CN106147176B - A kind of halogen-free flameproof biomass board - Google Patents
A kind of halogen-free flameproof biomass board Download PDFInfo
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- CN106147176B CN106147176B CN201610870210.5A CN201610870210A CN106147176B CN 106147176 B CN106147176 B CN 106147176B CN 201610870210 A CN201610870210 A CN 201610870210A CN 106147176 B CN106147176 B CN 106147176B
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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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
A kind of halogen-free flameproof biomass board, by PLA, plasticized starch, SBS, string, hydroxyl-terminated polylactic acid, nanometer sodium-based montmorillonite, 9, the oxide of 10 dihydro, 9 oxa-, 10 phospho hetero phenanthrene 10, melamine cyanurate, antioxidant, UV resistant agent composition, melting extrusion is into plate after the sheet material is blended by composition.Sheet material has good mechanical strength and toughness and an excellent combustion-supporting property, and materials environmental protection, processing are simple, available for high-grade ornamental flame-proof sheet material.
Description
Technical field
The present invention relates to a kind of preparation method of poly- biomass board, more particularly to it is a kind of have excellent in strength, toughness and
The preparation method of the biomass board of excellent flame retardancy.
Background technology
Although plastic material possesses more excellent performance and wide applicability, but it is from oil product and can not drop
Solution, in crisis of resource and environmental pollution serious today all the more, finds function admirable and reproducible alternative materials then turns into mesh
The most important thing of preceding Material Field research.Sheet material consumption now is huge, and is still plastic plate substantially, and exploitation has similar modeling
Expect the degradable sheet material of performance by with huge value.
In current degradation material, biomass source in naturally, and can realize degradable, be most potentiality to be exploited
Degradation material.Biological material category main at present is starch and PLA, and starch is because of its cheap price and widely
Furtherd investigate and be prepared for a variety of lives and industrial goods, such as starch basement membrane, starch dishware with compound by being modified in source
Deng.But starch has its natural defect, its poor mechanical property, performance is unstable, can only apply to low to mechanical property requirements
Field.And the appearance of PLA changes this present situation.PLA (PLA) is aliphatic polyester, with lactic acid (2- hydroxyls third
Acid) it is basic structural unit.PLA can be made by natural materials such as fermented maizes, can be also made using lactic acid polycondensation.PLA and
Its end product can turn into CO 2 and water in natural decomposition under composting conditionses, reduce solid waste discharge amount, be a kind of green
The biogenic material that colour circle is protected.PLA has the mechanical characteristic similar to polystyrene, and bending modulus and tensile strength are preferable,
It is used as preparing the major ingredient of sheet material, but its heat endurance and shock resistance are poor, exist in thermoforming process molten
The low defect of body viscosity, limits its application.After these shortcomings are improved, PLA can will be expected to as plastic material most
Good substitute can be employed for industry, civil area.In the toughening modifying research of PLA, PLA is combined with multiple material
To reach toughening effect, such as starch, polycaprolactone, polyethylene, above method for toughening has been widely studied, but due to blending material
The intensity of material itself is relatively low, and there is larger difference with PLA compatibility, therefore toughening effect is limited, and has a strong impact on PLA
The intensity of composite.In addition, also a variety of methods carry out toughening modifying to PLA.As CN101333333 is announced
A kind of toughened polylactic resin and preparation method thereof, the resin is by PLA base resin, toughener Styrene And Chloroalkyl Acrylates
Butyl ester-acrylic copolymer, antioxidant B215 compositions；CN101935390A discloses a kind of by by poly-succinic acid-butanediol
The terminal hydroxy group of ester triggers after lactide ring-opening polymerization, purified to obtain the polylactic acid toughening modifier, rear to add poly- breast
The preparation method of the composite of toughening modifying is carried out in acid.But all in all, PLA is the material of main body especially with PLA
Based on the mechanical property problem of biomass board be not fully solved yet.
