CN110105732A - A kind of powdered rice hulls/polylactic acid biodegradable composite and preparation method thereof - Google Patents
A kind of powdered rice hulls/polylactic acid biodegradable composite and preparation method thereof Download PDFInfo
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- CN110105732A CN110105732A CN201910416534.5A CN201910416534A CN110105732A CN 110105732 A CN110105732 A CN 110105732A CN 201910416534 A CN201910416534 A CN 201910416534A CN 110105732 A CN110105732 A CN 110105732A
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- polylactic acid
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- rice hulls
- powdered rice
- biodegradable composite
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- 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
- C08L2201/06—Biodegradable
-
- 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
-
- 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
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
Abstract
The invention discloses a kind of powdered rice hulls/polylactic acid biodegradable composites and preparation method thereof.The invention material is made of the raw material of following parts by weight: 60 parts of polylactic acid, 40 parts of powdered rice hulls, 4-6 parts of maleic anhydride grafted polylactic acid, 14 parts of nanometer calcium carbonate, 1 part of nano-titanium dioxide, 2 parts of lubricant.Specific production method is the following steps are included: by rice husk grinds, drying for standby after being handled with sodium hydroxide solution；The raw materials such as powdered rice hulls, polylactic acid, maleic anhydride grafted polylactic acid after drying are injected into Twin screw extruder, powdered rice hulls/polylactic acid biodegradable composite is obtained by Screw Extrusion.This method is simple and raw material is easy to get, and easily realizes large-scale production.The powdered rice hulls obtained through preparation method provided by the invention/polylactic acid biodegradable composite, except can be voluntarily degraded into outside organic fertilizer after terminating use, also possess good toughness with the characteristics such as hard, high density, nontoxic, environmentally friendly, it is more resistance to fall, improve its service life.
Description
Technical field:
The present invention relates to chemical material fields, and in particular to be a kind of powdered rice hulls and the biodegradable composite wood of polylactic acid
Material and its production method.
Background technique:
In recent years, degradable biological based composites are paid more and more attention as novel ecological environment-friendly materials.Its compound work
Skill mitigates environmental pressure and raising productivity effect etc. all to making full use of China's agriculture and forestry organic waste material resource, improving resource utilization
Want significance.Degradable biological based composites abandoned polyethylene (PE), polypropylene (PP) and polyvinyl chloride (PVC) etc. according to
The non-renewable plastics for relying fossil resources, have selected the fully biodegradables plastics such as polylactic acid (PLA), avoid plastics use
Afterwards because of the secondary pollution caused to environment that can not degrade, answered in multiple fields such as automobile, interior decoration, urban landscapes
With.Therefore, the attention rate of polylactic acid-base composite material increasingly improves in academia and business circles.
For PLA with corn constantly regenerating on the earth etc. for raw material, raw material sources are abundant.Meanwhile PLA has and conventional plastic
Quite even more excellent physical and chemical performance can meet the needs of people's life.But PLA is expensive, and it is straight to limit it
Tap into row processing and utilization.Rice husk is the renewable resource that a kind of source is wide, at low cost as paddy processing residue.By rice husk
Fiber and polylactic acid are combined RH/PLA composite material, can make full use of the natural resources, improve the comprehensive performance of polylactic acid,
Reduce production cost.
However, PLA is the linear poly- macromolecule of nonpolarity, and the lignin and cellulose in powdered rice hulls have it is highly polar, two
The interface compatibility of person is poor.PLA is hard and crisp hydrophobic material, and the crystallinity of PLA product is low, is not easy to form a film, generally in non-
Crystalline state causes the heat resistance of PLA material and mechanical property poor.In addition, powdered rice hulls surface have one layer with SiO2For main component
Cover film, SiO2PLA can be interfered to influence fiber and the interface cohesion of PLA to the infiltration of fiber, it is multiple that this all limits RH/PLA
The application of condensation material.Therefore, the interface compatibility improved between PLA and powdered rice hulls is the excellent wood and plastic composite of processability
Expect, expand the key of its application range.
