Preparation method and application of a bi-parental lignin interfacial compatibilizer
By preparing an amphiphilic lignin interfacial compatibilizer, the problem of poor interfacial compatibility of biodegradable plastic film materials was solved, the mechanical and processing properties of the composite film were improved, and low-cost, high-performance sustainable development was achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- HUAZHONG AGRI UNIV
- Filing Date
- 2025-01-15
- Publication Date
- 2026-08-04
AI Technical Summary
Existing biodegradable plastic film materials suffer from problems such as poor thermal stability, low mechanical properties, weak aging resistance, and high production costs. Furthermore, poor interfacial compatibility during the addition of fillers affects the processing and application performance of the materials.
An amphiphilic lignin interface compatibilizer was prepared by reacting lignin with alcohol compounds under specific conditions. The compatibilizer was then mixed with materials such as PBAT, PLA, PHA, PCL, and PBS to prepare a composite film.
It significantly improves the intermolecular interfacial compatibility of composite films, enhances their mechanical properties, and reduces production costs, which aligns with the concept of green and sustainable development.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of interface compatibilizer technology, and in particular to a method for preparing and applying an amphiphilic lignin interface compatibilizer. Background Technology
[0002] Traditional non-biodegradable plastics, due to their widespread use, cause white pollution, posing a potential threat to human health and the environment. Therefore, biodegradable plastics are increasingly seen as an effective solution to replace traditional non-biodegradable plastics. However, existing biodegradable membrane materials have many shortcomings, such as poor thermal stability, low mechanical properties, weak aging resistance, and high production costs. To address these issues, adding fillers to biodegradable plastic films has become a common improvement method. However, poor interfacial compatibility is the biggest bottleneck in the process of adding fillers, affecting the material's processing performance and final application performance. By introducing interfacial compatibility agents, the interfacial compatibility between the filler and the matrix can be effectively improved, thereby improving the processability and applicability of the plastic. Traditional interfacial compatibility agents are divided into three categories: hydrophilic, oleophilic, and amphiphilic. Although these interfacial compatibility agents can improve the material's performance to some extent, their modification effect is usually limited, and they may cause environmental harm during use, which is inconsistent with the concept of green and sustainable development. Therefore, developing an interfacial compatibility agent derived from wood biomass is crucial for promoting the production of low-cost, high-performance biodegradable membrane materials that meet green environmental standards.
[0003] The purpose of this invention is to provide an amphiphilic lignin interfacial compatibilizer, its preparation method, and its application. The compatibilizer of this invention is used to improve the compatibility between molecules, thereby improving the mechanical properties of composite films. This method uses lignin as a raw material to prepare an amphiphilic compatibilizer, which enables the composite film to have good mechanical properties while achieving sustainable development. Summary of the Invention
[0004] The purpose of this invention is to provide a method for preparing and applying an amphiphilic lignin interfacial compatibilizer. This amphiphilic lignin interfacial compatibilizer can significantly improve the interfacial compatibility between two phase molecules, thereby improving the overall performance of the composite film and enabling the composite film to be used in fields such as mulch film, packaging film, and vest bags.
[0005] To achieve the above objectives, the present invention provides a method for preparing an amphiphilic lignin interface compatibilizer, comprising the following steps: reacting lignin with an alcohol compound, cooling to room temperature after the reaction, adding the reactants dropwise into deionized water with a pH of 2-7, stirring for 10-60 min, centrifuging, washing, collecting the solid, and freeze-drying for 24-96 h to obtain the amphiphilic lignin interface compatibilizer.
[0006] Furthermore, the lignin includes one or more of sulfate lignin, alkali lignin, organic solvent lignin, DES lignin, ionic liquid lignin, and enzymatically hydrolyzed lignin.
[0007] Further, the alcohol compounds include one or more of polyethylene glycol methyl ether methacrylate, polyethylene glycol methyl ether acrylate, polyethylene glycol methacrylate, polyethylene glycol diacrylate, glycerol, ethylene glycol, or polyethylene glycol and its derivative polyethylene glycol polymers.
[0008] Furthermore, the ratio of lignin to alcohol compounds is 1:10-50 (g / g).