In addition, for the use of sheet material, anti-flammability is also the ring that must take into consideration.For the biomass of environmental protection, use
The fire-retardant mode of environmental protection can just keep the environmental protection characteristic of material in itself.At present, the sheet material based on biomass is main with PLA material
Situation based on material, the research about flame-proof polylactic acid is of much attention.In addition to halogenated flame retardant not environmentally, Duo Zhongwu
Halogen, inorganic, nano-meter flame retardantses are employed in PLA.The BACN reported in recent years includes the phosphate of phosphorus system, phosphatization
Compound etc., the melamine and its esters of nitrogen system etc., but exclusive use effect is poor, and if cooperative flame retardant such as phosphorus-nitrogen synergistic
Better effects can be achieved.Nano-meter flame retardantses such as montmorillonite has a blocking effect, and its nanoscale can reduce composite density,
Mechanical strength is improved, but is easily reunited when measuring big；It is the preferable flame-retardant system of effect to expand flame retardant, and it includes acid source (such as
Ammonium phosphate salt, phosphate etc.), carbon source (such as pentaerythrite rich carbon polyhydroxy compound), source of the gas (amine or amides compound) 3
Part.Different system innovations can obtain being more applicable for PLA high-efficiency environment friendly Intumescent Retardant System.Such as in traditional APP/MA
Nano filling synergistic is added in flame-retardant system fire-retardant, petroleum base carbon forming agent is changed to the starch in green source into, part acid source is by giving birth to
Thing sill etc..In addition, novel nano-material such as POSS, it is fire-retardant that CNT is also used for PLA.But in general, at present
Flame-proof polylactic acid technology remains difficult to find balance between fire resistance, mechanical property and the feature of environmental protection, it is especially domestic with
The poly-lactic acid material field of excellent properties is still for space state.Exploitation is new to have excellent mechanical performance and anti-flammability
The biomass board of PLA material and preparation with excellent properties is extremely urgent.
The content of the invention
The invention aims to the defect that biomass board mechanical property is poor and anti-flammability is not good, there is provided one kind tool
There is the biomass board of excellent mechanical performance and fire resistance.
The purpose of the present invention is achieved through the following technical solutions：
A kind of halogen-free flameproof biomass board, by PLA, plasticized starch, SBS, string, hydroxyl-terminated polylactic acid, receives
Rice sodium-based montmorillonite, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, melamine cyanurate, antioxidant, anti-purple
Outside line agent
Composition.Wherein, the mass fraction of each component is：
PLA：100 parts
Plasticized starch：20-40 parts
SBS：10-20 parts
String：5-10 parts
Hydroxyl-terminated polylactic acid：5-10 parts
Nanometer receives base montmorillonite：3-6 parts
9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide：8-16 parts
Melamine cyanurate：4-8 parts
Antioxidant：2-4 parts
UV resistant agent：2-4 parts.
Further, heretofore described PLA is poly (l-lactic acid), poly- D-ALPHA-Hydroxypropionic acid or poly- L, D-ALPHA-Hydroxypropionic acid composition, is somebody's turn to do
The molecular weight of PLA most preferably 300000-500000g/mol, is again 150000-300000g/mol, again 80000-
150000g/mol。
Further, heretofore described plasticized starch is the cornstarch or tapioca that glycerine is plastified, for plastifying
Qualities of glycerin for starch 20%-35% between.
Further, string of the present invention be the bamboo fibre through physical or chemical treatment, it is wood-fibred, cotton fiber, thin
One kind in bacterium fiber, its diameter is between 200nm-2 μm, and draw ratio is between 20-500.Physical method can be machinery
Crush method, steam explosion method, chemical method can use acid activation method or alkali activation method.
Further, the molecular weight of heretofore described hydroxyl-terminated polylactic acid be 30000-100000g/mol between, end group
Middle hydroxyl ratio accounts for total end group mol ratio between 70-90%.
Further, nanometer sodium-based montmorillonite of the present invention is lamella particle, and its average wafer thickness is less than 25nm, can
Using commercially available nanometer sodium-based montmorillonite, it can be also modified using calcium-base montmorillonite, modification can use NaCl ethanol solutions, sodium carbonate, Jiao
It is sodium-based montmorillonite that sodium phosphate, sodium polyphosphate exchange calcium-base montmorillonite as modifying agent.
Further, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide of the present invention is organic phosphates jeterocyclic chemistry
Compound, with higher heat endurance, inoxidizability and excellent water resistance can use commercially available prod.
Further, antioxidant of the present invention is in antioxidant BHT, antioxidant 1010, antioxidant 1076, antioxidant 164
One or more of arbitrary proportions mixing.
Further, UV resistant agent of the present invention is in ultraviolet absorbent UV-531, UVP-327, UV-9, RMB
One or more of arbitrary proportion mixing.
Further, the processing technology of halogen-free flameproof biomass board of the present invention is：
(1) it is standby by all raw materials in vacuum drying 24 hours under 50 degree；
(2) by all raw materials in, in 5-10min is blended in high-speed mixer, rotating speed is 100-200rad/min under 60 degree；
(3) raw material input screw extruder melting extrusion after being blended, its melting extrusion temperature is 170-200 degree, screw rod
Rotating speed is 150-250rad/min, and the residence time is 1-2 minutes.
Further, the beneficial effect of this invention is that such as hydroxyl-terminated polylactic acid can based on the interaction between all components
Interacted with PLA, starch, hydroxyl-terminated polylactic acid can produce polycondensation in high temperature extrusion, promotion system compatibility
Improve, SBS plays toughening effect in system, string plays humidification, the miscellaneous -10- phospho hetero phenanthrenes of 9,10- dihydro-9-oxies -
10- oxides, melamine cyanurate are respectively as the source of the gas and acid source in chemically expansible based flame retardant, and starch is both as resistance
The carbon source in agent is fired, also serves as reducing cost component in sheet material system, nanometer receives base montmorillonite and plays blocking heat source wherein
With enhanced effect.