Summary of the invention:
The present invention is prepared for a kind of biodegradable powdered rice hulls/lactic acid composite material, and the product of material preparation is available
In the recyclable indoor and outdoor furniture recycled, floor, packaging etc., the composite material of powdered rice hulls and PLA material being mixed is comprehensive
It has closed the plurality of advantages of both sides, and has improved powdered rice hulls and PLA compatibility using maleic anhydride-PLA, while nanometer calcium carbonate and having received
Rice titanium dioxide improves the mechanical property of composite material.The composite material not only has preferable mechanical property, good heat-resisting
Property, and the recycling of material may be implemented, it is a kind of novel green material.
The technical solution adopted in the present invention is as follows:
(1) rice husk is washed 1~2 time with clear water, removes solid impurity and dust, use Universalpulverizer pearling flour after air-drying
It is broken to 80-200 mesh.
(2) NaOH solution that 100mL 5% is added with the solid-to-liquid ratio of 1:5 for rice husk, immersion treatment 48h under room temperature are weighed.Leaching
Sealed beaker mouth when bubble, instills in a small amount of acetum and aqueous slkali after 48 hours, is rinsed with a large amount of clear water to neutrality.
(3) by the powdered rice hulls handled well temperature be 103 ± 2 DEG C at be dried for 24 hours, make its moisture content 2% or so.
(4) by polylactic acid temperature be 50 DEG C at 12h is dried.
(5) control polylactic acid is 60 parts, and powdered rice hulls are 40 parts, and maleic anhydride grafted polylactic acid is 5 parts, and nanometer calcium carbonate is
14 parts, nano-titanium dioxide is 1 part, and lubricant is 2 parts.By treated, mixing is added in powdered rice hulls, polylactic acid and selected auxiliary agent
Machine stirs 5-10 minutes at normal temperature.
(6) mixed material in (5) is added in double screw extruder, is squeezed out by melt blending, twin-screw squeezes
The temperature setting of machine is 180 DEG C out.Extruded material cooling obtains yellow bar.
The beneficial effects of the present invention are:
The present invention makes full use of rice husk as raw material, and source is wide, at low cost, improves its by-product value.And gather
For lactic acid with corn constantly regenerating on the earth etc. for raw material, raw material sources are abundant, have good physical and mechanical property.It combines
The advantage of powdered rice hulls and polylactic acid, product of the invention have good water resistance, also have hard, high density, smooth, nothing
The characteristics such as malicious, environmentally friendly, degradable can replace the classes such as plastics, wood, bamboo in multiple fields such as automobile, interior decoration, urban landscapes
The wasting of resources, and can voluntarily be degraded to organic fertilizer in nature after terminating use, mitigate the pressure to environment.
The present invention improves the interface compatibility between powdered rice hulls and polylactic acid with maleic anhydride grafted polylactic acid, so that
Manufactured material has good toughness, and more resistance to fall, improving powdered rice hulls/polylactic acid biodegradable composite makes
With the service life, have a vast market foreground.
Specific example:
For convenient for further illustrating the present invention, below with reference to specific example, the present invention will be described:
Primary raw material rice husk, ten thousand Mu Di organic fertilizer Co., Ltds, mesh number are 80-200 mesh；Polylactic acid, injection grade, Dongguan City
Contain nation's engineering plastic raw material Co., Ltd；Maleic anhydride-PLA, Dongguan City contain nation's engineering plastic raw material Co., Ltd；Rutile-type
Nano-titanium dioxide, purity 92.5%, Shanghai Kai Yuan Chemical Industry Science Co., Ltd；Nanometer calcium carbonate, purity 96%, Jiangxi Province are safe
Magnificent calcium carbonate Co., Ltd.
