CN112662090A - Modified rigid polyvinyl chloride foam and preparation method thereof - Google Patents
Modified rigid polyvinyl chloride foam and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of polymer foam materials, and in particular relates to modified rigid polyvinyl chloride foam and a preparation method thereof, wherein the modified rigid polyvinyl chloride foam comprises 90-100 parts of polyvinyl chloride paste resin, 0-10 parts of chlorinated polyvinyl chloride resin, 35-70 parts of isocyanate, 10-25 parts of anhydride, 5-15 parts of epoxy resin, 5-10 parts of a foaming agent, 10-40 parts of a conductive agent and 5-10 parts of a filler. The hard crosslinked polyvinyl chloride foam with better conductivity is prepared by adding a conductive agent, in particular to a modified carbon nanotube obtained by processing, in the preparation process of the hard crosslinked polyvinyl chloride foam. In addition, by optimizing the proportion and the preparation process of each component in the formula, the prepared hard cross-linked polyvinyl chloride foam not only has conductive performance, but also has better mechanical property; in addition, the preparation method is simple, the process controllability is strong, and the application field and the application range of the hard crosslinked polyvinyl chloride foam are increased.
Description
Technical Field
The invention relates to the field of polymer foam materials, in particular to modified rigid polyvinyl chloride foam and a preparation method thereof
Background
The rigid cross-linked polyvinyl chloride foam has the typical characteristics of light weight, high strength, high modulus and other structural core materials, has the advantages of low manufacturing cost, high water resistance, good flame retardant effect and the like compared with other high-performance foams such as polymethacrylimide foam, polyetherimide foam and the like, and has increasingly wide application in the fields of ships, wind energy, transportation, sports equipment, aerospace and the like. However, since polyvinyl chloride has good electrical insulation, static charges are easily generated on the surface and are not easily transferred on the surface. When the static charge on the surface has accumulated to a certain extent, it poses serious danger, which greatly limits the range of use. Therefore, the research on the antistatic modification of PVC has important significance on the expansion of the application range of the PVC.
The filling of the conductive filler is a main method for preparing antistatic PVC at present due to simple process and low cost. The commonly used conductive fillers mainly comprise graphite, metal powder and the like, but the fillers have poor compatibility with polyvinyl chloride and weak conductive capability, cannot achieve an antistatic effect when the filling amount is small, and can cause the mechanical property of the polyvinyl chloride material to be obviously reduced when the filling amount is large. Therefore, a similar low-cost two-dimensional filler system and a similar low-cost one-dimensional filler system are sought, and the realization of composite modification is an important development direction for realizing that the polyvinyl chloride maintains the mechanical property and is endowed with the electrical conductivity.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention aims to provide modified rigid polyvinyl chloride foam which has better mechanical property and better conductivity, so that the application range of the rigid cross-linked polyvinyl chloride foam is wider.
Through repeated experiments, when the modified carbon nano tube obtained by pretreating the conductive agent, particularly the carbon nano tube, or a plurality of conductive agents are used simultaneously, the prepared hard crosslinked polyvinyl chloride foam has good conductive performance, and the mechanical properties and mechanical properties of light weight, high strength and high modulus of the hard crosslinked polyvinyl chloride foam are not influenced.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
the invention provides modified rigid polyvinyl chloride foam which is mainly prepared from the following raw materials:
90-100 parts of polyvinyl chloride paste resin, 0-10 parts of chlorinated polyvinyl chloride resin, 35-70 parts of isocyanate, 10-25 parts of anhydride, 5-15 parts of epoxy resin, 5-10 parts of foaming agent, 10-40 parts of conductive agent and 5-10 parts of filler.
On the basis of the technical scheme, 95-99 parts of polyvinyl chloride paste resin, 1-5 parts of chlorinated polyvinyl chloride resin, 50-70 parts of isocyanate, 12-23 parts of acid anhydride, 5-10 parts of epoxy resin, 6-8 parts of foaming agent, 20-40 parts of conductive agent and 5-8 parts of filler.
On the basis of the technical scheme, the K value of the polyvinyl chloride paste resin is 75-80, and the chlorine content of the chlorinated polyvinyl chloride resin is 75%.
