CN111518344A - Preparation method of low-temperature-resistant polyvinyl chloride composite material - Google Patents
Preparation method of low-temperature-resistant polyvinyl chloride composite material Download PDFInfo
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Abstract
The invention relates to a preparation method of a low-temperature-resistant polyvinyl chloride composite material, and belongs to the technical field of composite materials. The invention relates to a low-temperature resistant polyvinyl chloride composite material which is prepared by taking liquid paraffin, n-hexadecane and n-octadecane as heat storage and preservation agents and calcium carbonate as a wall material to coat the heat storage and preservation agents, wherein a mixed phase change material prepared from the liquid paraffin, the n-hexadecane and the n-octadecane forms a net-shaped matrix through an inorganic substance to maintain the mechanical property and the structural framework of the material, the phase change microcapsule coats the phase change material in the wall material through a microcapsule technology to form tiny particles, the structure of the phase change microcapsule can be divided into two parts, the interior of the phase change microcapsule is a phase change material core material, the phase change microcapsule can absorb or release a large amount of phase change latent heat in the phase change process, the particle size of the phase change microcapsule is small, the specific surface area is large, the heat transfer effect is good, and the cold.
Description
Technical Field
The invention relates to a preparation method of a low-temperature-resistant polyvinyl chloride composite material, and belongs to the technical field of composite materials.
Background
Polyvinyl chloride (PVC) is a general-purpose resin which is widely used, has a large relation with human life, is an indispensable important material, and is second only to polyethylene in global demand. The development of the polyvinyl chloride industry can be divided into three phases: the first is the polyvinyl chloride coming out and industrial induction period, the second is the polyvinyl chloride industrial development period, and the last is the industrial maturity period.
The density of the polyvinyl chloride is 1.35-1.45g/cm3Insofar as the characteristics and average molecular weight contained in the polyvinyl chloride are closely related in the production of the product. Polyvinyl chloride resins with higher molecular weights have higher impact strength and elasticity, and poorer processability. In terms of polymerization methods, polymerization of polyvinyl chloride is classified into bulk polymerization, emulsion polymerization and suspension polymerization, and a method of manufacturing polyvinyl chloride resin generally employs suspension polymerization, and the produced resin may be referred to as SG resin, since the SG resin has a small density and a large number of microcells, so the processing property is better, the plasticizer is easy to permeate into the resin, the polyvinyl chloride produced by the emulsion method is pasty, the average molecular weight is larger, the polymerization time is short, the control is easy, the process of producing the polyvinyl chloride by the bulk method can be divided into two steps, the monomer in the first step is polymerized under the initiation of an initiator, the reaction in the second step is that the substance generated in the first step is further polymerized with the monomer, the conversion rate of the monomer can reach 90 percent, the method for preparing the polyvinyl chloride by the bulk method is not complex, the capital investment in the production process is low, and the quality of the obtained polyvinyl chloride resin is good.
The polyvinyl chloride can be applied to the fields of medical treatment, agriculture, manufacturing industry and the like, is plastic with the longest development time after being industrialized, and has more advantages, such as better insulating property, corrosion resistance, good wear resistance, flame retardant property and the like. Polyvinyl chloride has become a general-purpose resin with a large demand amount due to its own advantages such as the above-mentioned advantages and low price, and has been developed smoothly on the basis of this momentum. The PVC has different hardness, including hard, semi-hard and soft, and the plasticizer is hard polyvinyl chloride in 0-5 weight portions, semi-hard polyvinyl chloride in 5-25 weight portions and soft polyvinyl chloride in over 25 weight portions.
The polyvinyl chloride has wide application and lower cost, the hard polyvinyl chloride can be made into soft products with different hardness after being added with different parts of plasticizer, the hard polyvinyl chloride has wide application and can be used for producing pipes, door and window products and the like, but the polyvinyl chloride has poor thermal stability and is easy to degrade in the environment of illumination, so the stability of the polyvinyl chloride product must be improved, and the polyvinyl chloride can be applied to outdoor products. There are two methods for increasing the heat distortion temperature of polyvinyl chloride, one method is to add fillers to polyvinyl chloride resin, but this method has poor modification effect because the addition of fillers can only make the heat distortion temperature of amorphous material close to its glass transition temperature. Another effective method is to mix polyvinyl chloride with other high polymer materials with higher softening point, so as to achieve the purpose of ensuring that the blend has better mechanical properties in the aspect of selecting the high polymer materials, and the materials with similar solubility to the polyvinyl chloride are selected.
