CN109385059A - A kind of PLA/PPC biological degradable composite material of high tenacity and preparation method thereof - Google Patents
A kind of PLA/PPC biological degradable composite material of high tenacity and preparation method thereof Download PDFInfo
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- CN109385059A CN109385059A CN201811263123.9A CN201811263123A CN109385059A CN 109385059 A CN109385059 A CN 109385059A CN 201811263123 A CN201811263123 A CN 201811263123A CN 109385059 A CN109385059 A CN 109385059A
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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
- 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
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
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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
- C08L2205/06—Polymer mixtures characterised by other features having improved processability or containing aids for moulding methods
Abstract
The invention belongs to the preparations and application technology of the new functional macromolecule material of high molecular material in new material, are related to modified plastics technical field, specifically a kind of preparation method of the PLA/PPC biological degradable composite material of high tenacity.The present invention extracts active constituent as natural antibacterial agent from Radix Notoginseng, Fructus Forsythiae, cloves first;Then it will be granulated after mixing after poly (propylene carbonate), starch micro mist, polylactic acid drying with natural, natural antibacterial agent, auxiliary agent, PLA/PPC biological degradable composite material be prepared;PLA/PPC biological degradable composite material is finally modified into the PLA/PPC biological degradable composite material that high tenacity is made in raising toughness with silylating reagent using after alkali process.Through the PLA/PPC composite material that is prepared of the present invention not only easily biological-degradable but also anti-microbial property is good, excellent in mechanical performance and safe and non-toxic.
Description
Technical field
The invention belongs to the preparations and application technology of the new functional macromolecule material of high molecular material in new material, are related to
Modified plastics technical field, specifically the PLA/PPC biological degradable composite material and preparation method thereof of a kind of high tenacity.
Background technique
Polylactic acid (PLA) due to its excellent biocompatibility and biodegradability and its thermoplasticity, anti-permeability,
Mechanical property is similar to polyester, in production film, sheet material, bottle and various hot forming product and injecting products and various weavings
Product or nonwoven products field show huge application prospect.But some performance deficiencies existing for PLA itself, such as property
Crisp, melt strength low-heat stablizes difference etc. and limits its application.
Poly (propylene carbonate) (PPC) is by CO2It participates in reacting complete biodegradable polymer obtained, have similar to PLA
Chemical structure, therefore PPC and PLA have certain compatibility simultaneously PPC with preferable toughness, can toughening PLA, from
And the biodegradation material of high tenacity can be prepared.
Summary of the invention
In order to solve the problems such as property is crisp existing for traditional polylactic acid plastic, melt strength low-heat stablizes difference.Of the invention mentions
A kind of preparation method of the PLA/PPC biological degradable composite material of high tenacity is supplied.In order to achieve the above objectives, the present invention will
Using following technology:
A kind of preparation method of the PLA/PPC biological degradable composite material of high tenacity, which comprises the following steps:
(1) will Radix Notoginseng, Fructus Forsythiae, cloves it is dry after crushed respectively three kinds of herb powders are mixed after 60 meshes after through microwave treatment
After 10-15min, after herb powder is mixed with ethanol-water mixture by the mass volume ratio (g/mL) of 1:15-20, in 60-75
It being filtered after refluxing extraction 2-4h under the conditions of DEG C, filter residue uses refluxing extraction-filtration step to repeat merging filtrate after extracting 2-3 times again,
Filtrate is crossed after ultrafiltration membrane and is concentrated into after the density of solution is 1.1-1.2g/mL, concentrate and ethyl alcohol-salt aqueous two-phase are pressed into 1:2-
After 3 volume ratio mixing, after ultrasonic 5-10min standing is divided into two-phase, upper phase is isolated with separatory funnel, upper phase is depressurized and is steamed
It crushed 60 meshes after dry, obtain natural antibacterial agent;
(2) it will be mixed after poly (propylene carbonate), starch micro mist, polylactic acid drying with natural, natural antibacterial agent, auxiliary agent
It is transferred in double screw extruder after uniformly, PLA/PPC biological degradable composite material is prepared after extruding pelletization;
(3) it after further crushing step (2) resulting biological degradable composite material, is scattered in dehydrated alcohol, Xiang Wushui second
After the NaOH alcoholic solution of saturation is added in alcohol, the solid was filtered part after 3-5h is impregnated at room temperature, under the conditions of 300-500rpm,
Obtained solid part is dispersed again in the acetone soln of silylating reagent, is reacted under the conditions of 40-60 DEG C, 400-600rpm
After 12-14h, filtering solid portion obtains high tenacity after being dried in vacuo under the conditions of 75-85 DEG C after being cleaned 2-3 times with acetone
PLA/PPC biological degradable composite material.