In one preferred embodiment, powdered rice hulls of the 200g80-200 mesh through alkali process are weighed according to mass ratio, are put into 103 DEG C
It is 24 hours dry in drying machine, so that its water content is down to 3%.Powdered rice hulls and 300gPLA after weighing the drying of 200g80 mesh, 10g
Lubricant, 5g nano TiO 2,70g nm level CaCO_3,20g maleic anhydride grafted polylactic acid are sufficiently mixed.By uniformly mixed material
It is added in twin-screw extruder barrel and carries out extruding pelletization, twin-screw extruder barrel temperature is 185 DEG C.By basic material wind
It is dry and cold but to use Material disintegrator particle afterwards, obtain granular samples.Pressing plate, heat pressing process such as table 1 are carried out to granular samples with hot press
It is shown.It after hot pressing, is cooled down using cold press, cold-press process 4Mpa, 5min.Biodegradable can be obtained in taking-up
Powdered rice hulls/Polylactic acid composite board.
1 heat pressing process table of table
In one preferred embodiment, powdered rice hulls of the 200g80-200 mesh through alkali process are weighed according to mass ratio, are put into 103 DEG C
It is 24 hours dry in drying machine, so that its water content is down to 3%.Powdered rice hulls and 300gPLA after weighing the drying of 200g80 mesh, 10g
Lubricant, 5g nano TiO 2,70g nm level CaCO_3,22.5g maleic anhydride grafted polylactic acid are sufficiently mixed.By uniformly mixed object
Material, which is added in twin-screw extruder barrel, carries out extruding pelletization, and twin-screw extruder barrel temperature is 185 DEG C.By basic material
Material disintegrator particle is used after air-drying cooling, obtains granular samples.Pressing plate, heat pressing process such as table are carried out to granular samples with hot press
Shown in 1.It after hot pressing, is cooled down using cold press, cold-press process 4Mpa, 5min.Biology, which can be obtained, in taking-up to drop
Solve powdered rice hulls/Polylactic acid composite board.
In one preferred embodiment, powdered rice hulls of the 200g80-200 mesh through alkali process are weighed according to mass ratio, are put into 103 DEG C
It is 24 hours dry in drying machine, so that its water content is down to 3%.Powdered rice hulls and 300gPLA after weighing the drying of 200g80 mesh, 10g
Lubricant, 5g nano TiO 2,70g nm level CaCO_3,25g maleic anhydride grafted polylactic acid are sufficiently mixed.By uniformly mixed material
It is added in twin-screw extruder barrel and carries out extruding pelletization, twin-screw extruder barrel temperature is 185 DEG C.By basic material wind
It is dry and cold but to use Material disintegrator particle afterwards, obtain granular samples.Pressing plate, heat pressing process such as table 1 are carried out to granular samples with hot press
It is shown.It after hot pressing, is cooled down using cold press, cold-press process 4Mpa, 5min.Biodegradable can be obtained in taking-up
Powdered rice hulls/Polylactic acid composite board.
In one preferred embodiment, powdered rice hulls of the 200g80-200 mesh through alkali process are weighed according to mass ratio, are put into 103 DEG C
It is 24 hours dry in drying machine, so that its water content is down to 3%.Powdered rice hulls and 300gPLA after weighing the drying of 200g80 mesh, 10g
Lubricant, 5g nano TiO 2,70g nm level CaCO_3,27.5g maleic anhydride grafted polylactic acid are sufficiently mixed.By uniformly mixed object
Material, which is added in twin-screw extruder barrel, carries out extruding pelletization, and twin-screw extruder barrel temperature is 185 DEG C.By basic material
Material disintegrator particle is used after air-drying cooling, obtains granular samples.Pressing plate, heat pressing process such as table are carried out to granular samples with hot press
Shown in 1.It after hot pressing, is cooled down using cold press, cold-press process 4Mpa, 5min.Biology, which can be obtained, in taking-up to drop
Solve powdered rice hulls/Polylactic acid composite board.