On the basis of the technical scheme, the isocyanate is one or more of diphenylmethane diisocyanate, toluene diisocyanate, 4' -dicyclohexylmethane diisocyanate, hexamethylene diisocyanate and polymethylene polyphenyl polyisocyanate.
On the basis of the technical scheme, the acid anhydride is one or more of maleic anhydride, succinic anhydride, acrylic anhydride, itaconic anhydride, cyclohexane-1, 2-dicarboxylic anhydride, dodecenyl succinic anhydride, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, trimellitic anhydride and pyromellitic dianhydride.
On the basis of the technical scheme, the foaming agent is one or more of p-methyl sulfonamide, azodiisobutyronitrile and N, N-dinitrosopentamethylenetetramine.
On the basis of the technical scheme, the conductive agent is one or more of modified carbon nanotubes, carbon fibers and conductive carbon black.
On the basis of the technical scheme, the modified carbon nanotube material is prepared by the following steps: firstly, putting a multi-walled carbon nanotube into a closed container containing concentrated nitric acid, and treating for 12 hours at 150 ℃; then centrifugally washing the filtrate by using deionized water and ethanol until the filtrate is neutral, and drying the filtrate at 55-60 ℃; finally, heat treatment is carried out at the temperature of 400-600 ℃ in inert gas to obtain the modified carbon nano tube.
On the basis of the technical scheme, the filler is one or more of wollastonite, titanium dioxide and montmorillonite.
The invention provides a preparation method of modified rigid polyvinyl chloride foam, which comprises the following steps:
step one, uniformly mixing the raw materials which are liquid in the components according to the weight under 0.09MPa, then adding the raw materials which are solid in the components into the liquid according to the weight, and fully stirring to obtain a uniform pasty mixture;
step two, pouring the uniform pasty mixture into a well-sealed die, carrying out compression molding under the conditions that the temperature is 145-195 ℃ and the pressure is 5-35 MPa, cooling the die, and opening the die to obtain a compression molded block;
step three, placing the mould pressing block obtained in the step two in a steam chamber at the temperature of 65-98 ℃ for foaming to obtain foam;
and step four, curing the foam obtained in the step three in a steam chamber at the temperature of 45-80 ℃ to obtain the modified rigid polyvinyl chloride foam.
The technical scheme provided by the invention has the beneficial effects that:
the hard crosslinked polyvinyl chloride foam with better conductivity is prepared by adding a conductive agent, in particular to a modified carbon nanotube obtained by processing, in the preparation process of the hard crosslinked polyvinyl chloride foam. In addition, the modified carbon nano tube can not only increase the conductivity of the polyvinyl chloride foam, but also increase the mechanical property of the polyvinyl chloride foam after being processed, thereby ensuring the advantages of light weight and high strength.
By optimizing the proportion and the preparation process of each component in the formula, the prepared hard cross-linked polyvinyl chloride foam not only has conductive performance, but also has better mechanical property; in addition, the preparation method is simple, the process controllability is strong, and the application field and the application range of the hard crosslinked polyvinyl chloride foam are increased.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the contents in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
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. It is to be understood that the various starting materials of the present invention are commercially available, unless otherwise specified.
Example 1
The invention provides modified rigid polyvinyl chloride foam which is prepared from the following raw materials:
90 parts of polyvinyl chloride paste resin with a K value of 75, 10 parts of chlorinated polyvinyl chloride resin, 35 parts of polymethylene polyphenyl polyisocyanate, 10 parts of maleic anhydride, 5 parts of epoxy resin, 5 parts of azodiisobutyronitrile, 5 parts of modified carbon nanotube and 5 parts of titanium dioxide.
Wherein the modified carbon nanotube material is prepared by the following steps: firstly, putting a multi-walled carbon nanotube into a closed container containing concentrated nitric acid, and treating for 12 hours at 150 ℃; then, centrifugally washing the filtrate by using deionized water and ethanol until the filtrate is neutral, and drying the filtrate at 55 ℃; finally, heat treatment is carried out at 450 ℃ in inert gas to obtain the modified carbon nano tube.
