CN115449165A - Environment-friendly flame-retardant polyvinyl chloride/graphene composite decorative film for rail transit - Google Patents
Environment-friendly flame-retardant polyvinyl chloride/graphene composite decorative film for rail transit Download PDFInfo
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- CN115449165A CN115449165A CN202211064488.5A CN202211064488A CN115449165A CN 115449165 A CN115449165 A CN 115449165A CN 202211064488 A CN202211064488 A CN 202211064488A CN 115449165 A CN115449165 A CN 115449165A
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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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- 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
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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- 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
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T30/00—Transportation of goods or passengers via railways, e.g. energy recovery or reducing air resistance
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Abstract
The invention discloses an environment-friendly flame-retardant polyvinyl chloride/graphene composite decorative film for rail transit, and relates to the technical field of decorative materials, the prepared flame-retardant enhanced graphene is compounded with polyvinyl chloride to prepare a polyvinyl chloride/graphene composite material, so that the flame retardant property of the polyvinyl chloride is effectively improved, and the environment friendliness of the polyvinyl chloride when the flame retardant property is exerted is improved; according to the invention, the prepared polyvinyl chloride/graphene composite material is adopted to process the rail transit decorative film, so that the good decorative function can be exerted, the flame retardant effect, the mechanical property and the like of the decorative film can be enhanced, the VOC emission in the use process of the decorative film is reduced, and the environmental protection property of the decorative film is improved, thereby being suitable for the rail transit environment.
Description
The technical field is as follows:
the invention relates to the technical field of decorative materials, in particular to an environment-friendly flame-retardant polyvinyl chloride/graphene composite decorative film for rail transit.
Background art:
with the rapid development of the rail transit industry in China in recent years, the environmental protection and aesthetic requirements of people on rail transit interior trim are higher and higher, the traditional paint coating process is difficult to meet the personalized requirements of modern interior trim design, and the environmental protection problem is increasingly highlighted by VOC (volatile organic compounds) emission in the paint coating process. Under the condition, the decorative film which is characterized by rich colors, simple and convenient picture manufacture, rapid construction and environmental protection is gradually popularized and applied to the rail transit interior decoration.
The polyvinyl chloride decorative film is a decorative material which is formed by calendering and compounding polyvinyl chloride serving as a raw material after a proper amount of auxiliary agent is added. Due to the characteristics of the molecular structure of polyvinyl chloride, the polyvinyl chloride has poor stability in the processing and using processes, the forming and the application of a polyvinyl chloride decorative film are seriously influenced, and the defect of the polyvinyl chloride is usually improved by adopting a physical modification method in the field.
The graphene is sp 2 The hybridized and connected carbon atoms are tightly stacked into a material with a single-layer two-dimensional honeycomb-shaped lattice structure, and the material has the characteristics of ultrahigh strength, ultrahigh electrical conductivity, ultrahigh thermal conductivity, ultrahigh specific surface area, ultrahigh light transmittance and the like, and can be widely applied to preparation of composite materials. And the graphene has the characteristics of high stability, strong barrier property, large surface adsorption and the like, can effectively reduce heat transfer and mass transfer in the material combustion process, and can be used as a flame retardant to enhance the flame retardant property of a high polymer material.
Therefore, the mechanical property of the polyvinyl chloride can be improved and the flame retardant property of the polyvinyl chloride can be enhanced by adding a proper amount of graphene into the polyvinyl chloride. However, since graphene is an inorganic nonmetallic material, the compatibility between graphene and a high molecular polymer is poor.
The invention content is as follows:
the invention aims to solve the technical problem of providing an environment-friendly flame-retardant polyvinyl chloride/graphene composite decorative film for rail transit, which improves the flame retardant property and the mechanical property by blending and modifying polyvinyl chloride with graphene.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
one of the purposes of the invention is to provide a preparation method of an environment-friendly flame-retardant polyvinyl chloride/graphene composite material, which comprises the following steps:
(1) Preparing a flame retardant modifier by condensation reaction of dibenzyl phosphoramidate and 2-chloroethyl sodium sulfonate;
(2) Carrying out non-covalent modification on graphene oxide by using the prepared flame retardant modifier to obtain flame retardant enhanced graphene;
(3) And mixing polyvinyl chloride, the prepared flame-retardant enhanced graphene, a plasticizer and a heat stabilizer, then carrying out melt extrusion, cooling and granulating to obtain the polyvinyl chloride/graphene composite material.
Preferably, the mole ratio of the dibenzyl phosphoramidate to the sodium 2-chloroethyl sulfonate is (1-1.2): 1.
Preferably, the mass ratio of the graphene oxide to the flame retardant modifier is 1 (1-10).
Although graphene has a certain flame-retardant effect, the graphene is poor in compatibility with polyvinyl chloride, and the flame-retardant enhanced graphene is prepared by carrying out nitrogen and phosphorus doping modification on the graphene, so that the flame-retardant property of the graphene can be enhanced, the compatibility of the graphene and the polyvinyl chloride can be improved, and the prepared flame-retardant enhanced graphene can be promoted to efficiently exert the flame-retardant property. Meanwhile, the comprehensive application performance of the polyvinyl chloride material can be improved by utilizing the specific mechanical property, thermal property and electrical property of the graphene.
