CN113248877A - Antioxidant starch-based biodegradable material and preparation method thereof - Google Patents
Antioxidant starch-based biodegradable material and preparation method thereof Download PDFInfo
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- CN113248877A CN113248877A CN202110384911.9A CN202110384911A CN113248877A CN 113248877 A CN113248877 A CN 113248877A CN 202110384911 A CN202110384911 A CN 202110384911A CN 113248877 A CN113248877 A CN 113248877A
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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
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
Abstract
The invention relates to the technical field of degradable materials, in particular to an antioxidant starch-based biodegradable material and a preparation method thereof. The preparation raw materials of the antioxidant starch-based biodegradable material comprise, by weight: 50-70 parts of a copolymer of butanediol adipate and butanediol terephthalate; 15-30 parts of starch; 5-9 parts of an antioxidant plasticizer; 0.1-3 parts of an auxiliary agent; 2-10 parts of water; the antioxidant plasticizer is selected from one or more of sorbitol, mannitol and erythritol. According to the invention, a plasticizing system of glycerin and water is replaced by adding the biological-based plasticizer (one or more of sorbitol, mannitol and erythritol) with oxidation resistance, so that the discoloration phenomenon of starch in a high-temperature process is inhibited, the biodegradation performance and the mechanical property of the material are not influenced, and the intrinsic oxidation resistance of the material is realized.
Description
Technical Field
The invention relates to the technical field of degradable materials, in particular to an antioxidant starch-based biodegradable material and a preparation method thereof.
Background
With continuous popularization of plastic forbidden commands in various places, biodegradable materials gradually become a hot point of research, and are continuously developed in the fields of injection molding, plastic uptake and films, and particularly in the field of disposable films, the application of the biodegradable materials is wider. However, the cost of biodegradable materials is 2-3 times higher than that of general-purpose plastics such as polyethylene, polypropylene, etc. Therefore, in order to reduce the cost, bio-based materials such as starch, cellulose and the like are mostly adopted for filling, and the plasticizer and the like are adopted for realizing uniform dispersion so as to prepare the biodegradable materials, and the biodegradable materials are widely applied to the fields of disposable garbage bags, shopping bags and the like.
For example, the biodegradable material is mostly prepared by using a copolymer (PBAT) of butylene adipate and butylene terephthalate as a main body, starch as a filling material, and a mixture of glycerol and water as a plasticizer.
However, the biodegradable material of PBAT/starch described above, which uses glycerol as a plasticizer, causes yellowing of starch during processing due to the high temperature during processing, thereby affecting the appearance of the material. And if the conventional antioxidant is added for preventing the yellowing of the starch, the biodegradation performance and the mechanical property of the material are influenced. If the conventional antioxidant is not added, but a non-bio-based filling material such as titanium dioxide and the like is added for covering, the cost of the material is increased.
Disclosure of Invention
Based on the above, the invention provides an oxidation-resistant starch-based biodegradable material. The yellowing of starch is not easy to cause, and the biodegradation performance and the mechanical property of the material are not influenced.
The technical scheme is as follows:
an oxidation-resistant starch-based biodegradable material comprises the following preparation raw materials in parts by weight:
the antioxidant plasticizer is selected from one or more of sorbitol, mannitol and erythritol.
In one embodiment, the raw materials for preparing the oxidation-resistant starch-based biodegradable material comprise the following components in parts by weight:
in one embodiment, the copolymer of butylene adipate and butylene terephthalate has a melt index of 1g/10min to 10g/10min at 190 ℃.
In one embodiment, the starch is selected from one or more of corn starch, potato starch and wheat starch.
In one embodiment, the auxiliary agent is selected from one or more of a compatilizer, a opener and a lubricant.
In one embodiment, the compatibilizing agent is basf ADR-4468.
In one embodiment, the lubricant is selected from one or more of PEG400 and erucamide.
In one embodiment, the opening agent is talc.
In one embodiment, the raw materials for preparing the antioxidant starch-based biodegradable material comprise, by weight:
the invention also provides a preparation method of the antioxidant starch-based biodegradable material.
The technical scheme is as follows:
a preparation method of an oxidation-resistant starch-based biodegradable material comprises the following steps:
mixing an antioxidant plasticizer, a copolymer of butylene adipate and butylene terephthalate, starch, an auxiliary agent and water to obtain a mixture;
extruding and granulating the mixture at the extrusion temperature of 150 ℃ and 170 ℃ to obtain granules;
and blowing a film on the particles, wherein the temperature of a neck mold is 150-170 ℃.