Preferably, Radix Notoginseng, Fructus Forsythiae, cloves mass ratio are 1:0.5-2:0.5-2 in herb powder as described in step (1);
The volume fraction of ethyl alcohol is 30-45% in the ethanol-water mixture.
Preferably, 5000 in the molecular cut off of ultrafiltration membrane as described in step (1).
Preferably, ethyl alcohol as described in step (1)-salt aqueous two-phase is the preparation method comprises the following steps: by ethyl alcohol and 0.2-0.4g/mL
K2HPO4After solution is by the volume ratio mixing of 1:1-3, ultrasound is stood up to ethyl alcohol-salt aqueous two-phase.
Preferably, starch micro mist described in step (2) is one of cornstarch, wheaten starch, red pigment starch;Institute
The partial size for the starch micro mist stated is not more than 2 μm;The natural is one of vitamin C, gallic acid;Institute
The auxiliary agent stated is one of talcum powder, calcium carbonate, mica powder or a variety of.
Preferably, poly (propylene carbonate) described in step (2), starch micro mist, polylactic acid, natural, natural
Antibacterial agent, auxiliary agent mixing when additional amount by mass fraction be followed successively by 25-30 parts, 25-45 parts, 40-50 parts, 1-3 parts, 1-3 parts,
1-3 parts.
Preferably, silylating reagent described in step (2) are as follows: hexadecyl, three second of octadecyl
One of oxysilane, myristyl triethoxysilane;The additional amount of the silylating reagent is that biodegrade is compound
The 15-20% of quality of materials.
In addition, the PLA/PPC biological degradable composite material of high tenacity of the invention, as prepared by above-mentioned preparation method.
Compared with prior art, the preparation method of the PLA/PPC biological degradable composite material of a kind of high tenacity of the invention
Have it is following the utility model has the advantages that
Joint aqueous two-phase purification technique is extracted using alcohol reflux and extracts active skull cap components from Chinese medicine as the natural of plastics
Antibacterial agent not only strengthens the anti-microbial property of material, while not using artificial synthesized antibacterial agent, so that material is safer;
Polylactic acid is modified using poly (propylene carbonate), the high tenacity of poly (propylene carbonate) enhances the toughness of material;Using alkali
Solution and silylating reagent modify material table, further strengthen the resistance to of the mechanical properties such as the toughness of material and material
It is aqueous.In addition, the adding ingredient that the present invention prepares material is mostly natural component, product safety performance is further ensured.Through this
Invent the PLA/PPC composite material that is prepared not only easily biological-degradable but also anti-microbial property is good, excellent in mechanical performance and peace
Atoxic.
Specific embodiment
[embodiment 1]
A kind of preparation method of the PLA/PPC biological degradable composite material of high tenacity, which comprises the following steps:
(1) will Radix Notoginseng, Fructus Forsythiae, cloves it is dry after crushed Radix Notoginseng, Fructus Forsythiae, the dry herb powder of cloves after 60 meshes respectively by 1:
After the mass ratio mixing of 1:1 after microwave treatment 10min, the ethanol-water mixture of herb powder and 35% is pressed to the quality of 1:20
After volume ratio after (g/mL) mixing, filtered after refluxing extraction 3h under the conditions of 70 DEG C, filter residue uses refluxing extraction-filtration step weight again
Merging filtrate after extracting 2 times again, it is 1.1- that filtrate, which is crossed after the ultrafiltration membrane that molecular cut off is 5000, and is concentrated into the density of solution
After 1.2g/mL, after concentrate is mixed with ethyl alcohol-salt aqueous two-phase by the volume ratio of 1:3, ultrasonic 6min, after standing is divided into two-phase,
Upper phase is isolated with separatory funnel, 60 meshes will be crushed after upper phase evaporated under reduced pressure, obtain natural antibacterial agent;
(2) after 25 parts of poly (propylene carbonate)s, 30 parts of starch micro mists, 40 parts of polylactic acid being dried naturally with 1.5 parts of vitamin Cs, 1.5
Antibacterial agent, 2 parts of calcium carbonate are transferred in double screw extruder after mixing, and it is raw that PLA/PPC is prepared after extruding pelletization
Object degrading composite;
(3) it after further crushing step (2) resulting biological degradable composite material, is scattered in dehydrated alcohol, Xiang Wushui second
After the NaOH alcoholic solution of saturation is added in alcohol, the solid was filtered part after 3-5h is impregnated at room temperature, under the conditions of 400rpm, by institute
In the acetone soln for obtaining the hexadecyl that solid portion is dispersed again in 15%, at 50 DEG C, under the conditions of 500rpm
After reacting 13h, filtering solid portion cleans after 3 times the PLA/ for obtaining high tenacity after vacuum drying under the conditions of 75-85 DEG C with acetone
PPC biological degradable composite material.
