CN109943039A - A kind of methylation lignin/PBAT biodegradable plastics and preparation method thereof - Google Patents
A kind of methylation lignin/PBAT biodegradable plastics and preparation method thereof Download PDFInfo
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- CN109943039A CN109943039A CN201910117247.4A CN201910117247A CN109943039A CN 109943039 A CN109943039 A CN 109943039A CN 201910117247 A CN201910117247 A CN 201910117247A CN 109943039 A CN109943039 A CN 109943039A
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Abstract
The invention discloses a kind of methylation lignin/PBAT biodegradable plastics and preparation method thereof, the preparation method of the biodegradable plastics includes: the synthesis of methylation lignin, methylation lignin/PBAT biodegradable plastics master batch synthesis and methylation lignin/PBAT biodegradable plastics preparation.Methylation lignin/PBAT the biodegradable plastics of methylate lignin and polyadipate/mutual-phenenyl two acid bromide two alcohol ester (PBAT) compound preparation by being met the requirement of completely degradable plastic by the present invention.The compatibility to methylate between modified lignin resin and PBAT plastic substrate is fine, and in 60% methylation lignin additive amount, the mechanical property of composite material still keeps excellent.The biodegradable plastics do not add any plastic additive, it can be achieved that lignin high additive amount, be effectively reduced the preparation cost of composite material, improve the market competitiveness.
Description
Technical field
The invention belongs to biodegradable plastics fields, and in particular to a kind of methylation lignin/PBAT is biodegradable
Plastics and preparation method thereof.
Background technique
In recent years, petroleum-based energy problem and problem of environmental pollution are just causing the general concern of the whole society.Using petroleum as raw material
The plastic products of production are the main reason for causing " white pollution ", because these plastics are generally nondegradable.Exactly this
A little reasons, the production and use of biodegradable plastics increasingly cause the concern of society.
PBAT is the copolymer of PBA and PBT, combines the excellent degradation property of aliphatic polyester and aromatic polyester is good
Mechanics, thermal property, have good tensile strength and elongation at break.The hot-working condition and low density polyethylene (LDPE) of PBAT
(LDPE) similar, it is at present using best one of biodegradable plastics.
Lignin is the maximum natural aroma compound of reserves in nature, has high, biodegradable, the anti-purple of thermostabilization
Outside, the properties such as anti-oxidant.By-product of the lignin as pulping and paper-making and bio-ethanol industry, it is cheap and easy to get but most wooden
Element is directly burnt to provide the energy for factory.
Lignin is blended with PBAT and prepares biodegradable composite, can not only reduce the price of PBAT material,
It can also realize the higher value application of lignin.The more hydrogen bond of lignin itself and poor with the biggish polarity of plastic substrate,
So that lignin and PBAT matrix compatibility are bad.It often needs that plastic additive is added in the industrial production, such as acetyl tributyl citrate three
N-butyl (ATBC), maleic anhydride (MAH) etc. improve compatibility.Although used various plastic additives, answered with PBAT
In conjunction, the additive amount of lignin is still less, so that final product price is still higher.Lignin is passed through into chemical modification,
While guaranteeing that performance meets the requirements, the additive amount of lignin can be significantly improved, the price of composite material is effectively reduced, very
With application prospect.
Summary of the invention
The present invention prepares one kind with high lignin addition using PBAT and methylation lignin as raw material, by mixing extrusion
The biodegradable environmentally-friendly plastic of amount, excellent mechanical performance, can be used for the production of the products such as refuse bag, mulch, green house of vegetables film.
The object of the invention to solve the technical problems adopts the following technical solutions to realize:
A kind of methylation lignin/PBAT biodegradable plastics proposed according to the present invention and preparation method thereof, including
Following steps:
The synthesis of methylation lignin: by lignin dissolution in dimethyl sulfoxide (DMSO), cesium carbonate and carbonic acid is added
Dimethyl ester (DMC) after being put into reaction kettle sealing, carries out the first reaction, after the reaction was completed, mixture is cooled to room temperature, use
Lignin is precipitated in hydrochloric acid solution, is cleaned with deionized water to neutrality, and drying, ball milling obtain methylation lignin, spare；
Methylation lignin/PBAT biodegradable plastics master batch synthesis: PBAT masterbatch, methylation lignin are existed respectively
Forced air drying is carried out under first drying condition, and dried PBAT masterbatch, methylation lignin are added in a high speed mixer,
After being sufficiently mixed, obtain mixed material, by gained mixed material through double screw extruder the extruding pelletization under the first extrusion condition,
Methylation lignin/PBAT biodegradable plastics master batch is obtained, it is spare；
Methylate lignin/PBAT biodegradable plastics preparation: can biology by above-mentioned gained methylation lignin/PBAT
Degradative plastics master batch carries out hot-forming, obtained methylation lignin/PBAT biodegradable plastics under the first hot pressing condition.