In one embodiment, the moisture content of the granules is controlled to be 3 ‰ ± 1 ‰ before the granules are blown with a film.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, a plasticizing system of glycerin and water is replaced by adding the biological base plasticizer (one or more of sorbitol, mannitol and erythritol) with oxidation resistance, so that the discoloration phenomenon of starch in a high-temperature process is inhibited, the biodegradation performance and the mechanical property of the material are not influenced, and the white oxidation-resistant starch-based biodegradable material is prepared by adjusting the content of each formula. The intrinsic oxidation resistance of the material is realized.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
An oxidation-resistant starch-based biodegradable material comprises the following preparation raw materials in parts by weight:
the antioxidant plasticizer is selected from one or more of sorbitol, mannitol and erythritol.
Preferably, the raw materials for preparing the oxidation-resistant starch-based biodegradable material comprise the following components in parts by weight:
preferably, the copolymer of butylene adipate and butylene terephthalate has a melt index of 1g/10min to 10g/10min at 190 ℃. Is favorable for meeting the requirement of raw material film blowing.
Preferably, the starch is selected from one or more of corn starch, potato starch and wheat starch. Further preferred is corn starch and/or wheat starch.
Preferably, the auxiliary agent is selected from one or more of a compatilizer, an opening agent and a lubricant.
Preferably, the compatibilizer is basf ADR-4468. The addition of the compatilizer is beneficial to improving the melt strength of the raw materials.
Preferably, the lubricant is selected from one or more of PEG400 and erucamide. The addition of the lubricant facilitates uniform dispersion of the components.
Preferably, the opening agent is talc. The addition of the opening agent is beneficial to improving the surface roughness of the film and preventing the blown film from being bonded together.
Further preferably, the talcum powder is superfine talcum powder, and the particle size is 100nm-1000 nm.
Preferably, the raw materials for preparing the antioxidant starch-based biodegradable material comprise, by weight:
preferably, the raw materials for preparing the antioxidant starch-based biodegradable material comprise, by weight:
preferably, the raw materials for preparing the antioxidant starch-based biodegradable material comprise, by weight:
it is understood that the above-mentioned oxidation-resistant starch-based biodegradable material is an oxidation-resistant starch-based biodegradable film.
A preparation method of an oxidation-resistant starch-based biodegradable material comprises the following steps:
mixing an antioxidant plasticizer, a copolymer of butylene adipate and butylene terephthalate, starch, an auxiliary agent and water to obtain a mixture;
extruding and granulating the mixture at the extrusion temperature of 150 ℃ and 170 ℃ to obtain granules;
and blowing a film on the particles, wherein the temperature of a neck mold is 150-170 ℃.
It can be understood that, when the raw materials are mixed, the antioxidant plasticizer can be dissolved in a part of water, and after being completely dissolved, the antioxidant plasticizer is added into the composition of the copolymer of the butylene adipate and the butylene terephthalate, the starch, the auxiliary agent and the rest of water, and the mixture is obtained by stirring and dispersing at a high speed.
The mixture is extruded by a double screw and then granulated, and the extrusion temperature is controlled at 150 ℃ and 170 ℃ to obtain the granules. Drying the granulated particles in an oven at 80 ℃ for 4 hours to ensure that the water content of the particles is 3 +/-1 per mill. It is understood that moisture content refers to the mass percentage of moisture in the granules.
Then, a single-screw film blowing machine is used for carrying out film blowing verification on the particles, and the temperature of a neck ring is set at 150-170 ℃.
The following examples and comparative examples are further described below, and the starting materials used in the following examples can be commercially available, unless otherwise specified, and the equipment used therein can be commercially available, unless otherwise specified. Specifically, the method comprises the following steps:
a copolymer of butylene adipate and butylene terephthalate (PBAT) was purchased from tunghe blue mountain and was model number TH 801T.
The particle size of the superfine talcum powder is 100nm-1000 nm.
