CN112226048A - Synthetic process of degradable biopolymer material - Google Patents
Synthetic process of degradable biopolymer material Download PDFInfo
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- CN112226048A CN112226048A CN202011084479.3A CN202011084479A CN112226048A CN 112226048 A CN112226048 A CN 112226048A CN 202011084479 A CN202011084479 A CN 202011084479A CN 112226048 A CN112226048 A CN 112226048A
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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
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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
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
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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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Abstract
The invention discloses a synthesis process of a degradable biopolymer material, which relates to the technical field of synthesis of degradable biopolymer materials, in particular to a synthesis process of a degradable biopolymer material, and the synthesis process comprises the following components in parts by weight: 40-50 parts of degradable polymer produced by microorganism, 30-40 parts of epoxy resin, 10-20 parts of unitary polyamide resin, 15-25 parts of lactide, 10-20 parts of lactic acid, 6-10 parts of talcum powder, 4-8 parts of film-forming additive, 3-5 parts of catalyst, 1-3 parts of modifier, 2-5 parts of thickener, 1-2 parts of compatilizer, 3-5 parts of coupling agent, 2-3 parts of flexibilizer and 1-5 parts of bactericide. According to the synthesis process of the degradable biological high polymer material, the film-forming auxiliary agent can promote plastic flow and elastic deformation of a high polymer compound, improve the coalescence performance, and form a film in a wider construction temperature range, the catalyst can effectively promote the mixing efficiency of raw materials, and the thickening agent can effectively increase the mixing concentration of the raw materials and provide the uniform degree of raw material mixing.
Description
Technical Field
The invention relates to the technical field of synthesis of degradable biopolymer materials, in particular to a synthesis process of a degradable biopolymer material.
Background
The biodegradability of different biodegradable polymer materials is intensively studied and found to be greatly related to the structure, including chemical structure, physical structure, surface structure and the like. The chemical structure of the high molecular material directly influences the biodegradability, and generally: aliphatic ester bond, peptide bond > carbamate > aliphatic ether bond > methylene. When the solid structures of the same material are different, the degradation speeds of different aggregation states have the following sequence: rubbery > glassy > crystalline. Generally, the high-molecular material with high polarity can adhere to the enzyme and have good affinity, and the way of the microorganism adhering to the surface is influenced by the surface tension of the plastic, the surface structure, the multi-wriggling property, the stirring degree of the environment and the encroachment of the surface. The biodegradable polymer material is a polymer material which can be degraded by microorganisms or secretion thereof under the action of enzyme or chemical decomposition in a certain time and under a certain condition.
The existing degradable biological high molecular material has the defects of complex synthesis process, long consumed time, short storage time, difficult long-term transportation and inconvenient molding.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a synthesis process of a degradable biopolymer material, and solves the problems of complex synthesis process, long consumed time, short storage time, difficulty in long-term transportation and inconvenience in molding of the existing degradable biopolymer material in the background art.
In order to achieve the purpose, the invention is realized by the following technical scheme: a synthesis process of a degradable biopolymer material comprises the following components in parts by weight: 40-50 parts of degradable polymer produced by microorganism, 30-40 parts of epoxy resin, 10-20 parts of unitary polyamide resin, 15-25 parts of lactide, 10-20 parts of lactic acid, 6-10 parts of talcum powder, 4-8 parts of film-forming additive, 3-5 parts of catalyst, 1-3 parts of modifier, 2-5 parts of thickener, 1-2 parts of compatilizer, 3-5 parts of coupling agent, 2-3 parts of flexibilizer and 1-5 parts of bactericide.
Optionally, the microorganism-produced degradable polymer is one or more of a microorganism polyester, a polylactic acid, a microorganism polysaccharide and a copolymer of 3-hydroxybutyrate and 3-hydroxyvalerate, and the film-forming aid is at least one of propylene glycol butyl ether and propylene glycol methyl ether acetate.
Optionally, the catalyst is a homogeneous catalyst comprising one or two of acid, alkali, soluble transition metal compound and peroxide catalyst, and the heterogeneous catalyst is one or more of solid acid catalyst, organic base catalyst, metal oxide catalyst, complex catalyst, rare earth catalyst, molecular sieve catalyst, biocatalyst and nano catalyst.
Optionally, the thickener is one or more of methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, acrylic acid and methacrylic acid, and the coupling agent is one or more of organic chromium complex, silanes, titanates and aluminate compounds.
