CN113637235A - Full-biodegradable starch material and preparation method thereof - Google Patents
Full-biodegradable starch material and preparation method thereof Download PDFInfo
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- CN113637235A CN113637235A CN202110750156.1A CN202110750156A CN113637235A CN 113637235 A CN113637235 A CN 113637235A CN 202110750156 A CN202110750156 A CN 202110750156A CN 113637235 A CN113637235 A CN 113637235A
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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
- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
- C08L3/02—Starch; Degradation products thereof, e.g. dextrin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
-
- 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
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/20—Carboxylic acid amides
-
- 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
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- 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
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
Abstract
The application discloses a full-biodegradable starch material and a preparation method thereof, wherein the full-biodegradable starch material comprises the following components in percentage by mass: 40-70% of starchy raw material, 10-40% of glycerol complex, 2-10% of limestone and 0-30% of degradable high polymer material. The glycerol complex comprises glycerol and at least one of formamide, ethanolamine, fatty acid sucrose polyester, glycerol mono-fatty acid ester, citric acid, epoxy triglyceride, and polyethylene glycol. The starch material is used as a main raw material, the defect of strong water absorption of the starch material is effectively overcome by matching with the glycerol complex, the rigidity, the thermal stability and the processing performance of the starch material are effectively improved by matching with limestone, and the full-biodegradable starch material with good mechanical strength, water resistance and plasticizing performance can be obtained by blending and modifying with other degradable high polymer materials.
Description
Technical Field
The application relates to the technical field of degradable materials, in particular to a full-biodegradable starch material and a preparation method thereof.
Background
Since the existing plastics are hard to decompose in natural environment to cause 'white pollution' and cause serious harm to the ecological environment, the development of fully biodegradable plastics is needed.
The traditional starch mixed petroleum-based plastic is prepared by blending starch with petroleum-based plastics such as PE (polyethylene), PVC (polyvinyl chloride) and the like, belongs to non-completely degradable plastics essentially, and the non-degradable part after disintegration is difficult to recover, so that the problem of white pollution is aggravated and the starch mixed petroleum-based plastic is eliminated in the market. Patent application No. CN201910391126.9, entitled "a lignocellulose-starch degradable plastic and a preparation method thereof", discloses that lignocellulose is used for reinforcing starch, but the cellulose needs to be chemically modified, and chemical waste and waste water are generated in the process; the patent application No. CN03141982.8 is named as a full-biodegradable starch material and a preparation method thereof, the patent utilizes a pure physical mixing method to prepare starch degradation particles by using simple raw materials, but has the problems of longer plasticizing time, softer material, relatively poorer strength and the like, and has certain limitation on industrial application.
Disclosure of Invention
The application provides a full-biodegradable starch material and a preparation method thereof, which can obtain the full-biodegradable starch material with good mechanical strength, processability and degradability.
The application provides a full-biodegradable starch material, which comprises the following components in percentage by mass: starchy material (formula (C)6H10O5)nMolecular weight of 50000-60000, 10-40% of glycerol complex, and limestone (CaCO)3) 2-10% of degradable high polymer material and 0-30% of degradable high polymer material. According to the method, the glycerol complex is added into the starchy raw material, so that the fluidity of a melt generated by the interaction between the molecules of the starchy raw material can be improved, and then the plasticized granules are prepared.
Optionally, in some embodiments of the present application, the starchy material is a non-edible starchy material, such as tuber starch (e.g., sweet potato, tapioca, banana, etc.) and wild starch (e.g., acorn, golden steel head, palm, etc.), and the viscosity of the non-edible starchy material varies less than the viscosity of the edible starchy material, which can increase the mechanical strength of the material.
Optionally, in some embodiments of the present application, the glycerol complex comprises glycerol, and at least one of organic amines, esters, organic acids, and alcohols.
Alternatively, in some embodiments herein, the organic amine comprises formamide or ethanolamine.
Optionally, in some embodiments herein, the esters include fatty acid sucrose polyesters, mono-fatty glycerides, or epoxy triglycerides.
Optionally, in some embodiments herein, the organic acid comprises citric acid.