There are three common methods for improving the cold resistance of polyvinyl chloride: toughening the elastomer, toughening the nano particles and toughening the composite material.
The elastomer toughening mechanism is a silver streak-shear band mechanism, and specifically, rubber is uniformly dispersed in resin as a dispersed phase and can be used as a stress concentration point to absorb energy, so that the matrix cannot be damaged by external force. In addition, the silver lines and the shear bands can appear around the rubber, the appearance of the silver lines and the shear bands reduces the action energy on the matrix, and the shear bands can prevent the silver lines or tiny cracks from expanding into destructive cracks, so that the matrix is protected from being damaged by external applied force. The network toughening is also one of elastomer toughening, the network toughening is that elastomers are connected together to form a network which is wrapped around polyvinyl chloride primary particles, and the network and the primary particles can be subjected to external impact skills, so that destructive cracks cannot be caused by impact energy.
The inorganic nano particles are used as a modifier to improve the cold resistance of the PVC, and have the advantages that the modified PVC not only has better toughness, but also has good heat resistance and dimensional stability. Because the contact area between the inorganic nano particles and the PVC is large, when the resin matrix is impacted by external force, more micro cracks can be generated around the resin matrix to absorb energy, and meanwhile, the nano particles can prevent the growth of cracks and prevent the cracks from developing into cracks which can break the matrix.
Currently, the more researched composite toughening systems mainly comprise two or more than two types of elastomer particles and the compound modification of elastomer/rigid particles. The synergistic effect of the elastomer particles is mainly reflected by the compatibilization among the elastomer particles. The nano inorganic rigid particles and the rubber particles are matched for toughening, so that the impact strength improvement range of the rigid particles can be greatly improved, the cost of toughening of the elastomer can be reduced, and the reinforcing effect is achieved, thereby becoming a hot point of research in recent years.
Although polyvinyl chloride has many advantages, so that the consumption of polyvinyl chloride is high, and the application range is wide, some disadvantages of polyvinyl chloride reduce the service performance of the product and limit the application to a certain extent. The processing temperature and the decomposition temperature of the polyvinyl chloride resin are similar, so that HCL gas is easily released to pollute the environment during processing, and conjugated olefin is formed to discolor the product, thereby influencing the appearance of the product. In addition, polyvinyl chloride has low impact strength, is easy to break when being subjected to external force, and is easy to be damaged under the condition of being subjected to the external force particularly in a low-temperature environment, so that the use of products is influenced. The soft polyvinyl chloride product usually contains a small molecular plasticizer, the small molecular plasticizer is easy to migrate in a high-temperature environment, the compatibility of the medical polyvinyl chloride product and blood is influenced, and the small molecular plasticizer enters a human body and further influences the health of the human body.
At present, there have been many researches on polyvinyl chloride modification, and the modification methods include chemical and physical methods, but the chemical modification method is complicated and difficult to implement industrial production, so that a simple and easy physical blending modification method is usually adopted. In the physical blending modification, the transparency of the product is reduced and the service performance and the appearance of the product are influenced due to the reasons of poor compatibility, large difference of refractive index and the like of the modifier and the polyvinyl chloride, so that the physical blending modification is carried out on the polyvinyl chloride, the plasticizing temperature of the polyvinyl chloride is reduced, the processability of the polyvinyl chloride is improved, the cold resistance of the polyvinyl chloride is improved, and the good transparency of the polyvinyl chloride is ensured, thereby having very important effect on improving the quality of the polyvinyl chloride product.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problem of poor low temperature resistance of the existing polyvinyl chloride composite material, the preparation method of the low temperature resistant polyvinyl chloride composite material is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
(1) placing polyvinyl chloride powder, phase-change microcapsules, modified nano cellulose whiskers, sodium stearate, glycerol and an antioxidant 1010 in a high-speed stirrer, and stirring at the normal temperature at the rotating speed of 800-1000 r/min for 20-30 min to obtain a mixture;
(2) and (3) placing the mixture into a double-roller open mill, performing triangular bag making under the condition of 160-170 ℃, mixing for 10-15 min, and cooling at normal temperature to obtain the low-temperature polyvinyl chloride composite material.