The invention provides a preparation method of modified rigid polyvinyl chloride foam, which comprises the following steps:
step one, uniformly mixing the raw materials which are liquid in the components according to the weight under 0.09MPa, then adding the raw materials which are solid in the components into the liquid according to the weight, and fully stirring to obtain a uniform pasty mixture;
step two, filling a steel mould with the thickness of 25mm with the uniform paste prepared in the step one, putting the mould into a flat press at 195 ℃ after mould closing, keeping the pressure at 5MPa for 10min, cooling the mould, and opening the mould when the temperature of the mould is lower than 60 ℃ to obtain a mould pressing block;
step three, the mould pressing block taken out in the step two is placed in a steam chamber at the temperature of 98 ℃ for foaming for 3 hours to prepare foam;
and step four, curing the foam obtained in the step three in a steam chamber at the temperature of 80 ℃ for 3 days to obtain the modified rigid polyvinyl chloride foam. The test performance index is shown in table 1.
Example 2
The invention provides modified rigid polyvinyl chloride foam which is prepared from the following raw materials:
99 parts of polyvinyl chloride paste resin with a K value of 76, 1 part of chlorinated polyvinyl chloride resin, 70 parts of diphenylmethane diisocyanate, 23 parts of dodecenyl succinic anhydride, 15 parts of epoxy resin, 8 parts of p-methyl sulfonamide, 20 parts of carbon fiber, 5 parts of titanium dioxide and 5 parts of silica fume.
The invention provides a preparation method of modified rigid polyvinyl chloride foam, which comprises the following steps:
step one, uniformly mixing the raw materials which are liquid in the components according to the weight under 0.09MPa, then adding the raw materials which are solid in the components into the liquid according to the weight, and fully stirring to obtain a uniform pasty mixture;
step two, filling a 25mm thick steel mould with the uniform paste prepared in the step one, placing the mould into a flat plate press at 145 ℃ after mould closing, keeping the pressure at 30MPa for 10min, cooling the mould, and opening the mould when the temperature of the mould is lower than 60 ℃ to obtain a mould pressing block;
step three, the mould pressing block taken out in the step two is placed in a steam chamber with the temperature of 90 ℃ for foaming for 4 hours to prepare foam;
and step four, curing the foam obtained in the step three in a steam chamber at 55 ℃ for 4 days to obtain the modified rigid polyvinyl chloride foam. The test performance index is shown in table 1.
Example 3
The invention provides modified rigid polyvinyl chloride foam which is prepared from the following raw materials:
95 parts of polyvinyl chloride paste resin with a K value of 75, 5 parts of chlorinated polyvinyl chloride resin, 25 parts of diphenylmethane diisocyanate, 25 parts of hexamethylene diisocyanate, 12 parts of hexahydrophthalic anhydride, 10 parts of epoxy resin, 6 parts of azobisisobutyronitrile, 20 parts of modified carbon nano tube, 10 parts of conductive carbon black and 6 parts of wollastonite.
Wherein the modified carbon nanotube material is prepared by the following steps: firstly, putting a multi-walled carbon nanotube into a closed container containing concentrated nitric acid, and treating for 12 hours at 150 ℃; then, centrifugally washing the filtrate by using deionized water and ethanol until the filtrate is neutral, and drying the filtrate at 60 ℃; finally, heat treatment is carried out at 550 ℃ in inert gas, and the modified carbon nano tube is obtained.
The invention provides a preparation method of modified rigid polyvinyl chloride foam, which comprises the following steps:
step one, uniformly mixing the raw materials which are liquid in the components according to the weight under 0.09MPa, then adding the raw materials which are solid in the components into the liquid according to the weight, and fully stirring to obtain a uniform pasty mixture;
step two, filling a steel mould with the thickness of 25mm with the uniform paste prepared in the step one, placing the mould into a flat plate press at 175 ℃ after mould closing, keeping the pressure at 22MPa for 10min, cooling the mould, and opening the mould when the temperature of the mould is lower than 60 ℃ to obtain a mould pressing block;
step three, the mould pressing block taken out in the step two is placed in a steam chamber at the temperature of 75 ℃ for foaming for 2 hours to prepare foam;
and step four, curing the foam obtained in the step three in a steam chamber at the temperature of 60 ℃ for 2 days to obtain the modified rigid polyvinyl chloride foam. The test performance index is shown in table 1.