Optionally, in some embodiments herein, the alcohol comprises polyethylene glycol.
By compounding glycerol with organic amines (such as formamide or ethanolamine), esters (such as fatty acid sucrose polyester, glycerol mono-fatty acid ester or epoxy triglyceride), organic acids (such as citric acid), alcohols (such as polyethylene glycol) and the like, the defects of strong water absorption of the starchy raw material and easy migration, seepage and water absorption of the glycerol are effectively overcome.
Optionally, in some embodiments of the present application, the mass percentage of the glycerol in the glycerol complex may be 40 to 90%, or 50 to 80%, or 60 to 70%.
Optionally, in some embodiments of the present application, the limestone comprises micro limestone or nano limestone. Limestone is added, so that the rigidity, thermal stability and processability of the starchy raw material are effectively improved.
Optionally, in some embodiments of the present application, the particle size of the limestone is 6 to 30 μm, or 10 to 25 μm, or 15 to 20 μm.
Optionally, in some embodiments of the present disclosure, the particle size of the nano limestone may be 10 to 100nm, 20 to 80nm, or 30 to 60 nm.
Optionally, in some embodiments of the present application, the degradable polymer material includes polylactide (structure shown in formula I), polybutylene succinate (structure shown in formula II), polycaprolactone (structure shown in formula III), or polybutylene adipate terephthalate (structure shown in formula IV). The starch raw material and the glycerol complex are modified by blending with other degradable high polymer materials, so that the full-biodegradable starch material with good mechanical strength, water resistance and plasticizing performance is obtained.
Optionally, in some embodiments of the application, the molecular weight of the degradable polymer material may be 60000 to 1000000, may also be 100000 to 800000, and may also be 300000 to 600000.
Correspondingly, the application also provides a preparation method of the full-biodegradable starch material, which comprises the following steps:
(1) mixing 40-70% of starchy raw material, 10-40% of glycerol complex, 2-10% of limestone and 0-30% of degradable high polymer material to obtain a premixed material;
(2) and mixing the premixed materials to obtain the fully biodegradable starch material.
Alternatively, in some embodiments of the present application, a method for preparing a fully biodegradable starch material comprises: (S1) stirring 40-70% of starchy raw material, 10-40% of glycerol complex, 2-10% of limestone and 0-30% of degradable high polymer material in a high-speed mixer to obtain a premixed material;
(S2) subjecting the premixed material to a first mixing in an internal mixer;
(S3) mixing the mixing product obtained in the step (S2) for the second time in a double-screw extruder, and then extruding and granulating to obtain the fully biodegradable starch material.
The fully biodegradable starch material is processed by combining the internal mixer and the double-screw extruder, so that the problem that the material is difficult to agglomerate and discharge is effectively solved, the material mixing and plasticizing efficiency is improved, and the performance of the fully biodegradable starch material is improved.
Optionally, in some embodiments herein, the glycerol complex comprises glycerol and at least one of formamide, ethanolamine, fatty acid sucrose polyesters, glycerol mono fatty acid esters, citric acid, epoxy triglycerides, polyethylene glycol.
Optionally, in some embodiments of the present application, the limestone comprises micro limestone or nano limestone.
Optionally, in some embodiments of the present application, the degradable polymeric material comprises polylactide, polybutylene succinate, polycaprolactone, or polybutylene adipate terephthalate.
Optionally, in some embodiments of the present disclosure, in the step (S1), the stirring temperature may be 20 to 120 ℃, or 30 to 110 ℃, or 40 to 100 ℃.
Optionally, in some embodiments of the present application, in the step (S1), the stirring time may be 10 to 30 minutes, 15 to 25 minutes, or 20 minutes.
Optionally, in some embodiments of the present application, in the step (S2), the mixing temperature may be 100 to 150 ℃, may also be 110 to 140 ℃, and may also be 120 to 130 ℃.
Optionally, in some embodiments of the present application, in the step (S2), the mixing time may be 10 to 60 minutes, 20 to 50 minutes, or 30 to 40 minutes.
Optionally, in some embodiments of the present application, in the step (S3), the mixing temperature may be 120 to 170 ℃, or 130 to 160 ℃, or 140 to 150 ℃.