The object of the invention to solve the technical problems also can be used following technical measures and further realize:
Preferably, preparation method above-mentioned, wherein the ratio of the lignin and dimethyl sulfoxide be 1:15-25 (g:
ML), the additive amount of the cesium carbonate is the 1.5-2.5 equivalent of content of phenolic hydroxyl groups in lignin sample, the dimethyl carbonate
Additive amount is the 6-10 equivalent of content of phenolic hydroxyl groups in lignin sample, and the mass ratio of the PBAT masterbatch and methylation lignin is
0.6-1.5:1。
Preferably, preparation method above-mentioned, wherein first reaction condition are as follows: 110-140 DEG C of temperature, time 5-7h；
First drying condition are as follows: 30-80 DEG C of temperature, time 1-6h；First extrusion condition are as follows: 120-170 DEG C of temperature, screw rod
Revolving speed 30-70r/min, master batch partial size 1-3mm；First hot pressing condition are as follows: 130-170 DEG C of temperature, preload pressure 0.4-
1.6MPa, boost pressure 2-8MPa.
Preferably, preparation method above-mentioned, wherein the lignin is alkali lignin, pre-hydrolyzed solution lignin, sulfuric acid
At least one of salt lignin.
Preferably, preparation method above-mentioned, wherein the hydrochloric acid solution is the hydrochloric acid solution that pH is 1-3.
A kind of methylation lignin/PBAT biodegradable plastics proposed according to the present invention and preparation method thereof, it is described
Methylation lignin/PBAT biodegradable plastics can be prepared by any of the above-described the method.
By above-mentioned technical proposal, methylation lignin/PBAT biodegradable plastics of the invention at least has following
Advantage:
(1) methylation of the invention lignin/PBAT biodegradable plastics preparation method, effectively improve lignin with
The problem of lignin is reunited in poor compatibility and process between PBAT plastic substrate, reach 60% in content of lignin
When, still there is excellent mechanical property.
(2) methylation of the invention lignin/PBAT biodegradable plastics is during the preparation process without using any modeling
Expect auxiliary agent, can still realize the high additive amount of lignin, the cost of composite material is effectively reduced.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, with presently preferred embodiments of the present invention, detailed description is as follows below.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Preferred embodiment, to a kind of methylation lignin/PBAT biodegradable plastics proposed according to the present invention and preparation method thereof
Its specific embodiment, feature and its effect, detailed description is as follows.In the following description, different " embodiment " or " implementation
What example " referred to is not necessarily the same embodiment.In addition, the special characteristic, structure or feature in one or more embodiments can be by any
Suitable form combination.
The embodiment of the present invention proposes a kind of methylation lignin/PBAT biodegradable plastics and preparation method thereof.
The preparation method the following steps are included:
The synthesis of methylation lignin: by lignin dissolution in dimethyl sulfoxide (DMSO), lignin and dimethyl are sub-
The ratio of sulfone is 1:15-25 (g:mL), and cesium carbonate and dimethyl carbonate (DMC) is added, and the additive amount of cesium carbonate is lignin sample
The 1.5-2.5 equivalent of content of phenolic hydroxyl groups in product, the additive amount of dimethyl carbonate are the 6-10 of content of phenolic hydroxyl groups in lignin sample
Equivalent is put into reaction kettle.Reaction kettle sealing is placed in 110-140 DEG C of heating muff and heats 5-7h, it after the reaction was completed, will
Mixture is cooled to room temperature, and lignin is precipitated using the hydrochloric acid solution of pH=1-3, is cleaned with deionized water to neutrality, through drying
Dry, ball milling obtains methylation lignin, spare；
Methylation lignin/PBAT biodegradable plastics master batch synthesis: PBAT masterbatch, methylation lignin are existed respectively
Dried PBAT masterbatch, methylation wood is added in dry 1-6h in 30-80 DEG C of temperature of convection oven in a high speed mixer
The mass ratio of quality, PBAT masterbatch and methylation lignin is 0.6-1.5:1.After being sufficiently mixed, mixed material is obtained, by gained
Mixed material extruding pelletization under 120-170 DEG C of temperature, screw speed 30-70r/min through double screw extruder, master batch partial size 1-
3mm obtains methylation lignin/PBAT biodegradable plastics master batch, spare；
Methylate lignin/PBAT biodegradable plastics preparation: can biology by above-mentioned gained methylation lignin/PBAT
Degradative plastics master batch is hot pressed under conditions of 130-170 DEG C of temperature, preload pressure 0.4-1.6MPa, boost pressure 2-8MPa
Methylation lignin/PBAT biodegradable plastics is made in type.