Example 4
The invention provides modified rigid polyvinyl chloride foam which is prepared from the following raw materials:
98 parts of polyvinyl chloride paste resin with a K value of 80, 2 parts of chlorinated polyvinyl chloride resin, 20 parts of 4,4' -dicyclohexylmethane diisocyanate, 30 parts of hexamethylene diisocyanate, 18 parts of cyclohexane-1, 2-dicarboxylic anhydride, 5 parts of epoxy resin, 3 parts of p-methyl sulfonamide, 4 parts of N, N-dinitrosopentamethylene tetramine, 20 parts of modified carbon nano tube, 20 parts of carbon fiber, 5 parts of titanium dioxide and 3 parts of montmorillonite.
Wherein the modified carbon nanotube material is prepared by the following steps: firstly, putting a multi-walled carbon nanotube into a closed container containing concentrated nitric acid, and treating for 12 hours at 150 ℃; then, centrifugally washing the filtrate by using deionized water and ethanol until the filtrate is neutral, and drying the filtrate at 55 ℃; finally, heat treatment is carried out at 600 ℃ in inert gas to obtain the modified carbon nano tube.
The invention provides a preparation method of modified rigid polyvinyl chloride foam, which comprises the following steps:
step one, uniformly mixing the raw materials which are liquid in the components according to the weight under 0.09MPa, then adding the raw materials which are solid in the components into the liquid according to the weight, and fully stirring to obtain a uniform pasty mixture;
step two, filling a 25mm thick steel mould with the uniform paste prepared in the step one, placing the mould into a flat press at 180 ℃ after mould closing, keeping the pressure at 28MPa for 10min, cooling the mould, and opening the mould when the temperature of the mould is lower than 60 ℃ to obtain a mould pressing block;
step three, the mould pressing block taken out in the step two is placed in a steam chamber with the temperature of 95 ℃ for foaming for 3 hours to prepare foam;
and step four, curing the foam obtained in the step three in a steam chamber at 70 ℃ for 3 days to obtain the modified rigid polyvinyl chloride foam. The test performance index is shown in table 1.
Comparative example
The invention provides modified rigid polyvinyl chloride foam which is prepared from the following raw materials:
98 parts of polyvinyl chloride paste resin with a K value of 80, 2 parts of chlorinated polyvinyl chloride resin, 20 parts of 4,4' -dicyclohexylmethane diisocyanate, 30 parts of hexamethylene diisocyanate, 18 parts of cyclohexane-1, 2-dicarboxylic anhydride, 5 parts of epoxy resin, 3 parts of p-methylsulfonamide, 4 parts of N, N-dinitrosopentamethylenetetramine, 5 parts of titanium dioxide and 3 parts of montmorillonite.
The invention provides a preparation method of modified rigid polyvinyl chloride foam, which comprises the following steps:
step one, uniformly mixing the raw materials which are liquid in the components according to the weight under 0.09MPa, then adding the raw materials which are solid in the components into the liquid according to the weight, and fully stirring to obtain a uniform pasty mixture;
step two, filling a 25mm thick steel mould with the uniform paste prepared in the step one, placing the mould into a flat press at 180 ℃ after mould closing, keeping the pressure at 28MPa for 10min, cooling the mould, and opening the mould when the temperature of the mould is lower than 60 ℃ to obtain a mould pressing block;
step three, the mould pressing block taken out in the step two is placed in a steam chamber with the temperature of 95 ℃ for foaming for 3 hours to prepare foam;
and step four, curing the foam obtained in the step three in a steam chamber at 70 ℃ for 3 days to obtain the modified rigid polyvinyl chloride foam. The test performance index is shown in table 1.