In one preferred embodiment, powdered rice hulls of the 200g80-200 mesh through alkali process are weighed according to mass ratio, are put into 103 DEG C
It is 24 hours dry in drying machine, so that its water content is down to 3%.Powdered rice hulls and 300gPLA after weighing the drying of 200g80 mesh, 10g
Lubricant, 5g nano TiO 2,70g nm level CaCO_3,30g maleic anhydride grafted polylactic acid are sufficiently mixed.By uniformly mixed material
It is added in twin-screw extruder barrel and carries out extruding pelletization, 185 DEG C of twin-screw extruder barrel temperature.Basic material is air-dried
Material disintegrator particle is used after cooling, obtains granular samples.Pressing plate, heat pressing process such as 1 institute of table are carried out to granular samples with hot press
Show.It after hot pressing, is cooled down using cold press, cold-press process 4Mpa, 5min.Biodegradable rice can be obtained in taking-up
Shell powder/Polylactic acid composite board.
The composite material and plate produce to above method carry out water imbibition and contact angle test:
Experiment one, water imbibition test:
Sample is prepared by GB/T 1462-2005；The batten prepared is placed in thermostatic water bath (water temperature is set as 23 DEG C),
After batten impregnate for 24 hours afterwards take out, dry, survey the variation of the quality of its immersion front and back, calculate the water absorption rate of sample.Experiment two connects
Feeler test:
It takes 1 droplets of fluid to be measured on specimen surface in the sampling control system of contact angle instrument, is contacted using CA-W
Angle measuring instrument is obtained from initially to balance different time sections drop in the form of specimen surface, and then directly measurement drop is in test specimen
The variation of surface contact angle.Test value is averaged after measuring 5 times.
Every group of scheme data measured table 2 is tested above:
Table 2
It should be understood that the above is only a preferred embodiment of the present invention, the scope of the patents of the invention cannot be therefore limited,
All the equivalent structure or equivalent process transformation made by using the contents of the present specification are applied directly or indirectly in other phases
The technical field of pass, is included within the scope of the present invention.
Claims (9)
1. a kind of powdered rice hulls and polylactic acid biodegradable composite, the raw material comprising following parts by weight: 60 parts of polylactic acid,
40 parts of powdered rice hulls, 4-6 parts of maleic anhydride grafted polylactic acid, 14 parts of nanometer calcium carbonate, 1 part of nano-titanium dioxide, 2 parts of lubricant.
2. powdered rice hulls and polylactic acid biodegradable composite according to claim 1, it is characterised in that: the polylactic acid
It is with one or more works in cornstarch, waxy corn starch, high waxy starch, tapioca, potato starch, amylopectin
For polylactic acid made of raw material.
3. powdered rice hulls and polylactic acid biodegradable composite according to claim 1, it is characterised in that: the polylactic acid
It is 60 parts, powdered rice hulls are 40 parts, and maleic anhydride grafted polylactic acid is 4 parts, and nanometer calcium carbonate is 14 parts, nano-titanium dioxide 1
Part, lubricant is 2 parts.
4. powdered rice hulls and polylactic acid biodegradable composite according to claim 1, it is characterised in that: the polylactic acid
It is 60 parts, powdered rice hulls are 40 parts, and maleic anhydride grafted polylactic acid is 4.5 parts, and nanometer calcium carbonate is 14 parts, and nano-titanium dioxide is
1 part, lubricant is 2 parts.
5. powdered rice hulls and polylactic acid biodegradable composite according to claim 1, it is characterised in that: the polylactic acid
It is 60 parts, powdered rice hulls are 40 parts, and maleic anhydride grafted polylactic acid is 5 parts, and nanometer calcium carbonate is 14 parts, nano-titanium dioxide 1
Part, lubricant is 2 parts.