In the present embodiment, lignin includes but is not limited to: alkali lignin, pre-hydrolyzed solution lignin, in sulfate-reducing conditions
At least one.
Embodiment 1
(1) by pre-hydrolyzed solution lignin dissolution in dimethyl sulfoxide (DMSO), the ratio of lignin and dimethyl sulfoxide
For 1:15 (g:mL), cesium carbonate and dimethyl carbonate (DMC) is added, the additive amount of cesium carbonate is that phenolic hydroxyl group contains in lignin sample
2 equivalents of amount, the additive amount of dimethyl carbonate are 6 equivalents of content of phenolic hydroxyl groups in lignin sample, are put into reaction kettle.It will be anti-
It answers kettle sealing to be placed in 120 DEG C of heating muffs and heats 5h, after the reaction was completed, mixture is cooled to room temperature, uses pH=2's
Lignin is precipitated in hydrochloric acid solution, is cleaned with deionized water to neutrality, and drying, ball milling obtain methylation lignin, spare；
(2) respectively by PBAT masterbatch, methylation lignin drying 3h in the convection oven of temperature 70 C, in mixed at high speed
Dried PBAT masterbatch, methylation lignin are added in machine, PBAT masterbatch and the mass ratio of methylation lignin are 1.5:
1.After being sufficiently mixed, mixed material is obtained, by gained mixed material through double screw extruder at 130 DEG C of temperature, screw speed
Extruding pelletization under 50r/min, master batch partial size 2mm obtain methylation lignin/PBAT biodegradable plastics master batch, spare；
(3) by above-mentioned gained methylation lignin/PBAT biodegradable plastics master batch at 130 DEG C of temperature, preload pressure
It is hot-forming under conditions of 1MPa, boost pressure 5.5MPa, methylation lignin/PBAT biodegradable plastics is made.
Plastics manufactured in the present embodiment are tested for the property, table 1 is as a result listed in.
Embodiment 2
(1) by pre-hydrolyzed solution lignin dissolution in dimethyl sulfoxide (DMSO), the ratio of lignin and dimethyl sulfoxide
For 1:18 (g:mL), cesium carbonate and dimethyl carbonate (DMC) is added, the additive amount of cesium carbonate is that phenolic hydroxyl group contains in lignin sample
2.5 equivalents of amount, the additive amount of dimethyl carbonate are 8 equivalents of content of phenolic hydroxyl groups in lignin sample, are put into reaction kettle.It will
Reaction kettle sealing, which is placed in 125 DEG C of heating muffs, heats 6h, and after the reaction was completed, mixture is cooled to room temperature, uses pH=2
Hydrochloric acid solution be precipitated lignin, cleaned with deionized water to neutrality, drying, ball milling obtain methylation lignin, it is spare；
(2) respectively by PBAT masterbatch, methylation lignin drying 3h in the convection oven of temperature 60 C, in mixed at high speed
Be added in machine dried PBAT masterbatch, methylation lignin, PBAT masterbatch and methylation lignin mass ratio be 1:1.
After being sufficiently mixed, mixed material is obtained, by gained mixed material through double screw extruder at 140 DEG C of temperature, screw speed 40r/
Extruding pelletization under min, master batch partial size 2mm obtain methylation lignin/PBAT biodegradable plastics master batch, spare；
(3) by above-mentioned gained methylation lignin/PBAT biodegradable plastics master batch at 140 DEG C of temperature, preload pressure
It is hot-forming under conditions of 1.2MPa, boost pressure 6MPa, methylation lignin/PBAT biodegradable plastics is made.
Plastics manufactured in the present embodiment are tested for the property, table 1 is as a result listed in.