Preferably, the non-covalent modification is carried out under the influence of ultrasound. The modification time is shortened, and the modification effect is improved.
Preferably, the mass ratio of the polyvinyl chloride to the flame-retardant enhanced graphene to the plasticizer to the heat stabilizer is 100 (0.5-5): 5-25): 1-8. The plasticizer can improve the plasticity of the polyvinyl chloride and endow the polyvinyl chloride product with good flexibility; the heat stability of the polyvinyl chloride can be improved by adding the heat stabilizer, and the normal operation of subsequent forming processing is ensured.
Preferably, the plasticizer is at least one of phthalate plasticizers, trimellitate plasticizers, citrate plasticizers and aliphatic dibasic acid ester plasticizers.
Preferably, the heat stabilizer is at least one of calcium-zinc composite stabilizer, organic tin stabilizer and rare earth composite stabilizer.
Preferably, the melt extrusion temperature is 130-160 ℃.
The invention also aims to provide the environment-friendly flame-retardant polyvinyl chloride/graphene composite material prepared by the preparation method.
The invention also aims to provide the application of the environment-friendly flame-retardant polyvinyl chloride/graphene composite material in the processing of track traffic decorative films.
The prepared environment-friendly flame-retardant polyvinyl chloride/graphene composite material can be directly processed into the rail transit decorative film by a calendering film-forming method, or the rail transit decorative film can be processed by the calendering film-forming method after adding an auxiliary agent on the basis of the prepared environment-friendly flame-retardant polyvinyl chloride/graphene composite material, wherein the auxiliary agent comprises a filler, a coloring agent, an antioxidant, an antistatic agent and the like.
The invention has the beneficial effects that:
(1) According to the invention, dibenzyl phosphoramidate and 2-chloroethyl sodium sulfonate are adopted to synthesize the flame retardant modifier, and the flame retardant modifier is utilized to carry out non-covalent modification (hydrogen bond action between sulfonic group and hydroxyl group) on graphene oxide, so that the prepared nitrogen-phosphorus doped graphene has good flame retardant property, and meanwhile, the compatibility between the graphene oxide and polyvinyl chloride is improved, and the subsequent melt processing is facilitated.
(2) According to the invention, the prepared flame-retardant enhanced graphene is compounded with polyvinyl chloride to prepare the polyvinyl chloride/graphene composite material, so that the flame-retardant property of the polyvinyl chloride is effectively improved, and the environmental friendliness when the flame-retardant property of the polyvinyl chloride is exerted is improved.
(3) According to the invention, the prepared polyvinyl chloride/graphene composite material is adopted to process the rail transit decorative film, so that the good decorative function can be exerted, the flame retardant effect, the mechanical property and the like of the decorative film can be enhanced, the VOC emission in the use process of the decorative film is reduced, and the environmental protection property of the decorative film is improved, thereby being suitable for the rail transit environment.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
The source of the raw materials in the following examples and comparative examples is illustrated:
polyvinyl chloride SG-5 was purchased from Ji nan Dai Hui chemical science and technology Limited.
Graphene oxide was purchased from beijing meiston scientific development ltd with an oxygen content of 46%.
The calcium-zinc composite stabilizer NC-105P is purchased from Hangzhou Furui specialization engineering and technology Co.
Organotin stabilizers 181 are available from Jiangsu Cheng Kai plasticizer technology, inc.
Preparing a flame retardant modifier: adding 2-chloroethyl sodium sulfonate (18.4 g, 0.1mol) and pyridine (7.9g, 0.1mol) into water, stirring and dissolving completely, then adding dibenzyl phosphoramidate (30.5 g, 0.11mol), carrying out ultrasonic reaction at 60 ℃, stopping reaction after the dibenzyl phosphoramidate is completely reacted, adding absolute ethyl alcohol, stirring, filtering precipitated solid, dissolving with water, recrystallizing, filtering, and drying at 70 ℃ to obtain the flame retardant modifier, wherein the yield is 94.27%, and the purity is 99.68%.
Example 1
Adding 200g of the prepared flame-retardant modifier into water, stirring and dissolving, then adding 100g of graphene oxide, carrying out ultrasonic treatment for 5h at 50 ℃, filtering, washing, and drying at 100 ℃ to obtain the flame-retardant enhanced graphene.
And (2) mixing polyvinyl chloride SG-5, the prepared flame-retardant enhanced graphene, dioctyl phthalate and calcium-zinc composite stabilizer NC-105P according to a mass ratio of 100.
And (3) rolling the prepared polyvinyl chloride/graphene composite material at 150 ℃ to form a film, wherein the linear speed of a roller is 10m/min, so that the rail transit decorative film is obtained.
