CN116080053A - Preparation method of graphitized carbon nitride degradable biological plastic film - Google Patents
Preparation method of graphitized carbon nitride degradable biological plastic film Download PDFInfo
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- CN116080053A CN116080053A CN202310354359.8A CN202310354359A CN116080053A CN 116080053 A CN116080053 A CN 116080053A CN 202310354359 A CN202310354359 A CN 202310354359A CN 116080053 A CN116080053 A CN 116080053A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/28—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of blown tubular films, e.g. by inflation
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- 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
- C08K3/34—Silicon-containing compounds
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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Abstract
The invention discloses a preparation method of a graphitized carbon nitride degradable biological plastic film, which comprises the following steps: step one, synthesizing graphitized carbon nitride; step two, weighing poly adipic acid/butylene terephthalate, talcum powder and graphitized carbon nitride according to a proportion, and physically mixing uniformly; step three, adding the mixture obtained in the step two into a granulator for granulation to obtain master batches; and fourthly, adding the master batch into a film blowing machine to perform film blowing, and obtaining the yellowish graphitized carbon nitride degradable biological plastic film. Compared with the traditional plastic reinforcing agent, the water-gas barrier agent or the ultraviolet absorbent with single function, the graphitized carbon nitride is adopted as the novel auxiliary agent, has the characteristic of multifunction, can meet the requirement of the degradable biological plastic film on the auxiliary agent in practical application, and has practical significance for improving the problems of the degradable biological plastic film.
Description
Technical Field
The invention belongs to the technical field of biological plastic films, and particularly relates to a preparation method of a graphitized carbon nitride degradable biological plastic film.
Background
The use of conventional polyolefin plastics in large quantities causes serious environmental pollution. The biodegradable plastic film (such as polylactic acid (PLA), polybutylene adipate/terephthalate (PBAT) and the like) is used for replacing the difficult-to-degrade polyolefin plastic, so that the problem of white pollution can be solved from the source, and the green sustainable development goal is met. However, the degradable biological plastic film has the problems of poor mechanical property, weak water-gas barrier capability, poor photo-oxidative aging resistance and the like, and limits the application of the degradable biological plastic film in some fields. To ameliorate these problems, it is common practice to add functional aids to degradable plastic films. For example, the introduction of inorganic nano materials such as hydrotalcite, montmorillonite and graphene can play a role in enhancing the mechanical property and the water vapor barrier property of plastics, but the inorganic materials have the problems of poor compatibility, easy aggregation, defect generation and the like. In the aspect of photo-oxidation aging resistance, benzophenone, benzotriazole, derivatives thereof and the like can be used as organic ultraviolet absorbers to effectively absorb ultraviolet rays in sunlight and convert the ultraviolet rays into heat energy, so that the degradable plastic film is reduced or prevented from photo-aging oxidation, and the service life is prolonged. However, these organic ultraviolet absorbers have problems such as insufficient stability and environmental pollution due to easy migration. Therefore, the application of the photo-oxidation resistant aging assistant has the defect. In summary, these conventional additives have a single function and have obvious disadvantages, and it is impossible to use one additive to obtain various modifications to the biodegradable plastic film. In view of the above, development and preparation of a novel multifunctional auxiliary agent are needed, and the novel auxiliary agent has the advantages of simple preparation, good stability, environmental friendliness, strong functionality and the like. The application of the multifunctional auxiliary agent can widen the application range of the biodegradable plastic film and reduce the use cost of the biodegradable plastic film.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a graphitized carbon nitride degradable biological plastic film, which can effectively improve the mechanical strength, the water-gas barrier capability and the photo-oxidation aging resistance of the degradable biological plastic film.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a preparation method of a graphitized carbon nitride degradable biological plastic film, which comprises the following steps:
step one, synthesizing graphitized carbon nitride;
step two, weighing poly adipic acid/butylene terephthalate, talcum powder and graphitized carbon nitride according to a proportion, and physically mixing uniformly;
step three, adding the mixture obtained in the step two into a granulator for granulation to obtain master batches;
and fourthly, adding the master batch into a film blowing machine to perform film blowing, and obtaining the yellowish graphitized carbon nitride degradable biological plastic film.
As a preferable technical scheme, the first step specifically includes the following steps:
s1, mixing and grinding the small organic molecules containing nitrogen and the template agent uniformly, wherein the mass ratio of the small organic molecules containing nitrogen to the template agent is 1:0.5-6;
s2, placing the mixture obtained after grinding of the S1 into a tube furnace protected by inert gas, carbonizing at a high temperature of between 550 and 600 ℃ for 2 to 6 h at a heating rate of between 1 and 3 ℃/min, and obtaining pale yellow solid powder, namely graphitized carbon nitride nano-sheets.