[0009] Furthermore, the reaction conditions are: 100~180℃ for 1-6 h.
[0010] This invention also provides a method for preparing a composite film with an added amphiphilic lignin interfacial compatibilizer, which is prepared according to the above method and includes the following steps: Step 1, Masterbatch preparation: The dried raw materials are mixed evenly with PBAT, PLA, PHA, PCL or PBS and amphiphilic lignin interface compatibilizer in a high-speed mixer, and the masterbatch is prepared in a twin-screw extruder at 120-170℃. Step 2, hot pressing of composite film: hot pressing the composite masterbatch at 140-190℃ and 2~25 MPa for 1-5 min to obtain composite film; Step 3, blow molding: The masterbatch is placed in a blow molding machine at a temperature of 130-180℃ to form a blown film.
[0011] Furthermore, the raw materials in step 1 include one or more of the following: straw powder, lignin, bamboo powder, wood powder, calcium carbonate, talc, humic acid, and biochar. The mass ratio of the raw materials to PBAT, PLA, PHA, PCL, and PBS is 5:95-70:30, and the amphiphilic lignin interface compatibilizer accounts for 1-6% of the total mass of the masterbatch.
[0012] The present invention also provides a composite film with an added amphiphilic lignin interface compatibilizer, which is prepared by the above preparation method.
[0013] The present invention also provides the application of a composite film with an added amphiphilic lignin interface compatibilizer in mulch films, packaging bags, and vest bags.
[0014] The advantages and positive effects of the preparation method and application of the amphiphilic lignin interface compatibilizer described in this invention are as follows: 1. The amphiphilic lignin interfacial compatibilizer in this invention can significantly improve the intermolecular interfacial compatibility, thereby improving the mechanical properties of the composite film.
[0015] 2. The raw materials used in this invention to prepare the amphiphilic lignin interface compatibilizer are green, low in cost, and low in pollution, which is of great significance to sustainable development.
[0016] The technical solution of the present invention will be further described in detail below through embodiments. Detailed Implementation
[0017] The technical solution of the present invention will be further described below through embodiments.
[0018] Unless otherwise defined, the technical or scientific terms used in this invention shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention pertains.
[0019] Unless otherwise defined, the instruments, equipment and reagents used in this invention are all commercially available.
[0020] Example 1 A composite film with added amphiphilic lignin interface compatibilizer was prepared by 50 parts PBAT, 50 parts bamboo powder and 1% amphiphilic lignin interface compatibilizer.
[0021] 1) 50 parts by weight of bamboo powder; 2) 50 parts by weight of PBAT; 3) 1% amphiphilic lignin interface compatibilizer.
[0022] The preparation method of the amphiphilic lignin interface compatibilizer is as follows: The organic solvent lignin was reacted with ethylene glycol (g / g) at a ratio of 1:10 and 0.01-0.1g of acidic catalyst at 100-180℃ for 4-6 h. After the reaction was completed, the mixture was cooled to room temperature, and the reactants were added dropwise to deionized water with a pH of 2-7. The mixture was then centrifuged, washed, and freeze-dried for 48 h to obtain an amphiphilic lignin interface compatibilizer.
[0023] A method for preparing a composite film with an added amphiphilic lignin interfacial compatibilizer includes the following steps: Step 1: Take 50 parts bamboo powder, 50 parts PBAT, and 1% amphiphilic lignin interface compatibilizer to prepare masterbatch via twin-screw extrusion. The twin-screw processing parameters are as follows: heating temperature set at 130~150℃, roller speed set at 20~35r / min, and extrusion times of 1-5 times.
[0024] Step 2: The masterbatch is hot-pressed into a film in a hot press to obtain a bamboo powder-based composite film material with added amphiphilic lignin interface compatibilizer. The hot press processing parameters are as follows: heating temperature set to 130~155℃, pressure set to 1-25 MPa, and running time set to 1~5 min.
[0025] Step 3: The masterbatch is blown into a film using a blown film machine to obtain a bamboo powder-based composite film with an added amphiphilic lignin interface compatibilizer. The processing parameters of the blown film machine are as follows: heating temperature is set to 130~155℃, and preheating time is set to 35~50min.