Example 2
Adding 300g of the prepared flame-retardant modifier into water, stirring for dissolving, adding 100g of graphene oxide, performing ultrasonic treatment at 50 ℃ for 8 hours, filtering, washing, and drying at 100 ℃ to obtain the flame-retardant enhanced graphene.
Mixing polyvinyl chloride SG-5, the prepared flame-retardant enhanced graphene, dibutyl phthalate and a calcium-zinc composite stabilizer NC-105P according to a mass ratio of 100.
And (3) rolling the prepared polyvinyl chloride/graphene composite material at 150 ℃ to form a film, wherein the linear speed of a roller is 10m/min, so that the rail transit decorative film is obtained.
Example 3
Adding 500g of the prepared flame-retardant modifier into water, stirring and dissolving, then adding 100g of graphene oxide, carrying out ultrasonic treatment for 10h at 50 ℃, filtering, washing, and drying at 100 ℃ to obtain the flame-retardant enhanced graphene.
And (2) mixing polyvinyl chloride SG-5, the prepared flame-retardant enhanced graphene, tributyl citrate and an organic tin stabilizer 181 according to a mass ratio of 100.
And (3) rolling the prepared polyvinyl chloride/graphene composite material at 150 ℃ to form a film, wherein the linear speed of a roller is 12m/min, so that the rail transit decorative film is obtained.
Example 4
Adding 800g of the prepared flame-retardant modifier into water, stirring and dissolving, adding 100g of graphene oxide, performing ultrasonic treatment at 50 ℃ for 12h, filtering, washing, and drying at 100 ℃ to obtain the flame-retardant enhanced graphene.
And (2) mixing polyvinyl chloride SG-5, the prepared flame-retardant enhanced graphene, acetyl tributyl citrate and an organic tin stabilizer 181 according to a mass ratio of 100.
And (3) rolling the prepared polyvinyl chloride/graphene composite material at 150 ℃ to form a film, wherein the linear speed of a roller is 12m/min, so that the rail transit decorative film is obtained.
Comparative example 1
The flame retardant modifier in example 3 was replaced with graphene oxide, and the remaining preparation steps were the same as in example 3.
Comparative example 2
The flame retardant modifier in example 3 was replaced with a mixture of graphene oxide and dibenzyl phosphoramidate in a mass ratio of 1:5, and the remaining preparation steps were the same as in example 3.
The decorative films prepared in examples 1 to 4 and comparative examples 1 to 2 have a thickness of 0.24mm, and were tested for flame retardancy according to standards GB/T2406-2008 and GB/T2408-2008, and tensile properties according to GB/T1040.3-2006, with the test results shown in Table 1.
TABLE 1
As can be seen from table 1, the flame retardant modifier prepared by the method can not only enhance the flame retardant property of the composite material, but also does not significantly reduce the mechanical property of the composite material, and the mechanical property of the composite material can be significantly reduced by directly adding the mixture of graphene oxide and dibenzyl phosphoramidate or directly adding graphene oxide, and the flame retardant property is not high.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and such changes and modifications are within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The preparation method of the environment-friendly flame-retardant polyvinyl chloride/graphene composite material is characterized by comprising the following steps of:
(1) Preparing a flame retardant modifier by condensation reaction of dibenzyl phosphoramidate and 2-chloroethyl sodium sulfonate;
(2) Carrying out non-covalent modification on graphene oxide by using the prepared flame-retardant modifier to obtain flame-retardant enhanced graphene;
(3) And mixing polyvinyl chloride, the prepared flame-retardant enhanced graphene, a plasticizer and a heat stabilizer, then carrying out melt extrusion, cooling and granulating to obtain the polyvinyl chloride/graphene composite material.
2. The method of claim 1, wherein: the mole ratio of the dibenzyl phosphoramidate to the 2-chloroethyl sodium sulfonate is (1-1.2) to 1.
3. The method of claim 1, wherein: the mass ratio of the graphene oxide to the flame-retardant modifier is 1 (1-10).
4. The method of claim 1, wherein: the non-covalent modification is carried out under the action of ultrasound.
5. The method of claim 1, wherein: the mass ratio of the polyvinyl chloride to the flame-retardant enhanced graphene to the plasticizer to the heat stabilizer is 100 (0.5-5) to (5-25) to (1-8).
6. The method of claim 1, wherein: the plasticizer is at least one of phthalate plasticizers, trimellitate plasticizers, citrate plasticizers and aliphatic dibasic acid ester plasticizers.
7. The method of claim 1, wherein: the heat stabilizer is at least one of calcium-zinc composite stabilizer, organic tin stabilizer and rare earth composite stabilizer.
8. The method of claim 1, wherein: the temperature of the melt extrusion is 130-160 ℃.
9. The environment-friendly flame-retardant polyvinyl chloride/graphene composite material prepared by the preparation method according to any one of claims 1 to 8.
10. The use of the environmentally friendly flame retardant polyvinyl chloride/graphene composite material of claim 9 in rail transit decorative film processing.
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