Optionally, in some embodiments of the present application, the production efficiency is 100 kg to 1000 kg per hour.
The fully biodegradable starch material is prepared by a simple melt blending method, and has the following beneficial effects:
(1) the starch raw material is used as a main raw material and is matched with the glycerol complex, so that the defects of strong water absorption of the starch raw material and easy migration and exudation and water absorption of glycerol are effectively overcome;
(2) the addition of limestone can effectively improve the rigidity, thermal stability and processability of the starchy raw material.
(3) The fully biodegradable starch material has the advantages that the fully biodegradable starch material expands the performance range of the fully biodegradable starch material, such as the mechanical strength, the plasticizing performance, the water resistance, the degradation performance and the like of the material, and better meets the technical requirements of the industries such as packaging, non-woven fabrics, plastic products, foam materials and the like through blending modification with other degradable high polymer materials;
(4) the preparation method has simple process, solves the problem that the material is difficult to feed due to agglomeration, improves the material mixing and plasticizing efficiency, and improves the performance of the full-biodegradable starch material.
Detailed Description
The technical solutions in the embodiments of the present application will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The application provides a full-biodegradable starch material and a preparation method thereof. The following are detailed below. It should be noted that the following description of the embodiments is not intended to limit the preferred order of the embodiments.
The first embodiment,
This example provides a method for preparing a fully biodegradable starch material.
(1) Stirring 700g of starchy raw material, 100g of micron limestone (10 microns), 300g of glycerol and 50g of formamide in a high-speed mixer at 20 ℃ for 15 minutes, and uniformly mixing to obtain a premix;
(2) mixing the premixed materials in an internal mixer at 100 ℃;
(3) and (3) directly conveying the mixed product obtained in the step (2) to a double-screw extruder after mixing, and mixing, extruding and granulating in the double-screw extruder at 140 ℃ to obtain the fully biodegradable starch material.
The obtained full-biodegradable starch material is subjected to performance test (test standard GB/T1040.2-2006), and the performance is shown in Table 1.
Example II,
This example provides a method for preparing a fully biodegradable starch material.
(1) Stirring 700g of starchy material, 60g of micron limestone (20 microns), 300g of glycerol, 100g of polyethylene glycol (with the polymerization degree of 1700) and 100g of polycaprolactone (with the molecular weight of 70000) in a high-speed mixer at 80 ℃ for 25 minutes, and uniformly mixing to obtain a premixed material;
(2) mixing the premixed materials in an internal mixer at 140 ℃;
(3) and (3) directly conveying the mixed product obtained in the step (2) to a double-screw extruder after mixing, and mixing, extruding and granulating in the double-screw extruder at 140 ℃ to obtain the full-biodegradable starchiness raw material.
The obtained full-biodegradable starch material is subjected to performance test (test standard GB/T1040.2-2006), and the performance is shown in Table 1.
Example III,
This example provides a method for preparing a fully biodegradable starch material.
(1) Stirring 700g of starchy raw material, 50g of nano limestone (30nm), 300g of glycerol, 50g of fatty acid sucrose polyester, 50g of citric acid and 100g of polybutylene adipate terephthalate (molecular weight of 210000) in a high-speed mixer for 25 minutes and uniformly mixing to obtain a premixed material;
(2) mixing the premixed materials in an internal mixer at 130 ℃;
(3) and (3) directly conveying the mixed product obtained in the step (2) to a double-screw extruder after mixing, and mixing, extruding and granulating in the double-screw extruder at 130 ℃ to obtain the fully biodegradable starch material.
The obtained full-biodegradable starch material is subjected to performance test (test standard GB/T1040.2-2006), and the performance is shown in Table 1.
Example four,
This example provides a method for preparing a fully biodegradable starch material.