Embodiment 3
(1) by pre-hydrolyzed solution lignin dissolution in dimethyl sulfoxide (DMSO), the ratio of lignin and dimethyl sulfoxide
For 1:20 (g:mL), cesium carbonate and dimethyl carbonate (DMC) is added, the additive amount of cesium carbonate is that phenolic hydroxyl group contains in lignin sample
1.5 equivalents of amount, the additive amount of dimethyl carbonate are 10 equivalents of content of phenolic hydroxyl groups in lignin sample, are put into reaction kettle.
Reaction kettle sealing is placed in 130 DEG C of heating muffs and heats 6h, after the reaction was completed, mixture is cooled to room temperature, uses pH
Lignin is precipitated in=2 hydrochloric acid solution, is cleaned with deionized water to neutrality, and drying, ball milling obtain methylation lignin, standby
With；
(2) respectively by PBAT masterbatch, methylation lignin drying 3h in the convection oven of temperature 60 C, in mixed at high speed
Dried PBAT masterbatch, methylation lignin are added in machine, PBAT masterbatch and the mass ratio of methylation lignin are 0.6:
1.After being sufficiently mixed, mixed material is obtained, by gained mixed material through double screw extruder at 150 DEG C of temperature, screw speed
Extruding pelletization under 50r/min, master batch partial size 2mm obtain methylation lignin/PBAT biodegradable plastics master batch, spare；
(3) by above-mentioned gained methylation lignin/PBAT biodegradable plastics master batch at 145 DEG C of temperature, preload pressure
It is hot-forming under conditions of 1.1MPa, boost pressure 6MPa, methylation lignin/PBAT biodegradable plastics is made.
Plastics manufactured in the present embodiment are tested for the property, table 1 is as a result listed in.
Comparative example 1
(1) PBAT masterbatch, pre-hydrolyzed solution lignin are dried into 3h in the convection oven of temperature 60 C respectively, in high mixer
Interior that dried PBAT masterbatch, pre-hydrolyzed solution lignin is added, PBAT masterbatch and the mass ratio of pre-hydrolyzed solution lignin are 1.5:
1.After being sufficiently mixed, mixed material is obtained, by gained mixed material through double screw extruder at 130 DEG C of temperature, screw speed 50r/
Extruding pelletization under the conditions of min, master batch partial size 2mm obtain lignin/PBAT biodegradable plastics master batch, spare.
(2) by gained lignin/PBAT biodegradable plastics master batch at 130 DEG C of temperature, preload pressure 1MPa, pressurization pressure
It is hot-forming under conditions of power 5.5MPa, lignin/PBAT biodegradable plastics is made.
The plastics of this comparative example preparation are tested for the property, table 1 is as a result listed in.
Comparative example 2
(1) PBAT masterbatch, pre-hydrolyzed solution lignin are dried into 3h in the convection oven of temperature 60 C respectively, in high mixer
The mass ratio of the dried PBAT masterbatch of interior addition, pre-hydrolyzed solution lignin, PBAT masterbatch and pre-hydrolyzed solution lignin is 1:1.
After being sufficiently mixed, mixed material is obtained, by gained mixed material through double screw extruder at 140 DEG C of temperature, screw speed 40r/min
Under the conditions of extruding pelletization, master batch partial size 2mm obtains lignin/PBAT biodegradable plastics master batch, spare.
(2) by gained lignin/PBAT biodegradable plastics master batch at 140 DEG C of temperature, preload pressure 1.2MPa, pressurization
It is hot-forming under conditions of pressure 6MPa, lignin/PBAT biodegradable plastics is made.
The plastics of this comparative example preparation are tested for the property, table 1 is as a result listed in.
Comparative example 3
(1) PBAT masterbatch, pre-hydrolyzed solution lignin are dried into 3h in the convection oven of temperature 60 C respectively, in high mixer
Interior that dried PBAT masterbatch, pre-hydrolyzed solution lignin is added, PBAT masterbatch and the mass ratio of pre-hydrolyzed solution lignin are 0.6:
1.After being sufficiently mixed, mixed material is obtained, by gained mixed material through double screw extruder at 150 DEG C of temperature, screw speed 50r/
Extruding pelletization under the conditions of min, master batch partial size 2mm obtain lignin/PBAT biodegradable plastics master batch, spare.
(2) by gained lignin/PBAT biodegradable plastics master batch at 145 DEG C of temperature, preload pressure 1.1MPa, pressurization
It is hot-forming under conditions of pressure 6MPa, lignin/PBAT biodegradable plastics is made.