Example 1
The embodiment provides an antioxidant starch-based biodegradable material and a preparation method thereof, and the preparation method comprises the following steps:
step 1, weighing the following raw materials in parts by weight:
step 2 preparation of antioxidant starch-based biodegradable material
Sorbitol is dissolved in a part of water, and after the sorbitol is completely dissolved, the sorbitol is added into a composition of butylene adipate-butylene terephthalate copolymer (PBAT), corn starch, basf ADR-4368, PEG400, superfine talcum powder and the rest water, and the mixture is stirred and dispersed at a high speed to obtain a mixture.
The mixture is extruded by a double screw and then granulated, and the extrusion temperature is controlled at 150 ℃ and 170 ℃ to obtain the granules. Drying the granulated particles in an oven at 80 ℃ for 4 hours to ensure that the water content of the particles is 3 +/-1 per mill.
And blowing the dried particles into a film by a single-screw film blowing machine, wherein the temperature of a neck mold is 150-170 ℃, and obtaining the white antioxidant starch-based biodegradable material.
Example 2
The embodiment provides an antioxidant starch-based biodegradable material and a preparation method thereof, and the main difference from the embodiment 1 is that the antioxidant plasticizer is different, and the steps are as follows:
step 1, weighing the following raw materials in parts by weight:
step 2 preparation of antioxidant starch-based biodegradable material
Dissolving mannitol in part of water, adding into a composition of butylene adipate-butylene terephthalate copolymer (PBAT), corn starch, Bass ADR-4368, PEG400, superfine talcum powder and residual water after completely dissolving, and stirring at high speed to disperse to obtain a mixture.
The mixture is extruded by a double screw and then granulated, and the extrusion temperature is controlled at 150 ℃ and 170 ℃ to obtain the granules. Drying the granulated particles in an oven at 80 ℃ for 4 hours to ensure that the water content of the particles is 3 +/-1 per mill.
And blowing the dried particles into a film by a single-screw film blowing machine, wherein the temperature of a neck mold is 150-170 ℃, and obtaining the white antioxidant starch-based biodegradable material.
Example 3
The embodiment provides an antioxidant starch-based biodegradable material and a preparation method thereof, and the main difference from the embodiment 1 is that the antioxidant plasticizer is different, and the steps are as follows:
step 1, weighing the following raw materials in parts by weight:
step 2 preparation of antioxidant starch-based biodegradable material
Firstly dissolving erythritol in a part of water, adding the erythritol into a composition of butylene adipate-butylene terephthalate copolymer (PBAT), corn starch, basf ADR-4368, PEG400, superfine talcum powder and the rest water after completely dissolving the erythritol, and stirring and dispersing at a high speed to obtain a mixture.
The mixture is extruded by a double screw and then granulated, and the extrusion temperature is controlled at 150 ℃ and 170 ℃ to obtain the granules. Drying the granulated particles in an oven at 80 ℃ for 4 hours to ensure that the water content of the particles is 3 +/-1 per mill.
And blowing the dried particles into a film by a single-screw film blowing machine, wherein the temperature of a neck mold is 150-170 ℃, and obtaining the white antioxidant starch-based biodegradable material.
Example 4
The embodiment provides an oxidation-resistant starch-based biodegradable material and a preparation method thereof, and the main difference from the embodiment 3 is that starch is different, and the steps are as follows:
step 1, weighing the following raw materials in parts by weight:
step 2 preparation of antioxidant starch-based biodegradable material
Firstly dissolving erythritol in a part of water, adding into a composition of butylene adipate-butylene terephthalate copolymer (PBAT), potato starch, BASF ADR-4368, PEG400, superfine talcum powder and the rest water after completely dissolving, and stirring at high speed to disperse to obtain a mixture.
The mixture is extruded by a double screw and then granulated, and the extrusion temperature is controlled at 150 ℃ and 170 ℃ to obtain the granules. Drying the granulated particles in an oven at 80 ℃ for 4 hours to ensure that the water content of the particles is 3 +/-1 per mill.
And blowing the dried particles into a film by a single-screw film blowing machine, wherein the temperature of a neck mold is 150-170 ℃, and obtaining the white antioxidant starch-based biodegradable material.
Example 5
The embodiment provides an oxidation-resistant starch-based biodegradable material and a preparation method thereof, and the main difference from the embodiment 3 is that starch is different, and the steps are as follows:
step 1, weighing the following raw materials in parts by weight:
step 2 preparation of antioxidant starch-based biodegradable material
Firstly dissolving erythritol in a part of water, adding the erythritol into a composition of butylene adipate-butylene terephthalate copolymer (PBAT), wheat starch, basf ADR-4368, PEG400, superfine talcum powder and the rest water after completely dissolving the erythritol, and stirring and dispersing at a high speed to obtain a mixture.