(1) Stirring 700g of starchy raw material, 30g of nano limestone (60nm), 300g of glycerol, 50g of ethanol amine, 50g of epoxy triglyceride and 100g of polybutylene succinate (molecular weight of 60000) in a high-speed mixer at 110 ℃ for 30 minutes, and uniformly mixing to obtain a premix;
(2) mixing the premixed materials in an internal mixer at 120 ℃;
(3) and (3) directly conveying the mixed product obtained in the step (2) to a double-screw extruder after mixing, and mixing, extruding and granulating in the double-screw extruder at 130 ℃ to obtain the fully biodegradable starch material.
The obtained full-biodegradable starch material is subjected to performance test (test standard GB/T1040.2-2006), and the performance is shown in Table 1.
TABLE 1 mechanical Properties of fully biodegradable starch materials
The fully biodegradable starch material prepared by the method has good mechanical strength and plasticizing performance, can be formed by processes such as injection molding, extrusion, blow molding, tape casting and the like, and is applied to packaging film materials, agricultural mulching films, injection molding/plastic uptake products, foam products, biomedical products and the like.
The fully biodegradable starch material and the preparation method thereof provided by the embodiments of the present application are described in detail above, and the principles and embodiments of the present application are illustrated herein by using specific examples, and the description of the above embodiments is only used to help understand the method and the core concept of the present application; meanwhile, for those skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and as described above, the content of the present specification should not be construed as a limitation to the present application.
Claims (10)
1. The fully biodegradable starch material is characterized by comprising the following components in percentage by mass: 40-70% of starchy raw material, 10-40% of glycerol complex, 2-10% of limestone and 0-30% of degradable high polymer material; wherein the glycerol complex comprises glycerol and at least one of organic amines, esters, organic acids and alcohols.
2. The fully biodegradable starch material according to claim 1, wherein the organic amine comprises formamide or ethanolamine; and/or the esters comprise fatty acid sucrose polyesters, glycerol mono fatty acid esters or epoxytriglycerides; and/or, the organic acid comprises citric acid; and/or, the alcohol comprises polyethylene glycol.
3. The fully biodegradable starch material according to claim 1, wherein the glycerol is present in the glycerol complex in an amount of 40-90% by weight.
4. The fully biodegradable starch material according to claim 1, wherein said limestone is micro limestone or nano limestone, said micro limestone having a particle size of 6-30 μm, said nano limestone having a particle size of 10-100 nm.
5. The fully biodegradable starch material according to claim 1, wherein the degradable polymer material comprises polylactide, polybutylene succinate, polycaprolactone or polybutylene adipate terephthalate, and the molecular weight of the degradable polymer material is 60000-1000000.
6. A preparation method of a full-biodegradable starch material is characterized by comprising the following steps:
(1) mixing 40-70% of starchy raw material, 10-40% of glycerol complex, 2-10% of limestone and 0-30% of degradable high polymer material to obtain a premixed material;
(2) and mixing the premixed materials to obtain the fully biodegradable starch material.
7. The glycerol complex comprises glycerol and at least one of organic amines, esters, organic acids and alcohols. The method for preparing the fully biodegradable starch material according to claim 6, wherein the organic amine comprises formamide or ethanolamine; and/or the esters comprise fatty acid sucrose polyesters, glycerol mono fatty acid esters or epoxytriglycerides; and/or, the organic acid comprises citric acid; and/or, the alcohol comprises polyethylene glycol.
8. The method for preparing the fully biodegradable starch material according to claim 6, wherein the limestone is micro limestone or nano limestone, the particle size of the micro limestone is 6-30 μm, and the particle size of the nano limestone is 10-100 nm.
9. The method for preparing the fully biodegradable starch material according to claim 6, wherein the degradable polymer material comprises polylactide, polybutylene succinate, polycaprolactone or polybutylene adipate terephthalate.
10. The preparation method of the fully biodegradable starch material according to claim 6, wherein in the step (1), the stirring temperature is 20-120 ℃; and/or the stirring time is 10-30 minutes; in the step (2), firstly, the premixed material is mixed for the first time in an internal mixer, the mixing temperature is 100 ℃ and 150 ℃, and the mixing time is 10-60 minutes; and then the mixed product is mixed for the second time in a double-screw extruder at the mixing temperature of 120-170 ℃, and the full-biodegradable starch material is obtained through the steps of extrusion and granulation.
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