Optionally, the bactericide is an inorganic bactericide and an organic bactericide, the inorganic bactericide is at least one of sulfur powder, lime sulphur, copper sulfate, mercury bichloride, lime bordeaux mixture, copper hydroxide and cuprous oxide, and the organic bactericide is at least one of amobam, sodium diquat, ziram, zineb, mancozeb and thiram.
Optionally, the preparation method of the degradable biopolymer material comprises the following steps:
s1, weighing the raw materials in parts by mass: sequentially weighing a microorganism-produced degradable macromolecule, epoxy resin, unitary polyamide resin, lactide, lactic acid, talcum powder, a film-forming auxiliary agent, a catalyst, a modifier, a thickening agent, a compatilizer, a coupling agent, a toughening agent and a bactericide according to the mass parts of the raw materials;
s2, crushing: s1, weighing the degradable polymer, the epoxy resin and the unitary polyamide resin produced by the microorganism in the raw materials in parts by mass, and sequentially adding the talcum powder into a supersonic jet mill, and sieving to prepare a mixture A of the degradable polymer powder, the epoxy resin powder, the unitary polyamide resin powder and the talcum powder produced by the microorganism;
s3, primary stirring: adding the mixture A obtained in the step S2 in the crushing process into a reaction kettle, stirring, adding lactide and lactic acid, and uniformly stirring to obtain a mixture B;
s4, continuing stirring: sequentially adding a catalyst and a modifier in the preliminary stirring in the step S3, stirring, and adding a thickening agent, a compatilizer, a coupling agent and a toughening agent until the materials are uniformly mixed to obtain a mixture C;
s5, stirring again: adding the film-forming aid into the mixture C in the step S4, continuously stirring, and adding the bactericide to prepare a mixture D;
s6, forming the degradable biopolymer material: and (5) adding the mixture D obtained in the step (S5) into a double-screw extruder for melt extrusion granulation, and cooling and forming to obtain the degradable biopolymer material.
Optionally, in the step S2, in the crushing, the model of the crusher is DF-25A, the rotation speed is 2840r/min, the fineness is 60-200 meshes, and the power is 2000W, and the crusher is sieved by 80-100 meshes.
Optionally, in the step S4, during the continuous stirring, the catalyst and the modifier are sequentially added in the step S3 and the preliminary stirring, and the mixture is stirred for 11-15min at the temperature of 80-120 ℃, and the thickener, the compatibilizer, the coupling agent and the toughening agent are added, and the mixture is stirred for 15-25min at the temperature of 120-150 ℃.
Optionally, in the step S5, stirring again, stirring is performed for 11-15min at the temperature of 120-160 ℃.
Optionally, in the step S6 and the step of forming the degradable biopolymer material, the extrusion temperature of the twin-screw extruder is 240-.
The invention provides a synthesis process of a degradable biopolymer material, which has the following beneficial effects:
1. the synthesis process of the degradable biological high molecular material comprises a film-forming auxiliary agent, a catalyst, a modifier, a thickening agent, a compatilizer, a coupling agent, a toughening agent and a bactericide, wherein the film-forming auxiliary agent can promote plastic flow and elastic deformation of a high molecular compound, improve coalescence performance, form a film in a wider construction temperature range, the catalyst can effectively promote the mixing efficiency of raw materials, the thickening agent can effectively increase the mixing concentration of the raw materials and provide the uniform degree of the mixing of the raw materials, the coupling agent promotes or establishes a substance with strong combination on the interface of a resin substrate and the reinforcing material, the bactericide can effectively avoid damage of insect pest raw materials, and can effectively prolong the long-term storage of the degradable biological high molecular material.
2. The synthesis process of the degradable biopolymer material has the advantages of simple process synthesis, high mixing uniformity and stable structure.
Detailed Description
In the following, technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Embodiment 1
The invention provides a technical scheme that: a synthesis process of a degradable biopolymer material comprises the following components in parts by weight: 40 parts of degradable polymer produced by microorganism, 30 parts of epoxy resin, 10 parts of unitary polyamide resin, 15 parts of lactide, 10 parts of lactic acid, 6 parts of talcum powder, 4 parts of film-forming assistant, 3 parts of catalyst, 1 part of modifier, 2 parts of thickener, 1 part of compatilizer, 3 parts of coupling agent, 3 parts of toughening agent and 5 parts of bactericide.
The microorganism produced degradable macromolecule is one or more of microorganism polyester, polylactic acid, microorganism polysaccharide and copolymer of 3-hydroxybutyrate and 3-hydroxyvalerate, and the film-forming assistant is at least one of propylene glycol butyl ether and propylene glycol methyl ether acetate.