As a preferable technical scheme, the small nitrogen-containing organic molecule is one of urea, melamine and dicyandiamide.
As a preferable technical scheme, the template agent is one of ammonium chloride, ammonium sulfate and boric acid.
According to the preferable technical scheme, when the template agent is ammonium chloride or ammonium sulfate, graphitized carbon nitride products are directly obtained, and when the template agent is boric acid, the obtained products need to be washed with water, centrifuged and filtered to remove the boron trioxide, and graphitized carbon nitride is obtained after further drying.
As a preferable technical scheme, the inert gas is one of nitrogen and argon.
As the preferable technical scheme, the mass ratio of the poly (adipic acid)/the butylene terephthalate, the talcum powder and the graphitized carbon nitride is 1000:20 (1-20).
As a preferable technical scheme, the granulator is a double-screw granulator, and the melting temperature of the granulator is 190 ℃ and the rotating speed of the granulator is 100 r/min.
As a preferable technical scheme, the film blowing temperature of the film blowing machine is 190 ℃, and the thickness of the graphitized carbon nitride degradable biological plastic film is 25-40 mu m.
Graphitized carbon nitride (g-C) 3 N 4 ) The two-dimensional nano sheet is an inorganic polymer semiconductor, is of a two-dimensional sheet structure, and has good mechanical strength and ultraviolet absorption capacity. In addition, consider g-C 3 N 4 g-C 3 N 4 The surface is rich in-NH 2 Equal groups, with g-C 3 N 4 g-C as an auxiliary agent for degradable biological plastic films 3 N 4 on-NH 2 Can form hydrogen bond with-C=O group of degradable biological plastic film base molecule to make g-C 3 N 4 Can be uniformly and stably present in the plastic substrate. g-C 3 N 4 Good mechanical strength makes it possible to enhance the mechanical properties of plastics, g-C 3 N 4 The layered structure of the (C) can improve the water-gas barrier capability of the plastic, g-C 3 N 4 Has good absorption capability to ultraviolet light smaller than 400 and nm, and can play a role in resisting photo-oxidative aging of plastics. Compared with the traditional plastic reinforcing agent, the water-gas barrier additive or the ultraviolet absorbent with single function, the graphitized carbon nitride is adopted as the novel auxiliary agent, has the characteristic of multifunction, can meet the requirement of the degradable biological plastic film on the auxiliary agent in practical application, and can improveThe problems of degradation of the bio-plastic film are of practical significance.
Drawings
FIG. 1 is a powder X-ray diffraction pattern of graphitized carbon nitride obtained in example 1 and example 2 of the present invention.
FIG. 2 is a low power transmission mirror image of graphitized carbon nitride obtained in example 1 of the present invention.
FIG. 3 is a low power transmission mirror image of graphitized carbon nitride obtained in example 2 of the present invention.
Fig. 4 shows the diffuse reflection uv-vis absorption spectra of graphitized carbon nitrides obtained in examples 1 and 2 of the present invention.
FIG. 5 is an infrared spectrum of the degradable bio-plastic film obtained in application example 1 and application example 2.
FIG. 6 shows the UV-visible absorption spectra of the degradable bioplastic films obtained in comparative example, application example 1, and application example 2.
Description of the embodiments
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present invention, which is described by the following specific examples.
Examples
Weighing 5g of melamine and 20g of NH 4 Cl, was ground uniformly in a mortar. The mixture was placed in a tube furnace, nitrogen was introduced at a gas flow rate of 50 ml/min for 30 minutes, then the tube furnace was warmed from room temperature to 600 ℃ at a warming rate of 3 ℃/min for 4 hours, and after stopping heating, naturally cooled to room temperature, to give graphitized carbon nitride CN1 (2.4 g, yield 48%) as a pale yellow solid product. The X-ray diffraction diagram of CN1 is shown in FIG. 1, the low-magnification transmission electron microscope diagram is shown in FIG. 2, and the diffuse reflection ultraviolet visible absorption spectrum is shown in FIG. 4.