[0026] Example 2 A composite film with added amphiphilic lignin interface compatibilizer was prepared by 50 parts of PBAT, 50 parts of corn stalk powder and 3% of amphiphilic lignin interface compatibilizer.
[0027] 1) 50 parts by weight of corn stalk powder; 2) 50 parts by weight of PBAT; 3) 3% amphiphilic lignin interface compatibilizer.
[0028] The preparation method of the amphiphilic lignin interface compatibilizer is as follows: Alkali lignin was reacted with polyethylene glycol (g / g) at a ratio of 1:50 and 0.02-0.1g of acidic catalyst at 100-180℃ for 6 hours. After the reaction was completed, the mixture was cooled to room temperature, and the reactants were added dropwise to deionized water with a pH of 2-7. The mixture was then centrifuged, washed, and freeze-dried for 48 hours to obtain an amphiphilic lignin interface compatibilizer.
[0029] The preparation steps of the composite film are the same as in Example 1.
[0030] Example 3 A composite film with added amphiphilic lignin interface compatibilizer was prepared by 50 parts PBAT, 50 parts cotton stalk powder and 4% amphiphilic lignin interface compatibilizer.
[0031] 1) 50 parts by weight of cotton stalk powder; 2) 50 parts by weight of PBAT; 3) 4% amphiphilic lignin interface compatibilizer.
[0032] The preparation method of the amphiphilic lignin interface compatibilizer is as follows: lignin, an organic solvent, is reacted with ethylene glycol (g / g) at a ratio of 1:20 and 0.01-0.05g of acidic catalyst at 100-180℃ for 6 h. After the reaction is completed, the mixture is cooled to room temperature, and the reactants are added dropwise to deionized water with a pH of 2-7. The mixture is then centrifuged, washed, and freeze-dried for 48 h to obtain the amphiphilic lignin interface compatibilizer.
[0033] The preparation steps of the composite film are the same as in Example 1.
[0034] Example 4 A composite film with added amphiphilic lignin interface compatibilizer was prepared by 50 parts PBAT, 50 parts calcium carbonate powder and 3% amphiphilic lignin interface compatibilizer.
[0035] 1) 50 parts by weight of calcium carbonate powder; 2) 50 parts by weight of PBAT; 3) 3% amphiphilic lignin interface compatibilizer.
[0036] The preparation methods for the amphiphilic lignin interface compatibilizer and composite film are the same as in Example 1.
[0037] Example 5 A composite film with added amphiphilic lignin interface compatibilizer was prepared by 50 parts PBAT, 50 parts talc powder and 3% amphiphilic lignin interface compatibilizer.
[0038] 1) 50 parts by weight of talc powder; 2) 50 parts by weight of PBAT; 3) 3% amphiphilic lignin interface compatibilizer.
[0039] The preparation methods for the amphiphilic lignin interface compatibilizer and composite film are the same as in Example 1.
[0040] Comparative Example 1 A bamboo powder-based PBAT composite film is prepared by mass percentage from 50 parts bamboo powder and 50 parts PBAT.
[0041] (1) 50 parts by weight of bamboo powder; (2) 50 parts by weight of PBAT.
[0042] The method for preparing composite thin films includes the following steps: Step 1: Take 50 parts bamboo powder and 50 parts PBAT and prepare masterbatch through twin-screw extrusion. The processing parameters of the twin-screw are as follows: heating temperature is set to 130~150℃, roller speed is set to 20~35r / min, and the number of passes is 1-5.
[0043] Step 2: Hot press the masterbatch into a film in a hot press. The hot press processing parameters are as follows: heating temperature set to 130~155℃, pressure set to 1-25 MPa, and running time set to 1~5 min.
[0044] Step 3: Blow-molde the masterbatch into a film using a blown film extruder. The processing parameters for the blown film extruder are as follows: heating temperature set to 130~155℃, preheating time set to 35~50min.
[0045] Comparative Example 2 A bamboo powder-based composite membrane material with added hydrophilic interfacial compatibilizer is prepared from 50 parts bamboo powder, 50 parts PBAT and 3% glycerol.
