CN105694400B - A kind of polylactic acid bamboo powder composite modification material production method - Google Patents
A kind of polylactic acid bamboo powder composite modification material production method Download PDFInfo
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- CN105694400B CN105694400B CN201610083662.9A CN201610083662A CN105694400B CN 105694400 B CN105694400 B CN 105694400B CN 201610083662 A CN201610083662 A CN 201610083662A CN 105694400 B CN105694400 B CN 105694400B
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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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- 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
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention belongs to environment-friendly materials field, a kind of polylactic acid bamboo powder composite modification material production method is provided firstly, nucleating agent and coupling agent room temperature are uniformly mixed, mixture A is made；Then, after evenly mixing by particles of polylactic acid, toughener and mixture A, the bamboo powder for adding filling reinforcing agent and drying processing uniformly mixes；Finally, the mixture obtained to step 2 carries out granulation processing.The composite modified material that changes of the polylactic acid bamboo powder produced by the above method has preferable mechanical energy, maintains the biodegradability of poly-lactic acid material.
Description
Technical field
The present invention relates to environment-friendly materials fields to particularly relate to one kind more particularly, to Biodegradable material field
Polylactic acid bamboo powder composite modification material.
Background technique
Clout after bamboo processing can directly apply to macromolecule modified application by the way that the bamboo powder of certain mesh number is made,
Further obtain the utility value of bamboo powder.
Currently, belonging to the with the fastest developing speed of poly-lactic acid material in environment-friendly materials field, application range is from initial
Medical field expands to daily life field, especially disposable knife-fork-spoon, cup, film, office appliance, garden supplies etc.；
But due to the cost of polylactic acid compared with common petroleum base plastics no advantage, cause it to promote on a large scale and be restricted；Cause
This, people start to have carried out a large amount of research to the cost for how reducing polylactic acid, are mainly combined to by biomass material
The mode of lactic acid composite material is formed in polylactic acid matrix to reduce the cost of polylactic acid；The prior art is biology base mostly
Matter starch also has using the bio-matrixes raw material such as rice hull cellulose or bagasse.
Summary of the invention
Object of the present invention is to improve the use value of bamboo powder, while solving the high cost problem of poly-lactic acid material.
To achieve the above object, present invention firstly provides a kind of polylactic acid bamboo powder composite modification material, using bamboo powder with
The compound of poly-lactic acid material carries out high value utilization to bamboo powder, and reduces the cost of poly-lactic acid material；The polylactic acid bamboo
The powder compound modified material that changes has preferable mechanical energy, maintains the biodegradability of poly-lactic acid material.
The further present invention proposes that a kind of polylactic acid bamboo powder composite modification material production method, the polylactic acid bamboo powder are compound
Modified material is 50-90 parts of polylactic acid, 0.5-2 parts of nucleating agent, 5-20 parts of filling reinforcing agent, 5-30 parts by parts by weight
Bamboo powder, 0.5-2 parts of coupling agent, 1-5 parts of toughener are composed；It is characterized in that, this method comprises the following steps:
One, nucleating agent and coupling agent room temperature are uniformly mixed, mixture A is made；
Two, under room temperature, after evenly mixing by particles of polylactic acid, toughener and mixture A, add filling reinforcing agent and warp
The bamboo powder of drying and processing uniformly mixes；
Three, the mixture obtained to step 2 carries out granulation processing.
In above-mentioned technique, the nucleating agent is mixed with coupling agent by the way of room temperature quickly (>=2000r/min) stirring,
Mixing time is 5-10 minutes；
The mixing of particles of polylactic acid, toughener and mixture A is stirred by the way of room temperature low speed (≤500r/min) stirring
Mixing the time is 10-15 minutes；
In such a way that room temperature stirs at low speed, mixing time is 15-30 points for mixing after filling reinforcing agent and bamboo powder is added
Clock；
It is granulated and is carried out using dual-screw pelletizer, prilling temperature is 170-220 DEG C.
Preferably, nucleating agent and coupling agent mixing time are 5 minutes；Particles of polylactic acid, toughener and mixture A are mixed
Closing mixing time is 10 minutes, and mixing time is 15 minutes after filling reinforcing agent and bamboo powder is added；Prilling temperature is 175
Degree.