Examples
Weigh 20g melamine and 5g NH 4 Cl, was ground uniformly in a mortar. Placing the mixture in a tube furnace, introducing nitrogen at a gas flow rate of 50 ml/min for 30 min, then heating the tube furnace from room temperature to 600 ℃ at a heating rate of 3 ℃/min for 4 hours, stopping heating, and naturally cooling to room temperature to obtain pale yellow solidThe bulk product graphitized carbon nitride CN2 (12 g, 60% yield). The X-ray diffraction diagram of CN2 is shown in figure 1, the low-magnification transmission electron microscope diagram is shown in figure 3, and the diffuse reflection ultraviolet visible absorption spectrum is shown in figure 4.
Examples
Weighing 5g dicyandiamide and 20g NH 4 Cl, was ground uniformly in a mortar. The mixture was placed in a tube furnace, nitrogen was introduced at a gas flow rate of 50 ml/min for 30 minutes, then the tube furnace was warmed from room temperature to 600 ℃ at a warming rate of 3 ℃/min for 4 hours, and after stopping heating, it was naturally cooled to room temperature to obtain a pale yellow solid product CN3.
Comparative example
1 kg polybutylene adipate/terephthalate (PBAT), 20g of talcum powder are weighed and physically mixed uniformly. And adding the mixture into a double-screw granulator for granulation, wherein the melting temperature of the granulator is 190 ℃, and the rotating speed is 100 r/min, so as to obtain the PBAT master batch. And (3) adding the prepared PBAT master batch into a film blowing machine for film blowing, wherein the film blowing temperature is 190 ℃, and finally, the milky PBAT degradable biological plastic film with the thickness of 25-40 mu m is obtained. The PBAT film was tested for mechanical properties, uv absorption and moisture barrier.
Application example 1
1 kg Poly (adipic acid)/polybutylene terephthalate (PBAT), 20g of talcum powder and 2.5g of CN1 are weighed and physically mixed uniformly. And adding the mixture into a double-screw granulator for granulation, wherein the melting temperature of the granulator is 190 ℃, and the rotating speed is 100 r/min, so as to obtain CN1-PBAT master batch. And (3) adding the prepared CN1-PBAT master batch into a film blowing machine for film blowing, wherein the film blowing temperature is 190 ℃, and finally, the yellowish CN1-PBAT degradable biological plastic film with the thickness of 25-40 mu m is obtained. The mechanical properties, ultraviolet absorption capacity and moisture blocking capacity of the CN1-PBAT film were tested.
Application example 2
1 kg Poly (adipic acid)/polybutylene terephthalate (PBAT), 20g of talcum powder and 2.5g of CN2 are weighed and physically mixed uniformly. And adding the mixture into a double-screw granulator for granulation, wherein the melting temperature of the granulator is 190 ℃, and the rotating speed is 100 r/min, so as to obtain CN2-PBAT master batch. And (3) adding the prepared CN1-PBAT master batch into a film blowing machine for film blowing, wherein the film blowing temperature is 190 ℃, and finally, the yellowish CN2-PBAT degradable biological plastic film with the thickness of 25-40 mu m is obtained. The mechanical properties, ultraviolet absorption capacity and moisture blocking capacity of the CN2-PBAT film were tested.
Application example 3
1 kg Poly (adipic acid)/polybutylene terephthalate (PBAT), 20g of talcum powder and 5g of CN1 are weighed and physically mixed uniformly. And adding the mixture into a double-screw granulator for granulation, wherein the melting temperature of the granulator is 190 ℃, and the rotating speed is 100 r/min, so as to obtain CN1-PBAT-2 master batch. And (3) adding the prepared CN1-PBAT-2 master batch into a film blowing machine for film blowing, wherein the film blowing temperature is 190 ℃, and finally, the yellowish CN1-PBAT-2 degradable biological plastic film with the thickness of 25-40 mu m is obtained. The mechanical properties, ultraviolet absorption capacity and moisture blocking capacity of the CN1-PBAT-2 film were tested.
Parameters of the degradable plastic biofilms prepared in comparative example, application example 1 and application example 2 are shown in table 1.
TABLE 1
The infrared spectra of the degradable biological plastic films obtained in application example 1 and application example 2 are shown in fig. 5, and the ultraviolet-visible absorption spectra of the degradable biological plastic films obtained in comparative example, application example 1 and application example 2 are shown in fig. 6. It can be seen that the absorption intensity of the PBAT doped with CN1 and CN2 to the ultraviolet part is obviously higher than that of the pure PBAT film, and compared with the pure PBAT film, each parameter of the PBAT film doped with CN1 and CN2 is obviously improved.
While the foregoing embodiments have been described in detail and with reference to the present invention, it will be apparent to one skilled in the art that modifications and improvements can be made based on the disclosure without departing from the spirit and scope of the invention.