[0046] (1) 50 parts by weight of bamboo powder; (2) 50 parts by weight of PBAT; (3) 3% glycerin.
[0047] The method for preparing composite thin films includes the following steps: Step 1: Take 50 parts bamboo powder, 50 parts PBAT, and 3% glycerol to prepare masterbatch through twin-screw extrusion. The processing parameters of the twin-screw extrusion are as follows: heating temperature set at 130~150℃, roller speed set at 20~35r / min, and extrusion times of 1-5 times.
[0048] Step 2: Hot press the masterbatch into a film in a hot press. The hot press processing parameters are as follows: heating temperature set to 130~155℃, pressure set to 1-25 MPa, and running time set to 1~5 min.
[0049] Step 3: Blow-molde the masterbatch into a film using a blown film extruder. The processing parameters for the blown film extruder are as follows: heating temperature set to 130~155℃, preheating time set to 35~50min.
[0050] Comparative Example 3 A bamboo powder-based composite membrane material with added oleophilic compatibilizer is prepared by using 50 parts bamboo powder, 50 parts PBAT and 3% dioctyl phthalate (DOP).
[0051] (1) 50 parts by weight of bamboo powder; (2) 50 parts by weight of PBAT; (3) 3% DOP.
[0052] The method for preparing composite thin films includes the following steps: Step 1: Take 50 parts bamboo powder, 50 parts PBAT, and 3% DOP to prepare masterbatch through twin-screw extrusion. The processing parameters of the twin-screw extrusion are as follows: heating temperature is set to 130~150℃, roller speed is set to 20~35r / min, and the number of passes is 1-5.
[0053] Step 2: Hot press the masterbatch into a film in a hot press. The hot press processing parameters are as follows: heating temperature set to 130~155℃, pressure set to 1-25 MPa, and running time set to 1~5 min.
[0054] Step 3: Blow-molde the masterbatch into a film using a blown film extruder. The processing parameters for the blown film extruder are as follows: heating temperature set to 130~155℃, preheating time set to 35~50min.
[0055] Comparative Example 4 A calcium carbonate powder-based composite film is prepared by mixing 50 parts of PBAT and 50 parts of calcium carbonate powder.
[0056] 1) 50 parts by weight of calcium carbonate powder; 2) 50 parts by weight of PBAT.
[0057] The method for preparing composite thin films includes the following steps: Step 1: Take 50 parts of calcium carbonate powder and 50 parts of PBAT and prepare masterbatch by twin-screw extrusion. The processing parameters of the twin-screw are as follows: heating temperature is set to 130~150℃, roller speed is set to 20~35r / min, and the number of passes is 1-5.
[0058] Step 2: Hot press the masterbatch into a film in a hot press. The hot press processing parameters are as follows: heating temperature set to 130~155℃, pressure set to 1-25 MPa, and running time set to 1~5 min.
[0059] Step 3: Blow-molde the masterbatch into a film using a blown film extruder. The processing parameters for the blown film extruder are as follows: heating temperature set to 130~155℃, preheating time set to 35~50min.
[0060] Comparative Example 5 A stone powder-based composite film was prepared from 50 parts of PBAT and 50 parts of talc powder.
[0061] 1) 50 parts by weight of talc powder; 2) 50 parts by weight of PBAT.
[0062] The method for preparing composite thin films includes the following steps: Step 1: Take 50 parts of talc powder and 50 parts of PBAT and prepare masterbatch through twin-screw extrusion. The processing parameters of the twin-screw extrusion are as follows: heating temperature is set to 130~150℃, roller speed is set to 20~35r / min, and the number of passes is 1-5.
[0063] Step 2: Hot press the masterbatch into a film in a hot press. The hot press processing parameters are as follows: heating temperature set to 130~155℃, pressure set to 1-25 MPa, and running time set to 1~5 min.
[0064] Step 3: Blow-molde the masterbatch into a film using a blown film extruder. The processing parameters for the blown film extruder are as follows: heating temperature set to 130~155℃, preheating time set to 35~50min.
[0065] The experimental setups for Examples 1-5 and Comparative Examples 1-5 are shown in Table 1: Table 1 Experimental Setup
[0066] Performance testing The composite films prepared in Examples 1-5 and Comparative Examples 1-5 were subjected to performance tests. The tensile strength, elastic modulus and elongation at break are shown in Table 2.