In the present invention, the polylactic acid can choose what Zhejiang sea just biomaterial or U.S. Natureworks produced
Polylactic acid pure material, such as Revode190,4032D etc.；Because the optical purity of polylactic acid crystallizes it and heat resistance plays decision
The effect of property, the heat resistance of the higher polylactic acid of optical purity after crystallisation will be lower than optical purity high, it is preferable that
The optical purity of the polylactic acid is 98% or more, and the optical purity of the more preferably described polylactic acid is 99.5% or more.
The nucleating agent is the inorganic material such as wollastonite, calcium sulfate crystal whiskers or silicon carbide；It is composite modified as polylactic acid
Nucleating agent, the silica of the present invention preferably ultra-fine 5000 mesh；It fills reinforcing agent and selects talcum powder, there are many performances, such as:
Improve inprocess shrinkage rate, finished surface hardness, surface anti-scratch performance, impact strength etc., meanwhile, talcum powder is as a kind of
Inorganic additive does not conflict with the biological degradability of polylactic acid；Moreover, the low cost of talcum powder can reduce to a certain extent it is poly-
The cost of lactic acid resin combination；However, the mesh number rank of talcum powder has a certain impact to the performance change of polylactic acid, mesh number
Higher or lower all unfavorable to modified performance, therefore, preferably, the mesh number of talcum powder is in 800-5000 mesh.
The bamboo powder needs to carry out drying and processing before composite modified；Preferably, the size of the bamboo powder is 40 mesh -400
Mesh；It is highly preferred that the size of the bamboo powder is 40-200 mesh, the bamboo powder advantage of lower cost of this mesh number range is obtained, while can
To be satisfied with the composite modified of poly-lactic acid material, and its it is composite modified after material property can satisfy industrial application.
The coupling agent can be organochromium complexes, silanes, titanate ester and aluminic acid compound, it is therefore preferable to silane
Class, such as KH-560.
The toughener can choose thermoplastic elastomer (TPE) (TPE), high molecular weight polyurethane (PU), biology base polyester etc.,
To keep the influence of the biological degradability and carrying capacity of environment of polylactic acid to consider that the present invention preferentially selects biology base kind polyester, specifically
Ground is the biology base polyester with flexible molecule chain, such as: polycaprolactone, poly butylene succinate, polybutyleneadipate
Ester, polyadipate/butylene terephthalate, polyethylene glycol succinate；The biology base polyester has biomass source
Speciality and biodegradable performance, there is good compatibility with polylactic acid, while the flexibility of polylactic acid can be improved；It is more excellent
Selection of land is polycaprolactone material as toughener.
The beneficial effects of the present invention are:
Above-mentioned polylactic acid bamboo powder composite modification material, is utilized bamboo powder and the compound of poly-lactic acid material carries out height to bamboo powder
Value utilizes, and reduces the cost of poly-lactic acid material, and it is composite modified after material there is preferable mechanical energy, while not changing
Become biodegradability possessed by poly-lactic acid material itself.
Specific embodiment
Polylactic acid selects the Revode190 of the positive biomaterial production in sea, and nucleating agent selects the silica of ultra-fine 5000 mesh,
It fills reinforcing agent and selects talcum powder, coupling agent selects KH-560, and toughener selects the polycaprolactone of biomass source, and bamboo powder is by certain
Bamboo product manufacturing enterprise provides, and mesh number is in two kinds of 40 mesh and 100 mesh.It is handled using following steps: 1, nucleating agent+coupling agent,
Using small-sized quick mixer (30L capacity) stirring at normal temperature 5 minutes, mixture A is made；2, particles of polylactic acid+toughener+mixing
Object A, after ten minutes using common low-speed mixer (200L capacity) stirring at normal temperature, add filling reinforcing agent (talcum powder) and
Bamboo powder, then stir at low speed 15 minutes；3, using double-screw extruding pelletizing machine to clicking blend compositions described in embodiment
It is granulated, prilling temperature is 170-220 DEG C.Mechanical property finally is carried out to polylactic acid bamboo powder composite modification material obtained
Test, is specifically shown in Table 1.
Embodiment 1: drying and processing is carried out to the bamboo powder of 40 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 5000 grams of polylactic acid, 100 grams of nucleating agent, 2000 grams of the filling reinforcing agent of 800 mesh, 3000 grams of the bamboo powder of 40 mesh, coupling agent
200 grams, 300 grams of toughener.