6. powdered rice hulls and polylactic acid biodegradable composite according to claim 1, it is characterised in that: the polylactic acid
It is 60 parts, powdered rice hulls are 40 parts, and maleic anhydride grafted polylactic acid is 5.5 parts, and nanometer calcium carbonate is 14 parts, and nano-titanium dioxide is
1 part, lubricant is 2 parts.
7. powdered rice hulls and polylactic acid biodegradable composite according to claim 1, it is characterised in that: the polylactic acid
It is 60 parts, powdered rice hulls are 40 parts, and maleic anhydride grafted polylactic acid is 6 parts, and nanometer calcium carbonate is 14 parts, nano-titanium dioxide 1
Part, lubricant is 2 parts.
8. powdered rice hulls and polylactic acid biodegradable composite according to claim 1, it is characterised in that: the lubricant
Select polyethylene wax, zinc stearate, calcium stearate, two or more arbitrary proportion mixture in erucyl amide.
9. the preparation method of any one of -7 powdered rice hulls and polylactic acid biodegradable composite according to claim 1,
It is characterized in that: the following steps are included:
(1) rice husk is washed 1~2 time with clear water, removes solid impurity and dust, milled and be crushed to Universalpulverizer after air-drying
80 mesh；
(2) NaOH solution that 100mL5% is added with 1: 5 solid-to-liquid ratio for rice husk is weighed, immersion treatment 48h under room temperature, when immersion is close
Beaker mouth is sealed, is instilled after 48 hours in a small amount of acetum and aqueous slkali, is rinsed with a large amount of clear water to neutrality；
(3) by the powdered rice hulls handled well temperature be 103 ± 2 DEG C at be dried for 24 hours, make its moisture content 2% or so；
(4) by polylactic acid temperature be 50 DEG C at 12h is dried；
(5) mass ratio for controlling powdered rice hulls and polylactic acid is 4: 6, and 2% lubricant, 1% nano-TiO is added2, 14% nanometer
CaCO3, 5% maleic anhydride grafted polylactic acid, batch mixer is added in treated powdered rice hulls, polylactic acid and selected auxiliary agent,
It is stirred 5-10 minutes under room temperature；
(6) mixed material in (5) is added in double screw extruder, is squeezed out by melt blending, double screw extruder
Temperature setting be 180 DEG C, extruded material cooling powdered rice hulls/lactic acid composite material can be obtained.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909496A (en) * | 2020-08-03 | 2020-11-10 | 日彩复合塑料(深圳)有限公司 | Biodegradable plastic, production process and application thereof |
| CN113185815A (en) * | 2021-05-17 | 2021-07-30 | 中北大学 | Biodegradable material for improving PBSeT puncture resistance by using vinegar residue and preparation method thereof |
| CN114230957A (en) * | 2021-12-20 | 2022-03-25 | 长春工业大学 | High-toughness PLA/rice hull composite material and preparation method thereof |
| CN115627013A (en) * | 2022-09-08 | 2023-01-20 | 苏州博大永旺新材股份有限公司 | Rice hull powder biomass-based fully-degradable material and preparation method thereof |
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| CN109306193A (en) * | 2018-08-15 | 2019-02-05 | 厦门壳氏新材料科技有限公司 | Polylactic acid/rice hull cellulose composite material preparation method and its application |
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| CN104356618A (en) * | 2014-10-29 | 2015-02-18 | 衢州学院 | Biomass wood-plastic composite material for 3D (three-dimensional) printing and preparation method for biomass wood-plastic composite material |
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| CN113185815A (en) * | 2021-05-17 | 2021-07-30 | 中北大学 | Biodegradable material for improving PBSeT puncture resistance by using vinegar residue and preparation method thereof |
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| CN115627013A (en) * | 2022-09-08 | 2023-01-20 | 苏州博大永旺新材股份有限公司 | Rice hull powder biomass-based fully-degradable material and preparation method thereof |
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Application publication date: 20190809 |