Embodiment
Illustrative embodiment of the invention described in detail below.But these implementations are only exemplary purpose, and
The invention is not restricted to this.
Embodiment 1
A kind of halogen-free flameproof biomass board, by PLA, plasticized starch, SBS, string, hydroxyl-terminated polylactic acid, receives
Rice sodium-based montmorillonite, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, melamine cyanurate, antioxidant, anti-purple
Outside line agent
Composition.Wherein, the mass fraction of each component is：
PLA：100 parts
Plasticized starch：32 parts
SBS：15 parts
String：8 parts
Hydroxyl-terminated polylactic acid：8 parts
Nanometer receives base montmorillonite：5 parts
9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide：12 parts
Melamine cyanurate：6 parts
Antioxidant：3 parts
UV resistant agent：3 parts.
Described PLA is poly (l-lactic acid), and the molecular weight of the PLA is 300000-500000g/mol.
Described plasticized starch is the tapioca that glycerine is plastified, and the qualities of glycerin for plasticizing is the 30% of starch.
The string be the bamboo fibre through physical treatment, its diameter between 400nm-1um, draw ratio between
Between 20-500.The physical method can dodge quick-fried method for mechanical crushing method coordinating with steam rapid heat cycle.
The molecular weight of described hydroxyl-terminated polylactic acid is between 50000-80000g/mol, hydroxyl ratio accounts for total end in end group
Base mol ratio is 85%.
The average wafer thickness of described nanometer sodium-based montmorillonite is less than 25nm, using commercially available nanometer sodium-based montmorillonite.
The 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is to use commercially available prod.
The antioxidant is antioxidant BHT.
The UV resistant agent is ultraviolet absorbent UV-531.
The processing technology of the halogen-free flameproof biomass board is：
1) it is standby by all raw materials in vacuum drying 24 hours under 50 degree；
2) by all raw materials in, in 6min is blended in high-speed mixer, rotating speed is 150rad/min under 60 degree；
3) raw material input screw extruder melting extrusion after being blended, its melting extrusion temperature is 170-200 degree, and screw rod turns
Speed is
180rad/min, the residence time is 1.5 minutes.
Embodiment 2
A kind of halogen-free flameproof biomass board, by PLA, plasticized starch, SBS, string, hydroxyl-terminated polylactic acid, receives
Rice sodium-based montmorillonite, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, melamine cyanurate, antioxidant, anti-purple
Outside line agent
Composition.Wherein, the mass fraction of each component is：
PLA：100 parts
Plasticized starch：26 parts
SBS：18 parts
String：6 parts
Hydroxyl-terminated polylactic acid：8.5 part
Nanometer receives base montmorillonite：4 parts
9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide：10 parts
Melamine cyanurate：5 parts
Antioxidant：3 parts
UV resistant agent：3 parts.
Described PLA is poly (l-lactic acid), the molecular weight most preferably 180000-400000g/mol of the PLA.
Described plasticized starch is the cornstarch that glycerine is plastified, and the qualities of glycerin for plasticizing is the 30% of starch.
The string is chemically treated pine cellulosic, and its diameter is between 400nm-1.5um, and draw ratio is situated between
Between 20-500.The chemical method is complex acid activation method after alkali lye activation.
The molecular weight of described hydroxyl-terminated polylactic acid is between 40000-60000g/mol, hydroxyl ratio accounts for total end in end group
Base mol ratio is 80%.
The average wafer thickness of described nanometer sodium-based montmorillonite is less than 25nm, using commercially available nanometer sodium-based montmorillonite.
The 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is to use commercially available prod.
The antioxidant is antioxidant 1010.
The UV resistant agent is ultra-violet absorber UVP-327.
The processing technology of the halogen-free flameproof biomass board is：
1) it is standby by all raw materials in vacuum drying 24 hours under 50 degree；
2) by all raw materials in, in 8min is blended in high-speed mixer, rotating speed is 180rad/min under 60 degree；
3) raw material input screw extruder melting extrusion after being blended, its melting extrusion temperature is 180-200 degree, and screw rod turns
Speed is 200rad/min, and the residence time is 1.5 minutes.