Embodiment 2: drying and processing is carried out to the bamboo powder of 40 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 6000 grams of polylactic acid, 100 grams of nucleating agent, 1500 grams of the filling reinforcing agent of 800 mesh, 2500 grams of the bamboo powder of 40 mesh, coupling agent
200 grams, 100 grams of toughener.
Embodiment 3: drying and processing is carried out to the bamboo powder of 40 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 7000 grams of polylactic acid, 100 grams of nucleating agent, 1000 grams of the filling reinforcing agent of 800 mesh, 2000 grams of the bamboo powder of 40 mesh, coupling agent
200 grams, 100 grams of toughener.
Embodiment 4: drying and processing is carried out to the bamboo powder of 40 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 8000 grams of polylactic acid, 100 grams of nucleating agent, 500 grams of the filling reinforcing agent of 1250 mesh, 1500 grams of the bamboo powder of 40 mesh, coupling agent
200 grams, 100 grams of toughener.
Embodiment 5: drying and processing is carried out to the bamboo powder of 40 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 8000 grams of polylactic acid, 100 grams of nucleating agent, 500 grams of the filling reinforcing agent of 1250 mesh, 1500 grams of the bamboo powder of 40 mesh, coupling agent
100 grams, 100 grams of toughener.
Embodiment 6: drying and processing is carried out to the bamboo powder of 40 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 8000 grams of polylactic acid, 100 grams of nucleating agent, 5 00 grams of the filling reinforcing agent of 1250 mesh, 2000 grams of the bamboo powder of 40 mesh, coupling agent
200 grams, 100 grams of toughener.
Embodiment 7: drying and processing is carried out to the bamboo powder of 40 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 8000 grams of polylactic acid, 200 grams of nucleating agent, 500 grams of the filling reinforcing agent of 1250 mesh, 2000 grams of the bamboo powder of 40 mesh, coupling agent
200 grams, 100 grams of toughener.
Embodiment 8: drying and processing is carried out to the bamboo powder of 40 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 8000 grams of polylactic acid, 100 grams of nucleating agent, 500 grams of the filling reinforcing agent of 1250 mesh, 2000 grams of the bamboo powder of 40 mesh, coupling agent
200 grams, 200 grams of toughener.
Embodiment 9: drying and processing is carried out to the bamboo powder of 40 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 8000 grams of polylactic acid, 100 grams of nucleating agent, 500 grams of the filling reinforcing agent of 1250 mesh, 1500 grams of the bamboo powder of 40 mesh, coupling agent
200 grams, 500 grams of toughener.
Embodiment 10: drying and processing is carried out to the bamboo powder of 100 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 8000 grams of polylactic acid, 100 grams of nucleating agent, 500 grams of the filling reinforcing agent of 1250 mesh, 2000 grams of the bamboo powder of 100 mesh, coupling agent
200 grams, 500 grams of toughener.
Embodiment 11: crushing is carried out to the bamboo powder of 40 mesh using pulverizer before the modified granulation of twin-screw and obtains 200 purposes
Bamboo powder, and drying and processing is carried out to the bamboo powder；8000 grams of polylactic acid, 100 grams of nucleating agent, the filling reinforcing agent 500 of 1250 mesh
Gram, 2000 grams of the bamboo powder of 200 mesh, 200 grams of coupling agent, 500 grams of toughener.
Embodiment 12: crushing is carried out to the bamboo powder of 100 mesh using ultrafine crusher before the modified granulation of twin-screw and obtains 400
Purpose bamboo powder, and drying and processing is carried out to the bamboo powder；8000 grams of polylactic acid, 100 grams of nucleating agent, the filling reinforcing agent of 1250 mesh
500 grams, 1500 grams of the bamboo powder of 400 mesh, 200 grams of coupling agent, 500 grams of toughener.
Embodiment 13: crushing is carried out to the bamboo powder of 100 mesh using ultrafine crusher before the modified granulation of twin-screw and obtains 400
Purpose bamboo powder, and drying and processing is carried out to the bamboo powder；8000 grams of polylactic acid, 100 grams of nucleating agent, the filling reinforcing agent of 1250 mesh
500 grams, 2000 grams of the bamboo powder of 400 mesh, 200 grams of coupling agent, 200 grams of toughener.