[embodiment 2]
A kind of preparation method of the PLA/PPC biological degradable composite material of high tenacity, which comprises the following steps:
(1) will Radix Notoginseng, Fructus Forsythiae, cloves it is dry after crushed Radix Notoginseng, Fructus Forsythiae, the dry herb powder of cloves after 60 meshes respectively by 1:
After the mass ratio mixing of 1.5:2 after microwave treatment 10min, the ethanol-water mixture of herb powder and 40% is pressed to the matter of 1:18
It after amount volume ratio (g/mL) mixes afterwards, is filtered after refluxing extraction 2.5h under the conditions of 70 DEG C, filter residue uses refluxing extraction-filtering step again
Merging filtrate after merging filtrate 2 times, is concentrated into after filtrate is crossed the ultrafiltration membrane that molecular cut off is 5000 after rapid repetition extraction 2 times
After the density of solution is 1.1-1.2g/mL, after concentrate is mixed with ethyl alcohol-salt aqueous two-phase by the volume ratio of 1:2.5, ultrasound
6min isolates upper phase with separatory funnel, will crushed 60 meshes after upper phase evaporated under reduced pressure, obtain naturally after standing is divided into two-phase
Antibacterial agent;
(2) by 25 parts of poly (propylene carbonate)s, 25 parts of starch micro mists, 47 parts of polylactic acid it is dry after with 1 part of vitamin C, 1 natural antibacterial
Agent, 1 part of calcium carbonate are transferred in double screw extruder after mixing, and PLA/PPC biology drop is prepared after extruding pelletization
Solve composite material;
(3) it after further crushing step (2) resulting biological degradable composite material, is scattered in dehydrated alcohol, Xiang Wushui second
After the NaOH alcoholic solution of saturation is added in alcohol, the solid was filtered part after 3-5h is impregnated at room temperature, under the conditions of 400rpm, by institute
It obtains solid portion to be dispersed again in 17% acetone soln of myristyl triethoxysilane, at 50 DEG C, under the conditions of 500rpm
After reacting 14h, filtering solid portion cleans after 3 times the PLA/ for obtaining high tenacity after vacuum drying under the conditions of 75-85 DEG C with acetone
PPC biological degradable composite material.
[embodiment 3]
A kind of preparation method of the PLA/PPC biological degradable composite material of high tenacity, which comprises the following steps:
(1) will Radix Notoginseng, Fructus Forsythiae, cloves it is dry after crushed Radix Notoginseng, Fructus Forsythiae, the dry herb powder of cloves after 60 meshes respectively by 1:
After the mass ratio mixing of 0.8:1.2 after microwave treatment 10min, the ethanol-water mixture of herb powder and 45% is pressed 1:15's
After being mixed after mass volume ratio, filtered after refluxing extraction 2.5h under the conditions of 70 DEG C, filter residue uses refluxing extraction-filtration step weight again
Merging filtrate after merging filtrate 2 times, is concentrated into solution after filtrate is crossed the ultrafiltration membrane that molecular cut off is 5000 after extracting 2 times again
Density be 1.1-1.2g/mL after, after concentrate is mixed with ethyl alcohol-salt aqueous two-phase by the volume ratio of 1:2.5, ultrasonic 6min,
After standing is divided into two-phase, upper phase is isolated with separatory funnel, 60 meshes will be crushed after upper phase evaporated under reduced pressure, obtain natural antibacterial
Agent;
(2) by 28 parts of poly (propylene carbonate)s, 29 parts of starch micro mists, 40 parts of polylactic acid it is dry after with 1 part of vitamin C, 1 natural antibacterial
Agent, 1 part of calcium carbonate are transferred in double screw extruder after mixing, and PLA/PPC biology drop is prepared after extruding pelletization
Solve composite material;
(3) it after further crushing step (2) resulting biological degradable composite material, is scattered in dehydrated alcohol, Xiang Wushui second
After the NaOH alcoholic solution of saturation is added in alcohol, the solid was filtered part after 3-5h is impregnated at room temperature, under the conditions of 400rpm, by institute
In the acetone soln for obtaining the hexadecyl that solid portion is dispersed again in 17%, at 50 DEG C, under the conditions of 500rpm
After reacting 14h, filtering solid portion cleans after 3 times the PLA/ for obtaining high tenacity after vacuum drying under the conditions of 75-85 DEG C with acetone
PPC biological degradable composite material.