Claims (9)
1. The preparation method of the graphitized carbon nitride degradable biological plastic film is characterized by comprising the following steps of:
step one, synthesizing graphitized carbon nitride;
step two, weighing poly adipic acid/butylene terephthalate, talcum powder and graphitized carbon nitride according to a proportion, and physically mixing uniformly;
step three, adding the mixture obtained in the step two into a granulator for granulation to obtain master batches;
and fourthly, adding the master batch into a film blowing machine to perform film blowing, and obtaining the yellowish graphitized carbon nitride degradable biological plastic film.
2. The method for preparing the graphitized carbon nitride degradable biological plastic film according to claim 1, wherein the first step specifically comprises the following steps:
s1, mixing and grinding the small organic molecules containing nitrogen and the template agent uniformly, wherein the mass ratio of the small organic molecules containing nitrogen to the template agent is 1:0.5-6;
s2, placing the mixture obtained after grinding of the S1 into a tube furnace protected by inert gas, carbonizing at a high temperature of between 550 and 600 ℃ for 2 to 6 h at a heating rate of between 1 and 3 ℃/min, and obtaining pale yellow solid powder, namely graphitized carbon nitride nano-sheets.
3. The method for preparing the graphitized carbon nitride degradable biological plastic film according to claim 2, wherein the small nitrogen-containing organic molecule is one of urea, melamine and dicyandiamide.
4. The method for preparing the graphitized carbon nitride degradable biological plastic film according to claim 2, wherein the template agent is one of ammonium chloride, ammonium sulfate and boric acid.
5. The method for preparing the graphitized carbon nitride degradable biological plastic film according to claim 4, wherein when the template agent is ammonium chloride or ammonium sulfate, graphitized carbon nitride products are directly obtained, and when the template agent is boric acid, the obtained products need to be washed with water, centrifuged, filtered to remove diboron trioxide, and further dried to obtain graphitized carbon nitride.
6. The method for preparing a graphitized carbon nitride degradable biological plastic film according to claim 2, wherein the inert gas is one of nitrogen and argon.
7. The preparation method of the graphitized carbon nitride degradable biological plastic film according to claim 1, wherein the mass ratio of poly (butylene adipate/terephthalate), talcum powder and graphitized carbon nitride is 1000:20 (1-20).
8. The method for preparing a graphitized carbon nitride degradable biological plastic film according to claim 1, wherein the granulator is a double-screw granulator, and the melting temperature of the granulator is 190 ℃ and the rotating speed of the granulator is 100 r/min.
9. The method for preparing the graphitized carbon nitride degradable biological plastic film according to claim 1, wherein the film blowing temperature of the film blowing machine is 190 ℃, and the thickness of the graphitized carbon nitride degradable biological plastic film is 25-40 μm.
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| CN113234304A (en) * | 2021-05-11 | 2021-08-10 | 贵州省材料产业技术研究院 | Biodegradable film material and preparation method of film |
| CN115109287A (en) * | 2022-07-21 | 2022-09-27 | 西南交通大学 | Preparation method and application of photodegradable nano carbon nitride-polyvinyl chloride composite film |
| CN115368602A (en) * | 2022-08-09 | 2022-11-22 | 山东农业大学 | Preparation method of carbon nitride based green light catalytic preservative film |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010280156A (en) * | 2009-06-05 | 2010-12-16 | Lintec Corp | Gas barrier film and method for manufacturing the same |
| CN108102391A (en) * | 2018-01-16 | 2018-06-01 | 镇江市荣发塑料制品有限公司 | g-C3N4Compound edible antibacterial film and preparation method thereof |
| CN112495412A (en) * | 2020-10-30 | 2021-03-16 | 江苏大学 | Porous thin-layer graphite phase carbon nitride and preparation method and application thereof |
| CN113186656A (en) * | 2021-04-29 | 2021-07-30 | 北京石油化工学院 | Carbon nitride-polyvinyl alcohol composite antibacterial film and preparation method and application thereof |
| CN113234304A (en) * | 2021-05-11 | 2021-08-10 | 贵州省材料产业技术研究院 | Biodegradable film material and preparation method of film |
| CN115109287A (en) * | 2022-07-21 | 2022-09-27 | 西南交通大学 | Preparation method and application of photodegradable nano carbon nitride-polyvinyl chloride composite film |
| CN115368602A (en) * | 2022-08-09 | 2022-11-22 | 山东农业大学 | Preparation method of carbon nitride based green light catalytic preservative film |
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