The specific performance data of embodiment 1,2 are as follows：
| Composite property | Embodiment 1 | Embodiment 2 |
| Fracture elongation (%) | 64.5±5 | 69.6±5 |
| Tensile strength (Mpa) | 42.4±2.41 | 46.4±2.58 |
| Impact strength (KJ/m2) | 28.4±2.28 | 26.1±2.43 |
| Oxygen index (OI) (%) | 30.2±1.2 | 28.4±1.2 |
| Vertical combustion grade | FV-0 | FV-0 |
Claims (5)
1. a kind of halogen-free flameproof biomass board, by PLA, plasticized starch, SBS, string, hydroxyl-terminated polylactic acid, nanometer
It is sodium-based montmorillonite, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, melamine cyanurate, antioxidant, anti-
Ultraviolet agent is constituted, wherein, the mass fraction of each component is：
PLA：100 parts
Plasticized starch：20-40 parts
SBS：10-20 parts
String：5-10 parts
Hydroxyl-terminated polylactic acid：5-10 parts
Nanometer sodium-based montmorillonite：3-6 parts
9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide：8-16 parts
Melamine cyanurate：4-8 parts
Antioxidant：2-4 parts
UV resistant agent：2-4 parts
It is further characterized in that：The molecular weight of the hydroxyl-terminated polylactic acid be 30000-100000g/mol between, hydroxyl ratio in end group
Example accounts for total end group mol ratio between 70-90%, and the PLA is poly (l-lactic acid), poly- D-ALPHA-Hydroxypropionic acid or poly- L, D-ALPHA-Hydroxypropionic acid combination
Thing, the molecular weight of the PLA is between 300000-500000g/mol.
2. a kind of halogen-free flameproof biomass board as claimed in claim 1, it is characterised in that：The plasticized starch is moulded for glycerine
The cornstarch or tapioca of change, the qualities of glycerin for plasticizing is between the 20%-35% of starch.
3. a kind of halogen-free flameproof biomass board as claimed in claim 1, it is characterised in that：The string is through physics
Or one kind in chemically treated bamboo fibre, wood-fibred, cotton fiber, bacterial fibers, its diameter is between 200nm-2 μm, length
Footpath ratio is between 20-500.
4. a kind of halogen-free flameproof biomass board as claimed in claim 1, it is characterised in that：The antioxidant is antioxidant
One or more of arbitrary proportions mixing in BHT, antioxidant 1010, antioxidant 1076, antioxidant 164.
5. a kind of halogen-free flameproof biomass board as claimed in claim 1, it is characterised in that：The UV resistant agent is ultraviolet
One or more of arbitrary proportions mixing in light absorbers UV-531, UVP-327, UV-9, RMB.
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| CN201610870210.5A CN106147176B (en) | 2016-10-05 | 2016-10-05 | A kind of halogen-free flameproof biomass board |
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| CN201610870210.5A CN106147176B (en) | 2016-10-05 | 2016-10-05 | A kind of halogen-free flameproof biomass board |
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| CN106147176A CN106147176A (en) | 2016-11-23 |
| CN106147176B true CN106147176B (en) | 2017-09-29 |
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| CN106752001A (en) * | 2016-12-21 | 2017-05-31 | 凤台县双利生物科技有限公司 | A kind of imvite modified waterproof flame-retardant type biomass board and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792602A (en) * | 2010-03-11 | 2010-08-04 | 四川大学 | Halogen-free expansible flame-retardant thermoplastic resin composition |
| CN101831156A (en) * | 2010-05-07 | 2010-09-15 | 四川大学 | Toughened halogen-free flame-retardant polylactic acid blending material |
| CN102746626A (en) * | 2012-07-02 | 2012-10-24 | 同济大学 | Natural fiber reinforced polylactic acid composite material having functionalized DOPO flame retardant and method for preparing same |
| CN105603564A (en) * | 2016-02-25 | 2016-05-25 | 东华大学 | Nitrogen-phosphorus synergetic copolymerization flame retardant polylactic acid fibers and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004061008A1 (en) * | 2002-12-27 | 2004-07-22 | Polyplastics Co., Ltd. | Flame-retardant resin composition |
| TWI503339B (en) * | 2009-05-19 | 2015-10-11 | Albemarle Corp | Dopo-derived flame retardant and epoxy resin composition |
| AT511395B1 (en) * | 2011-04-18 | 2013-12-15 | Sunpor Kunststoff Gmbh | FLAME-PROOF EXPANDABLE POLYMERISATE |
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2016
- 2016-10-05 CN CN201610870210.5A patent/CN106147176B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792602A (en) * | 2010-03-11 | 2010-08-04 | 四川大学 | Halogen-free expansible flame-retardant thermoplastic resin composition |
| CN101831156A (en) * | 2010-05-07 | 2010-09-15 | 四川大学 | Toughened halogen-free flame-retardant polylactic acid blending material |
| CN102746626A (en) * | 2012-07-02 | 2012-10-24 | 同济大学 | Natural fiber reinforced polylactic acid composite material having functionalized DOPO flame retardant and method for preparing same |
| CN105603564A (en) * | 2016-02-25 | 2016-05-25 | 东华大学 | Nitrogen-phosphorus synergetic copolymerization flame retardant polylactic acid fibers and preparation method thereof |
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