The mixture is extruded by a double screw and then granulated, and the extrusion temperature is controlled at 150 ℃ and 170 ℃ to obtain the granules. Drying the granulated particles in an oven at 80 ℃ for 4 hours to ensure that the water content of the particles is 3 +/-1 per mill.
And blowing the dried particles into a film by a single-screw film blowing machine, wherein the temperature of a neck mold is 150-170 ℃, and obtaining the white antioxidant starch-based biodegradable material.
Example 6
The embodiment provides an antioxidant starch-based biodegradable material and a preparation method thereof, and the main difference from the embodiment 1 is that the dosage of each raw material is different, and the steps are as follows:
step 1, weighing the following raw materials in parts by weight:
step 2 preparation of antioxidant starch-based biodegradable material
Firstly dissolving erythritol in a part of water, adding the erythritol into a composition of butylene adipate-butylene terephthalate copolymer (PBAT), corn starch, basf ADR-4368, PEG400, superfine talcum powder and the rest water after completely dissolving the erythritol, and stirring and dispersing at a high speed to obtain a mixture.
The mixture is extruded by a double screw and then granulated, and the extrusion temperature is controlled at 150 ℃ and 170 ℃ to obtain the granules. Drying the granulated particles in an oven at 80 ℃ for 4 hours to ensure that the water content of the particles is 3 +/-1 per mill.
And blowing the dried particles into a film by a single-screw film blowing machine, wherein the temperature of a neck mold is 150-170 ℃, and obtaining the white antioxidant starch-based biodegradable material.
Comparative example 1
The comparative example provides an antioxidant starch-based biodegradable material and a preparation method thereof, and the main difference from example 3 is that the antioxidant plasticizer is different, and the steps are as follows:
step 1, weighing the following raw materials in parts by weight:
step 2 preparation of antioxidant starch-based biodegradable material
Mixing glycerol, polybutylene adipate and butylene terephthalate copolymer (PBAT), corn starch, basf ADR-4368, PEG400, superfine talcum powder and water, and stirring at high speed to disperse to obtain a mixture.
The mixture is extruded by a double screw and then granulated, and the extrusion temperature is controlled at 150 ℃ and 170 ℃ to obtain the granules. Drying the granulated particles in an oven at 80 ℃ for 4 hours to ensure that the water content of the particles is 3 +/-1 per mill.
And blowing the dried particles into a film by a single-screw film blowing machine, wherein the temperature of a neck mold is 150-170 ℃, and obtaining the white antioxidant starch-based biodegradable material.
Comparative example 2
The comparative example provides an antioxidant starch-based biodegradable material and a preparation method thereof, and is mainly different from comparative example 1 in that an antioxidant is also added, and the steps are as follows:
step 1, weighing the following raw materials in parts by weight:
step 2 preparation of antioxidant starch-based biodegradable material
Mixing glycerol, antioxidant 1010, polybutylene adipate-butylene terephthalate copolymer (PBAT), corn starch, basf ADR-4368, PEG400, superfine talcum powder and water, and stirring at high speed to disperse to obtain a mixture.
The mixture is extruded by a double screw and then granulated, and the extrusion temperature is controlled at 150 ℃ and 170 ℃ to obtain the granules. Drying the granulated particles in an oven at 80 ℃ for 4 hours to ensure that the water content of the particles is 3 +/-1 per mill.
And blowing the dried particles into a film by a single-screw film blowing machine, wherein the temperature of a neck mold is 150-170 ℃, and obtaining the white antioxidant starch-based biodegradable material.
Comparative example 3
The comparative example provides an antioxidant starch-based biodegradable material and a preparation method thereof, and the main difference from example 3 is that the antioxidant plasticizer is different, and the steps are as follows:
step 1, weighing the following raw materials in parts by weight:
step 2 preparation of antioxidant starch-based biodegradable material
Dissolving xylitol in a part of water, adding the dissolved xylitol into a composition of butylene adipate-butylene terephthalate copolymer (PBAT), corn starch, basf ADR-4368, PEG400, superfine talcum powder and the rest water, and stirring at a high speed to disperse to obtain a mixture.