The plastics of this comparative example preparation are tested for the property, table 1 is as a result listed in.
The performance test of each embodiment of table 1 and comparative example
Note: it the detection of above-mentioned plastics: is measured according to national standard GB/T 1040.3-2006, design parameter GB/T
1040.3/5B-10.Using electronic universal tester, (high-tech stock in length and breadth is thought carefully in UTM6503 electronic universal tester, Shenzhen to batten
Part Co., Ltd) it is stretched, tensile speed 20mm/min, room temperature is 25 ± 2 DEG C.To guarantee that data are accurate, all mechanics
Performance test the data obtained is taken from least seven Test strips.
There is the test result in above-mentioned table it can be seen that embodiment is compared with comparative example, under identical mass ratio, uses first
Base lignin can significantly improve the tensile strength and elongation at break of composite material.Wherein, embodiment 2 and embodiment 3
Elongation at break has been respectively increased four times or more.The above comparison can show advantage of the invention.
The above is merely a preferred embodiment of the present invention, and is not intended to restrict the invention, and without departing substantially from this
In the case where the spirit or essential attributes of invention, the present invention can be realized in other specific forms.For the technology of this field
For personnel, it is still possible to modify the technical solutions described in the foregoing embodiments, or to part of technology
Feature is equivalently replaced.All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on,
It is included within protection scope of the present invention.
Claims (5)
1. a kind of methylation lignin/PBAT biodegradable plastics and preparation method thereof, which is characterized in that including following step
It is rapid:
The preparation synthesis of methylation lignin: by lignin dissolution in dimethyl sulfoxide (DMSO), cesium carbonate and carbonic acid is added
Dimethyl ester (DMC), is put into reaction kettle, carries out the first reaction, after the reaction was completed, mixture is cooled to room temperature, uses hydrochloric acid
Lignin is precipitated in solution, is cleaned with deionized water to neutrality, and drying, ball milling obtain methylation lignin, spare；
Methylate lignin/PBAT biodegradable plastics master batch synthesis: respectively by polyadipate/mutual-phenenyl two acid bromide two alcohol ester
(PBAT) masterbatch, methylation lignin carry out forced air drying under the first drying condition, are added in a high speed mixer dried
PBAT masterbatch, methylation lignin, after being sufficiently mixed, obtain mixed material, gained mixed material existed through twin-screw extrusion
Extruding pelletization under first extrusion condition obtains methylation lignin/PBAT biodegradable plastics master batch, spare；
Methylate lignin/PBAT biodegradable plastics preparation: above-mentioned gained methylation lignin/PBAT is biodegradable
Plastic master batch carries out hot-forming, obtained methylation lignin/PBAT biodegradable plastics under the first hot pressing condition.
2. preparation method according to claim 1, which is characterized in that
The ratio of the lignin and dimethyl sulfoxide is 1:15-25 (g:mL),
The additive amount of the cesium carbonate is the 1.5-2.5 equivalent of content of phenolic hydroxyl groups in lignin sample,
The additive amount of the dimethyl carbonate is the 6-10 equivalent of content of phenolic hydroxyl groups in lignin sample,
The mass ratio of the PBAT masterbatch and methylation lignin is 0.6-1.5:1.
3. preparation method according to claim 1, which is characterized in that
First reaction condition are as follows: 110-140 DEG C of temperature, time 5-7h；
First drying condition are as follows: 30-80 DEG C of temperature, time 1-6h；
First extrusion condition are as follows: 120-170 DEG C of temperature, screw speed 30-70r/min, master batch partial size 1-3mm；
First hot pressing condition are as follows: 130-170 DEG C of temperature, preload pressure 0.4-1.6MPa, boost pressure 2-8MPa.
4. preparation method according to claim 1, which is characterized in that
The lignin is at least one of alkali lignin, pre-hydrolyzed solution lignin, sulfate-reducing conditions.
5. preparation method according to claim 1, which is characterized in that
The hydrochloric acid solution is the hydrochloric acid solution that pH is 1-3.
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| CN113881195A (en) * | 2021-09-30 | 2022-01-04 | 宜宾天亿新材料科技有限公司 | Biodegradable resin composition and preparation method thereof |
| CN114933785A (en) * | 2022-04-29 | 2022-08-23 | 上海昶法新材料有限公司 | Modified lignin/PBAT biodegradable plastic and preparation method thereof |
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Application publication date: 20190628 |