The catalyst is one or two of homogeneous catalyst, acid, alkali, soluble transition metal compound and peroxide catalyst, and the heterogeneous catalyst is one or more of solid acid catalyst, organic base catalyst, metal oxide catalyst, complex catalyst, rare earth catalyst, molecular sieve catalyst, biological catalyst and nano catalyst.
The thickening agent is one or more of methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, acrylic acid and methacrylic acid, and the coupling agent is one or more of organic chromium complex, silanes, titanates and aluminate compounds.
The bactericide is an inorganic bactericide and an organic bactericide, the inorganic bactericide is at least one of sulfur powder, lime sulfur, copper sulfate, mercury bichloride, calbodol solution and copper hydroxide and cuprous oxide, and the organic bactericide is at least one of amobam, sodium diformate, ziram, zineb, mancozeb and thiram.
The preparation method of the degradable biopolymer material comprises the following steps:
s1, weighing the raw materials in parts by mass: weighing 40 parts of microorganism-produced degradable macromolecule, 30 parts of epoxy resin, 10 parts of unitary polyamide resin, 15 parts of lactide, 10 parts of lactic acid, 6 parts of talcum powder, 4 parts of film-forming assistant, 3 parts of catalyst, 1 part of modifier, 2 parts of thickener, 1 part of compatilizer, 3 parts of coupling agent, 3 parts of toughening agent and 5 parts of bactericide in sequence according to the mass parts of the raw materials;
s2, crushing: s1, weighing the degradable polymer, the epoxy resin and the unitary polyamide resin produced by the microorganism in the raw materials in parts by mass, and sequentially adding the talcum powder into a supersonic jet mill, and sieving to prepare a mixture A of the degradable polymer powder, the epoxy resin powder, the unitary polyamide resin powder and the talcum powder produced by the microorganism;
s3, primary stirring: adding the mixture A obtained in the step S2 in the crushing process into a reaction kettle, stirring, adding lactide and lactic acid, and uniformly stirring to obtain a mixture B;
s4, continuing stirring: sequentially adding a catalyst and a modifier in the preliminary stirring in the step S3, stirring, and adding a thickening agent, a compatilizer, a coupling agent and a toughening agent until the materials are uniformly mixed to obtain a mixture C;
s5, stirring again: adding the film-forming aid into the mixture C in the step S4, continuously stirring, and adding the bactericide to prepare a mixture D;
s6, forming the degradable biopolymer material: and (5) adding the mixture D obtained in the step (S5) into a double-screw extruder for melt extrusion granulation, and cooling and forming to obtain the degradable biopolymer material.
And step S2, in the crushing process, the model of the crusher is DF-25A, the rotating speed is 2840r/min, the fineness is 60-200 meshes, the power is 2000W, and the crushed material is sieved by a sieve of 80-100 meshes.
And S4, in the process of continuous stirring, sequentially adding the catalyst and the modifier in the preliminary stirring in the step S3, stirring for 11min at the temperature of 80 ℃, adding the thickening agent, the compatilizer, the coupling agent and the toughening agent, and stirring for 15min at the temperature of 120 ℃.
In the step S5, the mixture is stirred again for 11min at 120 ℃.
Step S6, in the step of forming the degradable biological high molecular material, the extrusion temperature of the double-screw extruder is 240 ℃, and the extrusion speed is 120-160 r/min.
Example II
A synthesis process of a degradable biopolymer material comprises the following components in parts by weight: 50 parts of degradable macromolecules produced by microorganisms, 40 parts of epoxy resin, 20 parts of unitary polyamide resin, 25 parts of lactide, 20 parts of lactic acid, 10 parts of talcum powder, 8 parts of film-forming auxiliary agent, 5 parts of catalyst, 3 parts of modifier, 5 parts of thickener, 2 parts of compatilizer, 5 parts of coupling agent, 3 parts of toughening agent and 5 parts of bactericide.
The microorganism produced degradable macromolecule is one or more of microorganism polyester, polylactic acid, microorganism polysaccharide and copolymer of 3-hydroxybutyrate and 3-hydroxyvalerate, and the film-forming assistant is at least one of propylene glycol butyl ether and propylene glycol methyl ether acetate.
The catalyst is one or two of homogeneous catalyst, acid, alkali, soluble transition metal compound and peroxide catalyst, and the heterogeneous catalyst is one or more of solid acid catalyst, organic base catalyst, metal oxide catalyst, complex catalyst, rare earth catalyst, molecular sieve catalyst, biological catalyst and nano catalyst.