The mixture is extruded by a double screw and then granulated, and the extrusion temperature is controlled at 150 ℃ and 170 ℃ to obtain the granules. Drying the granulated particles in an oven at 80 ℃ for 4 hours to ensure that the water content of the particles is 3 +/-1 per mill.
And blowing the dried particles into a film by a single-screw film blowing machine, wherein the temperature of a neck mold is 150-170 ℃, and obtaining the white antioxidant starch-based biodegradable material.
Comparative example 4
The comparative example provides an antioxidant starch-based biodegradable material and a preparation method thereof, and the main difference from example 3 is that the antioxidant plasticizer is different, and the steps are as follows:
step 1, weighing the following raw materials in parts by weight:
step 2 preparation of antioxidant starch-based biodegradable material
Dissolving maltose in part of water, adding into the composition of butylene adipate-butylene terephthalate copolymer (PBAT), corn starch, Bass ADR-4368, PEG400, superfine pulvis Talci and the rest water, stirring at high speed, and dispersing to obtain mixture.
The mixture is extruded by a double screw and then granulated, and the extrusion temperature is controlled at 150 ℃ and 170 ℃ to obtain the granules. Drying the granulated particles in an oven at 80 ℃ for 4 hours to ensure that the water content of the particles is 3 +/-1 per mill.
And blowing the dried particles into a film by a single-screw film blowing machine, wherein the temperature of a neck mold is 150-170 ℃, and obtaining the white antioxidant starch-based biodegradable material.
Testing
The performance of the oxidation resistant starch-based biodegradable materials prepared in the above examples and comparative examples was tested according to the following test methods, and the test results are shown in table 1:
the tensile strength test refers to GB/T1040-;
the elongation at break test is referred to GB/T1040-;
the flexural modulus test is referred to GB/T9341-2008;
the impact strength test refers to GB/T1843-2008;
the melt index test is referred to GB/T3682-.
TABLE 1
As can be seen from Table 1, compared with the glycerol plasticizing system of comparative example 1, the addition of the antioxidant plasticizers of examples 1-6 has little influence on the mechanical properties of the starch-based biodegradable material, but in the aspect of chromaticity test, the antioxidant plasticizer is obviously reduced in the b value, which indicates that the oxidation degree of the material is reduced in the processing process, and indicates that sorbitol, mannitol and erythritol can inhibit the discoloration phenomenon of starch in the high-temperature process on the basis of not influencing the mechanical properties of the material, and the materials can be biodegraded without influencing the overall biodegradation performance of the material, and the three antioxidant plasticizers have more remarkable effect on inhibiting the discoloration phenomenon of corn starch and wheat starch.
Comparative example 2 an antioxidant 1010 was added to the glycerin plasticizing system of comparative example 1, but the antioxidant performance was poor
Comparative examples 3 and 4 use materials having reducing properties such as maltose and xylitol, respectively, as antioxidant plasticizers, but it was found that corn starch is more easily oxidized at high temperature.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
3. the oxidation-resistant starch-based biodegradable material according to claim 2, wherein said copolymer of butylene adipate and butylene terephthalate has a melt index of 1g/10min to 10g/10min at 190 ℃.
4. The oxidation-resistant starch-based biodegradable material according to claim 1, wherein the starch is selected from one or more of corn starch, potato starch and wheat starch.
5. The oxidation-resistant starch-based biodegradable material according to any one of claims 1-4, wherein the auxiliary agent is selected from one or more of a compatibilizer, a opener, and a lubricant.
6. The oxidation-resistant starch-based biodegradable material according to claim 5, wherein said compatibilizer is basf ADR-4468.
7. The oxidation-resistant starch-based biodegradable material according to claim 5, wherein the lubricant is selected from one or more of PEG400 and erucamide.
8. The oxidation-resistant starch-based biodegradable material according to claim 5, wherein the opening agent is talc.
10. a method for preparing the oxidation-resistant starch-based biodegradable material according to any one of claims 1-9, comprising the steps of:
mixing an antioxidant plasticizer, a copolymer of butylene adipate and butylene terephthalate, starch, an auxiliary agent and water to obtain a mixture;
extruding and granulating the mixture at the extrusion temperature of 150 ℃ and 170 ℃ to obtain granules;
and blowing a film on the particles, wherein the temperature of a neck mold is 150-170 ℃.
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