[0067] Table 2. Mechanical property test results of the examples and comparative examples
[0068] After adding an amphiphilic lignin interface compatibilizer, the elongation at break of the composite film materials in Examples 1, 2, 3, 4, and 5 increased to 771.3%, 813.7%, 748.3%, 79.8%, and 125.9%, respectively, which were 18.1%, 24.5%, 14.6%, 56.1%, and 9.6% higher than those without the amphiphilic modifier (Comparative Examples 1, 4, and 5).
[0069] Compared with Comparative Example 1, Example 2 added an amphiphilic lignin-based interface compatibilizer. The tensile strength, elastic modulus and elongation at break of Example 2 were all improved, indicating that the amphiphilic lignin interface compatibilizer can significantly improve the interfacial compatibility of the composite film, thereby improving the mechanical properties of the film.
[0070] Compared with Comparative Examples 2 and 3, Comparative Example 2 added a hydrophilic compatibilizer, Comparative Example 3 added an oleophilic compatibilizer, and Example 2 added an amphiphilic lignin interface compatibilizer. The tensile strength, elastic modulus, and elongation at break of Example 2 were all improved, indicating that compared with hydrophilic (or oleophilic) compatibilizers, amphiphilic lignin interface compatibilizers can significantly improve the interfacial compatibility of the composite film and enhance its overall performance. This further demonstrates the effectiveness and superiority of amphiphilic lignin interface compatibilizers.
[0071] Therefore, the present invention adopts the above-mentioned preparation method and application of an amphiphilic lignin interface compatibilizer. This amphiphilic lignin interface compatibilizer can significantly improve the interfacial compatibility between two phase molecules, thereby improving the comprehensive performance of the composite film, enabling the composite film to be used in fields such as mulch film, packaging bags, vests, or food preservation film.
[0072] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the technical solutions of the present invention, and these modifications or equivalent substitutions cannot cause the modified technical solutions to deviate from the spirit and scope of the technical solutions of the present invention.
Claims
1. A method for preparing a composite film with an added amphiphilic lignin interfacial compatibilizer, characterized in that, Includes the following steps: Step 1, Masterbatch preparation: Mix the raw materials, PBAT and amphiphilic lignin interface compatibilizer evenly in a high-speed mixer, and prepare the masterbatch in a twin-screw extruder at 120-170℃. Step 2, hot pressing of composite film: hot pressing the masterbatch at 140-190℃ and 2~25 MPa for 1-5 min to obtain composite film; In step 1, the raw materials are calcium carbonate and / or talc, and the mass ratio of the raw materials to PBAT is (5-70):(30-95). The amphiphilic lignin interface compatibilizer accounts for 1-6% of the total mass of the masterbatch. The preparation method of the amphiphilic lignin interface compatibilizer includes the following steps: reacting lignin with alcohol compounds and acidic catalysts under the following conditions: reacting at 100~180℃ for 1-6 h; cooling to room temperature after the reaction is completed; adding the reactants dropwise into deionized water with pH 2-7; stirring for 10-60 min; centrifuging, washing, collecting the solid; and freeze-drying for 24-96 h to obtain the amphiphilic lignin interface compatibilizer. The alcohol compounds include one or more of glycerol, ethylene glycol, or polyethylene glycol.
2. The method for preparing a composite film with an added amphiphilic lignin interfacial compatibilizer according to claim 1, characterized in that: The lignin includes one or more of sulfate lignin, alkali lignin, organic solvent lignin, DES lignin, ionic liquid lignin, and enzymatically hydrolyzed lignin.
3. The method for preparing a composite film with an added amphiphilic lignin interfacial compatibilizer according to claim 1, characterized in that: The ratio of lignin to alcohol compounds is 1g:(10-50)g.
4. A composite film incorporating an amphiphilic lignin interfacial compatibilizer, characterized in that, It is prepared according to any one of claims 1-3.
5. The application of the composite film with added amphiphilic lignin interface compatibilizer as described in claim 4 in mulch film, packaging bags, and food preservation film.