The thickening agent is one or more of methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, acrylic acid and methacrylic acid, and the coupling agent is one or more of organic chromium complex, silanes, titanates and aluminate compounds.
The bactericide is an inorganic bactericide and an organic bactericide, the inorganic bactericide is at least one of sulfur powder, lime sulfur, copper sulfate, mercury bichloride, calbodol solution and copper hydroxide and cuprous oxide, and the organic bactericide is at least one of amobam, sodium diformate, ziram, zineb, mancozeb and thiram.
The preparation method of the degradable biopolymer material comprises the following steps:
s1, weighing the raw materials in parts by mass: weighing 50 parts of microorganism-produced degradable macromolecules, 40 parts of epoxy resin, 20 parts of unitary polyamide resin, 25 parts of lactide, 20 parts of lactic acid, 10 parts of talcum powder, 8 parts of film-forming assistant, 5 parts of catalyst, 3 parts of modifier, 5 parts of thickener, 2 parts of compatilizer, 5 parts of coupling agent, 3 parts of toughening agent and 5 parts of bactericide in sequence according to the parts by mass of the raw materials;
s2, crushing: s1, weighing the degradable polymer, the epoxy resin and the unitary polyamide resin produced by the microorganism in the raw materials in parts by mass, and sequentially adding the talcum powder into a supersonic jet mill, and sieving to prepare a mixture A of the degradable polymer powder, the epoxy resin powder, the unitary polyamide resin powder and the talcum powder produced by the microorganism;
s3, primary stirring: adding the mixture A obtained in the step S2 in the crushing process into a reaction kettle, stirring, adding lactide and lactic acid, and uniformly stirring to obtain a mixture B;
s4, continuing stirring: sequentially adding a catalyst and a modifier in the preliminary stirring in the step S3, stirring, and adding a thickening agent, a compatilizer, a coupling agent and a toughening agent until the materials are uniformly mixed to obtain a mixture C;
s5, stirring again: adding the film-forming aid into the mixture C in the step S4, continuously stirring, and adding the bactericide to prepare a mixture D;
s6, forming the degradable biopolymer material: and (5) adding the mixture D obtained in the step (S5) into a double-screw extruder for melt extrusion granulation, and cooling and forming to obtain the degradable biopolymer material.
And step S2, in the crushing process, the model of the crusher is DF-25A, the rotating speed is 2840r/min, the fineness is 60-200 meshes, the power is 2000W, and the crushed material is sieved by a sieve of 80-100 meshes.
And S4, in the process of continuous stirring, sequentially adding the catalyst and the modifier in the preliminary stirring in the step S3, stirring for 15min at 120 ℃, adding the thickening agent, the compatilizer, the coupling agent and the toughening agent, and stirring for 25min at 150 ℃.
In the step S5, the mixture is stirred for 15min at 160 ℃ during the stirring again.
Step S6, in the step of forming the degradable biological high molecular material, the extrusion temperature of the double-screw extruder is 300 ℃, and the extrusion speed is 120-160 r/min.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A synthesis process of a degradable biopolymer material is characterized by comprising the following components in parts by weight: 40-50 parts of degradable polymer produced by microorganism, 30-40 parts of epoxy resin, 10-20 parts of unitary polyamide resin, 15-25 parts of lactide, 10-20 parts of lactic acid, 6-10 parts of talcum powder, 4-8 parts of film-forming additive, 3-5 parts of catalyst, 1-3 parts of modifier, 2-5 parts of thickener, 1-2 parts of compatilizer, 3-5 parts of coupling agent, 2-3 parts of flexibilizer and 1-5 parts of bactericide.
2. The process for synthesizing a degradable biopolymer material according to claim 1, wherein: the microorganism produced degradable high polymer is one or more of microorganism polyester, polylactic acid, microorganism polysaccharide and a copolymer of 3-hydroxybutyrate and 3-hydroxyvalerate, and the film-forming assistant is at least one of propylene glycol butyl ether and propylene glycol methyl ether acetate.
3. The process for synthesizing a degradable biopolymer material according to claim 1, wherein: the catalyst is a homogeneous catalyst which comprises one or two of acid, alkali, soluble transition metal compound and peroxide catalyst, and the heterogeneous catalyst comprises one or more of solid acid catalyst, organic base catalyst, metal oxide catalyst, complex catalyst, rare earth catalyst, molecular sieve catalyst, biocatalyst and nano catalyst.