For the ordinary skill in the art, specific embodiment is only exemplarily described the present invention,
Obviously the present invention specific implementation is not subject to the restrictions described above, as long as use the inventive concept and technical scheme of the present invention into
The improvement of capable various unsubstantialities, or not improved the conception and technical scheme of the invention are directly applied to other occasions
, it is within the scope of the present invention.
Claims (8)
1. a kind of preparation method of the PLA/PPC biological degradable composite material of high tenacity, which comprises the following steps:
(1) will Radix Notoginseng, Fructus Forsythiae, cloves it is dry after crushed respectively three kinds of herb powders are mixed after 60 meshes after through microwave treatment
After 10-15min, after herb powder is mixed with ethanol-water mixture by the mass volume ratio (g/mL) of 1:15-20, in 60-75
It being filtered after refluxing extraction 2-4h under the conditions of DEG C, filter residue uses refluxing extraction-filtration step to repeat merging filtrate after extracting 2-3 times again,
Filtrate is crossed after ultrafiltration membrane and is concentrated into after the density of solution is 1.1-1.2g/mL, concentrate and ethyl alcohol-salt aqueous two-phase are pressed into 1:2-
After 3 volume ratio mixing, after ultrasonic 5-10min standing is divided into two-phase, upper phase is isolated with separatory funnel, upper phase is depressurized and is steamed
It crushed 60 meshes after dry, obtain natural antibacterial agent;
(2) it will be mixed after poly (propylene carbonate), starch micro mist, polylactic acid drying with natural, natural antibacterial agent, auxiliary agent
It is transferred in double screw extruder after uniformly, PLA/PPC biological degradable composite material is prepared after extruding pelletization;
(3) it after further crushing step (2) resulting biological degradable composite material, is scattered in dehydrated alcohol, Xiang Wushui second
After the NaOH alcoholic solution of saturation is added in alcohol, the solid was filtered part after 3-5h is impregnated at room temperature, under the conditions of 300-500rpm,
Obtained solid part is dispersed again in the acetone soln of silylating reagent, is reacted under the conditions of 40-60 DEG C, 400-600rpm
After 12-14h, filtering solid portion obtains high tenacity after being dried in vacuo under the conditions of 75-85 DEG C after being cleaned 2-3 times with acetone
PLA/PPC biological degradable composite material.
2. a kind of preparation method of the PLA/PPC biological degradable composite material of high tenacity according to claim 1, special
Sign is that Radix Notoginseng, Fructus Forsythiae, cloves mass ratio are 1:0.5-2:0.5-2 in herb powder as described in step (1);The second
The volume fraction of ethyl alcohol is 30-45% in alcohol-aqueous mixtures.
3. a kind of preparation method of the PLA/PPC biological degradable composite material of high tenacity according to claim 1, special
Sign is, 5000 in the molecular cut off of ultrafiltration membrane as described in step (1).
4. a kind of preparation method of the PLA/PPC biological degradable composite material of high tenacity according to claim 1, special
Sign is that ethyl alcohol as described in step (1)-salt aqueous two-phase is the preparation method comprises the following steps: by ethyl alcohol and 0.2-0.4g/mL K2HPO4Solution
After the volume ratio mixing of 1:1-3, ultrasound is stood up to ethyl alcohol-salt aqueous two-phase.
5. a kind of preparation method of the PLA/PPC biological degradable composite material of high tenacity according to claim 1, special
Sign is that starch micro mist described in step (2) is one of cornstarch, wheaten starch, red pigment starch;The starch
The partial size of micro mist is not more than 2 μm;The natural is one of vitamin C, gallic acid;The auxiliary agent is
One of talcum powder, calcium carbonate, mica powder are a variety of.
6. a kind of preparation method of the PLA/PPC biological degradable composite material of high tenacity according to claim 1, special
Sign is that poly (propylene carbonate) described in step (2), polylactic acid, natural, natural antibacterial agent, helps starch micro mist
Additional amount when agent mixes is followed successively by 25-30 parts, 25-45 parts, 40-50 parts, 1-3 parts, 1-3 parts, 1-3 parts by mass fraction.
7. a kind of preparation method of the PLA/PPC biological degradable composite material of high tenacity according to claim 1, special
Sign is, silylating reagent described in step (2) are as follows: hexadecyl, octadecyltriethoxy silane,
One of myristyl triethoxysilane;The additional amount of the silylating reagent is biological degradable composite material quality
15-20%。
8. the PLA/PPC biological degradable composite material of a kind of high tenacity, as described in -7 any one according to claim 1
Prepared by preparation method.
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