Embodiment 14: drying and processing is carried out to the bamboo powder of 100 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 7000 grams of polylactic acid, 100 grams of nucleating agent, 500 grams of the filling reinforcing agent of 1250 mesh, 2500 grams of the bamboo powder of 100 mesh, coupling agent
200 grams, 500 grams of toughener.
Embodiment 15: drying and processing is carried out to the bamboo powder of 100 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 7000 grams of polylactic acid, 100 grams of nucleating agent, 500 grams of the filling reinforcing agent of 3000 mesh, 3000 grams of the bamboo powder of 100 mesh, coupling agent
200 grams, 500 grams of toughener.
Embodiment 16: drying and processing is carried out to the bamboo powder of 100 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 7000 grams of polylactic acid, 100 grams of nucleating agent, 500 grams of the filling reinforcing agent of 5000 mesh, 2500 grams of the bamboo powder of 100 mesh, coupling agent
200 grams, 500 grams of toughener.
Embodiment 17: drying and processing is carried out to the bamboo powder of 40 mesh before twin-screw modified granulation；Mixture each group distribution ratio
Are as follows: 9500 grams of polylactic acid, 100 grams of nucleating agent, 500 grams of the filling reinforcing agent of 1250 mesh, 500 grams of the bamboo powder of 40 mesh, coupling agent 200
Gram, 100 grams of toughener.
Comparative example: Mechanics Performance Testing is carried out to the Revode190 polylactic acid pure material of sea positive biomaterial production, is as a result seen
Table 1.
Table 1: polylactic acid bamboo powder composite modification material and polylactic acid pure material mechanical property compare.
The result in conjunction with shown in above-mentioned table 1 it can be concluded that, the compositely proportional of bamboo powder and polylactic acid is higher, obtained polylactic acid bamboo
The mechanical property of powder compound modified material is poorer, is the principal element that material mechanical performance changes, but in the compound heavy of bamboo powder
The mechanical property that composite modification material is obtained when measuring part by 30 parts is almost suitable with the mechanical property of Revode190, therefore institute
The parts by weight for stating bamboo powder form preferably at 5-30 parts；Change in addition, the mesh number size of bamboo powder is compound to polylactic acid bamboo powder obtained
The mechanical property of property material is also relevant, and mesh number is bigger more advantageous to mechanical property.
Claims (4)
1. a kind of polylactic acid bamboo powder composite modification material production method, the polylactic acid bamboo powder composite modification material are by parts by weight
70-80 parts of polylactic acid, 1 part of 5000 mesh silica, 5 parts of 1250 mesh talcum powder, 20 parts of 400 mesh bamboo powders, 2 parts of silicon
Alkane coupling agent KH-560,2 parts of polycaprolactone are composed；It is characterized in that, this method comprises the following steps:
One, 5000 mesh silica and silane coupling agent KH-560 room temperature are uniformly mixed, mixture A is made；
Two, under room temperature, after evenly mixing by particles of polylactic acid, polycaprolactone and mixture A, add 1250 mesh talcum powder and warp
The bamboo powder of drying and processing uniformly mixes；
Three, the mixture obtained to step 2 carries out granulation processing.
2. polylactic acid bamboo powder composite modification material production method according to claim 1, which is characterized in that the titanium dioxide
In such a way that room temperature quickly stirs, mixing time is 5-10 minutes for silicon and silane coupling agent KH-560 mixing；Particles of polylactic acid,
In such a way that room temperature stirs at low speed, mixing time is 10-15 minutes for the mixing of polycaprolactone and mixture A；Talcum powder is added
With the mixing after bamboo powder in such a way that room temperature stirs at low speed, mixing time is 15-30 minutes；Granulation process is made using twin-screw
Grain machine carries out, and prilling temperature is 170-220 DEG C.
3. polylactic acid bamboo powder composite modification material production method according to claim 2, which is characterized in that silica and
Silane coupling agent KH-560 mixing time is 5 minutes；Particles of polylactic acid, polycaprolactone and mixture A mixing time
It is 10 minutes, mixing time is 15 minutes after talcum powder and bamboo powder is added；Prilling temperature is 175 degree.
4. polylactic acid bamboo powder composite modification material production method according to claim 1,2 or 3, which is characterized in that described
The polylactic acid pure material of polylactic acid selection optical purity > 98%.
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