4. The process for synthesizing a degradable biopolymer material according to claim 1, wherein: the thickening agent is one or more of methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, acrylic acid and methacrylic acid, and the coupling agent is one or more of organic chromium complex, silanes, titanates and aluminate compounds.
5. The process for synthesizing a degradable biopolymer material according to claim 1, wherein: the bactericide is an inorganic bactericide and an organic bactericide, the inorganic bactericide is at least one of sulfur powder, lime sulfur, copper sulfate, mercury bichloride, calbodol solution, copper hydroxide and cuprous oxide, and the organic bactericide is at least one of amobam, sodium diquat, ziram, zineb, mancozeb and thiram.
6. The process for synthesizing a degradable biopolymer material according to any one of claims 1-5, wherein the preparation method of the degradable biopolymer material comprises the following steps:
s1, weighing the raw materials in parts by mass: sequentially weighing a microorganism-produced degradable macromolecule, epoxy resin, unitary polyamide resin, lactide, lactic acid, talcum powder, a film-forming auxiliary agent, a catalyst, a modifier, a thickening agent, a compatilizer, a coupling agent, a toughening agent and a bactericide according to the mass parts of the raw materials;
s2, crushing: s1, weighing the degradable polymer, the epoxy resin and the unitary polyamide resin produced by the microorganism in the raw materials in parts by mass, and sequentially adding the talcum powder into a supersonic jet mill, and sieving to prepare a mixture A of the degradable polymer powder, the epoxy resin powder, the unitary polyamide resin powder and the talcum powder produced by the microorganism;
s3, primary stirring: adding the mixture A obtained in the step S2 in the crushing process into a reaction kettle, stirring, adding lactide and lactic acid, and uniformly stirring to obtain a mixture B;
s4, continuing stirring: sequentially adding a catalyst and a modifier in the preliminary stirring in the step S3, stirring, and adding a thickening agent, a compatilizer, a coupling agent and a toughening agent until the materials are uniformly mixed to obtain a mixture C;
s5, stirring again: adding the film-forming aid into the mixture C in the step S4, continuously stirring, and adding the bactericide to prepare a mixture D;
s6, forming the degradable biopolymer material: and (5) adding the mixture D obtained in the step (S5) into a double-screw extruder for melt extrusion granulation, and cooling and forming to obtain the degradable biopolymer material.
7. The process for synthesizing a degradable biopolymer material according to claim 6, wherein: and S2, in the crushing, the type of the crusher is DF-25A, the rotating speed is 2840r/min, the fineness is 60-200 meshes, the power is 2000W, and the crusher is sieved by 80-100 meshes.
8. The process for synthesizing a degradable biopolymer material according to claim 6, wherein: and S4, in the process of continuous stirring, adding the catalyst and the modifier in sequence in the step S3 and the preliminary stirring, stirring for 11-15min at the temperature of 80-120 ℃, adding the thickening agent, the compatilizer, the coupling agent and the toughening agent, and stirring for 15-25min at the temperature of 120-150 ℃.
9. The process for synthesizing a degradable biopolymer material according to claim 6, wherein: in the step S5, stirring again, stirring is carried out for 11-15min at the temperature of 120-160 ℃.
10. The process for synthesizing a degradable biopolymer material according to claim 6, wherein: in the step S6 and the step of forming the degradable biopolymer material, the extrusion temperature of the twin-screw extruder is 240-300 ℃, and the extrusion rate is 120-160 r/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101760037A (en) * | 2008-12-23 | 2010-06-30 | 金发科技股份有限公司 | Completely degraded plant powder modified thermoplastics composite material and preparation method thereof |
| CN103497529A (en) * | 2013-09-12 | 2014-01-08 | 青岛龙梅机电技术有限公司 | Environment-friendly degradable biological high polymer material |
| CN109912951A (en) * | 2019-04-08 | 2019-06-21 | 安徽律正科技信息服务有限公司 | A kind of novel degradable high molecular material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760037A (en) * | 2008-12-23 | 2010-06-30 | 金发科技股份有限公司 | Completely degraded plant powder modified thermoplastics composite material and preparation method thereof |
| CN103497529A (en) * | 2013-09-12 | 2014-01-08 | 青岛龙梅机电技术有限公司 | Environment-friendly degradable biological high polymer material |
| CN109912951A (en) * | 2019-04-08 | 2019-06-21 | 安徽律正科技信息服务有限公司 | A kind of novel degradable high molecular material and preparation method thereof |
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Application publication date: 20210115 |