Experimental results and Performance analysis
As can be seen from the test data in table 1, the conductive properties of the rigid crosslinked polyvinyl chloride foams prepared in examples 1 to 4 were all superior to those of the comparative example without the conductive agent, and the conductive properties of examples 1 to 4 were sequentially increased depending on the amount and the material of the conductive agent. Comparative example compared with example 4, which has similar density, example 4 is not only excellent in conductivity but also excellent in mechanical property index.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. The modified rigid polyvinyl chloride foam is characterized by being mainly prepared from the following raw materials:
90-100 parts of polyvinyl chloride paste resin, 0-10 parts of chlorinated polyvinyl chloride resin, 35-70 parts of isocyanate, 10-25 parts of anhydride, 5-15 parts of epoxy resin, 5-10 parts of foaming agent, 10-40 parts of conductive agent and 5-10 parts of filler.
2. The modified rigid polyvinyl chloride foam is characterized by being mainly prepared from the following raw materials:
95-99 parts of polyvinyl chloride paste resin, 1-5 parts of chlorinated polyvinyl chloride resin, 50-70 parts of isocyanate, 12-23 parts of anhydride, 5-10 parts of epoxy resin, 6-8 parts of foaming agent, 20-40 parts of conductive agent and 5-8 parts of filler.
3. The modified rigid polyvinyl chloride foam according to claim 2, wherein said polyvinyl chloride paste resin has a K value of 75 to 80 and a chlorine content of 75% in the chlorinated polyvinyl chloride resin.
4. The modified rigid polyvinyl chloride foam according to claim 2, wherein said isocyanate is one or more of diphenylmethane diisocyanate, toluene diisocyanate, 4' -dicyclohexylmethane diisocyanate, hexamethylene diisocyanate, and polymethylene polyphenyl polyisocyanate.
5. The modified rigid polyvinyl chloride foam of claim 2, wherein said anhydride is one or more of maleic anhydride, succinic anhydride, acrylic anhydride, itaconic anhydride, cyclohexane-1, 2-dicarboxylic anhydride, dodecenyl succinic anhydride, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, trimellitic anhydride, and pyromellitic dianhydride.
6. The modified rigid polyvinyl chloride foam of claim 2, wherein said blowing agent is one or more of p-methyl sulfonamide, azobisisobutyronitrile, and N, N-dinitrosopentamethylenetetramine.
7. The modified rigid polyvinyl chloride foam according to claim 2, wherein the conductive agent is one or more of modified carbon nanotubes, carbon fibers and conductive carbon black.
8. The modified rigid polyvinyl chloride foam according to claim 7, wherein the modified carbon nanotube material is prepared by the following steps: firstly, putting a multi-walled carbon nanotube into a closed container containing concentrated nitric acid, and treating for 12 hours at 150 ℃; then centrifugally washing the filtrate by using deionized water and ethanol until the filtrate is neutral, and drying the filtrate at 55-60 ℃; finally, heat treatment is carried out at the temperature of 400-600 ℃ in inert gas to obtain the modified carbon nano tube.
9. The modified rigid polyvinyl chloride foam according to claim 2, wherein the filler is one or more of wollastonite, titanium dioxide and montmorillonite.
10. A process for the preparation of a modified rigid polyvinyl chloride foam according to any of claims 1 to 9, characterized by comprising the following steps:
step one, uniformly mixing the raw materials which are liquid in the components according to the weight under 0.09MPa, then adding the raw materials which are solid in the components into the liquid according to the weight, and fully stirring to obtain a uniform pasty mixture;
step two, pouring the uniform pasty mixture into a well-sealed die, carrying out compression molding under the conditions that the temperature is 145-195 ℃ and the pressure is 5-35 MPa, cooling the die, and opening the die to obtain a compression molded block;
step three, placing the mould pressing block obtained in the step two in a steam chamber at the temperature of 65-98 ℃ for foaming to obtain foam;
and step four, curing the foam obtained in the step three in a steam chamber at the temperature of 45-80 ℃ to obtain the modified rigid polyvinyl chloride foam.
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Cited By (1)
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| WO2023219007A1 (en) * | 2022-05-09 | 2023-11-16 | 東レ株式会社 | Thermosetting resin composition, molded article, molding material for fiber-reinforced composite material, and fiber-reinforced composite material |
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Application publication date: 20210416 |