is poly (l-lactic acid), and the molecular weight of this polylactic acid is 200000g/mol-600000g/mol.
The molecular weight of described hydroxyl-terminated polylactic acid is between 100000-200000g/mol, and in end group, hydroxyl ratio accounts for the 85% of total end group ratio.
Specific performance is table 1 such as:
Table 1
| Performance parameter | Reference standard | Embodiment 1 | Embodiment 2 |
| Cell diameter | GB/T6343-1995 | 40-100um | 50-150um |
| Compressive strength | GB/T6669-2001 | 4800KPa | 4500KPa |
| Compression set | GB/T6669-2001 | After 30 minutes/24 hours 3.3%/0.5% | After 30 minutes/24 hours 4%/0.3% |
| Hot strength | GB/T6344-1996 | 74.5MPa | 78.5MPa |
| Elongation at break | GB/T6344-1996 | ≥280% | ≥260% |
| Oxygen index (OI) | GB/T2406-1993 | 2.43 | 2.51 |
Claims (4)
- null1. the preparation method of a high intensity high buffering POSS hydridization polylactic acid foam material，This expanded material is made up of major ingredient and adjuvant，Major ingredient includes hydroxyl-terminated polylactic acid、Thermoplastic polyurethanes、Polylactic acid，Adjuvant includes compatilizer eight arm maleic amide acidic group caged silsesquioxane，Polycondensation catalyst butyl titanate、And auxiliary agent antioxidant、Plasticiser、Ultraviolet (UV) resistant agent，In major ingredient，The mass ratio of hydroxyl-terminated polylactic acid is between 45-65%，The mass ratio of Polyurethane Thermoplastic Elastomer is between 25-45%，The mass ratio of polylactic acid is between 10-20%，In adjuvant, the consumption of eight arm maleic amide acidic group caged silsesquioxanes is the 3.5-6% of hydroxyl-terminated polylactic acid quality in major ingredient，The consumption of polycondensation catalyst butyl titanate is the 0.5-1.5% of hydroxyl-terminated polylactic acid quality in major ingredient，Antioxidant、Plasticizer、The mass fraction of ultraviolet (UV) resistant agent is all between the 1-2% of major ingredient quality；Its processing method is:(1): drying of material: hydroxyl-terminated polylactic acid, polylactic acid, Polyurethane Thermoplastic Elastomer, eight arm maleic amide acidic group caged silsesquioxanes, butyl titanate being dried 6-8 hour under 60 degree in vacuum drying oven, pressure is lower than 0.01MPa, standby；(2) extrusion foaming:(I) by hydroxyl-terminated polylactic acid, thermoplastic shape elastomer polyurethane, eight arm maleic amide acidic group caged silsesquioxanes, butyl titanate in proportion in blended 5-8 minute of 50 degree of lower high speeds of high speed blender, evacuation extruding pelletization in rear input extruder, extrusion temperature is between 170-180 degree, vacuum is lower than 0.01MPa, find time as 3-4 minute, obtain masterbatch A；(II) by masterbatch A, polylactic acid, other auxiliary agents in blended 5-8 minute of 50 degree of lower high speeds of high speed blender, in rear input extruder, extrusion temperature is between 170-190 degree, extrusion passes into water vapour, steam temperature is between 120-140 degree, and Stress control is between 1-1.5MPa, and the extrusion time of staying is 2-3 minute, decompression rate is between 20-50MPa/s, and extrusion obtains expanded material.
- 2. a kind of high intensity high buffering POSS hydridization polylactic acid foam material as claimed in claim 1, it is characterized in that, described polylactic acid is poly (l-lactic acid), gathers D-ALPHA-Hydroxypropionic acid or poly-L, poly-D-ALPHA-Hydroxypropionic acid compositions, and the molecular weight of this polylactic acid is 80000g/mol-600000g/mol.
- 3. a kind of high intensity high buffering POSS hydridization polylactic acid foam material as claimed in claim 1, it is characterized in that, the molecular weight of described hydroxyl-terminated polylactic acid is between 50000-300000g/mol, and in end group, hydroxyl ratio accounts for total end group mol ratio between 70-90%.
- 4. a kind of high intensity high buffering POSS hydridization polylactic acid foam material according to claims 1, it is characterised in that described Polyurethane Thermoplastic Elastomer is Polyether-type thermoplastic polyurethane elastomer.
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Cited By (2)
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| CN110016213A (en) * | 2019-03-21 | 2019-07-16 | 北京工商大学 | A kind of polylactic acid foam material and preparation method thereof with micro-nano compound abscess |
| CN117209887A (en) * | 2023-09-06 | 2023-12-12 | 广东科净塑料制品有限公司 | High-toughness durable polypropylene material and preparation process thereof |
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| CN110016213A (en) * | 2019-03-21 | 2019-07-16 | 北京工商大学 | A kind of polylactic acid foam material and preparation method thereof with micro-nano compound abscess |
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Application publication date: 20160720 |