The weight parts of the polyvinyl chloride powder, the phase change microcapsule, the modified nano cellulose whisker, the sodium stearate, the glycerol and the antioxidant 1010 are 80-100 parts of the polyvinyl chloride powder, 20-25 parts of the phase change microcapsule, 16-20 parts of the modified nano cellulose whisker, 8-10 parts of the sodium stearate, 4-5 parts of the glycerol and 0.4-0.5 part of the antioxidant 1010.
And (3) the triangular packaging times in the step (2) are 6-8.
The specific preparation steps of the modified nano cellulose whisker in the step (1) are as follows:
(1) adding absorbent cotton and vinyl trimethoxy silane into sulfuric acid, stirring for 30-40 min at a rotating speed of 160-180 r/min under a water bath condition of 60-70 ℃, adding deionized water, and adjusting the pH value to 7 to obtain a mixed suspension;
(2) and placing the mixed suspension in a centrifuge, centrifuging and separating at the normal temperature at the rotating speed of 5000-6000 r/min for 10-20 min, taking the lower-layer solid, and centrifuging and washing for 3-5 times by using deionized water to obtain the modified nano cellulose whisker.
The absorbent cotton comprises absorbent cotton, sulfuric acid, vinyl trimethoxy silane, 10-20 parts of deionized water, 100-200 parts of sulfuric acid with the mass fraction of 40%, 4-8 parts of vinyl trimethoxy silane and 100-200 parts of deionized water.
The pH adjustment in the step (1) adopts a sodium hydroxide solution with the mass fraction of 1%.
The phase-change microcapsule described in the step (1) comprises the following specific preparation steps:
(1) adding n-hexadecane and n-octadecane into liquid paraffin, and stirring at the normal temperature at the rotating speed of 200-250 r/min for 10-15 min to obtain paraffin mixed liquid;
(2) adding a mixed solution of sodium dodecyl sulfate, anhydrous calcium chloride and paraffin into 1/2 deionized water, placing the mixture into a high-shear emulsifying machine, stirring the mixture for 1 to 2 hours at the normal temperature at the rotating speed of 10000 to 12000r/min, and placing the mixture into an ultrasonic dispersion machine to perform ultrasonic treatment for 20 to 30 minutes at the power of 300 to 400W to obtain an emulsion;
(3) adding anhydrous sodium carbonate into deionized water, stirring uniformly, slowly dripping into the emulsion, and stirring at the rotating speed of 300-350 r/min for 3-4 h at normal temperature to obtain a mixed solution;
(4) and (3) placing the mixed solution into a decompression suction filter for suction filtration, washing the filter cake with deionized water for 3-5 times, and placing the filter cake into a drying oven at the temperature of 60-80 ℃ for drying for 1-2 hours to obtain the phase-change microcapsule.
The liquid paraffin, the n-hexadecane, the n-octadecane, the sodium dodecyl sulfate, the anhydrous calcium chloride, the anhydrous sodium carbonate and the deionized water are 10-20 parts by weight of the liquid paraffin, 5-10 parts by weight of the n-hexadecane, 5-10 parts by weight of the n-octadecane, 2-4 parts by weight of the sodium dodecyl sulfate, 12-24 parts by weight of the anhydrous calcium chloride, 8-16 parts by weight of the anhydrous sodium carbonate and 100-120 parts by weight of the deionized water.
And (3) the power of ultrasonic treatment in the step (2) is 300-400W.
And (4) the dropping rate of the sodium carbonate solution in the step (3) is 20-40 mL/min.
Compared with other methods, the method has the beneficial technical effects that:
(1) the invention takes liquid paraffin, n-hexadecane and n-octadecane as heat storage and preservation agents, and takes calcium carbonate as a wall material to coat the heat storage and preservation agents, thus preparing the low temperature resistant polyvinyl chloride composite material, the phase change material is a substance which changes form along with the temperature change and can provide latent heat, the process of changing the phase change material from solid state to liquid state or from liquid state to solid state is called as the phase change process, at the moment, the phase change material absorbs or releases a large amount of latent heat, when the ambient temperature reaches the melting point of the phase change material, the phase change material absorbs the heat and converts the heat from the solid state to the liquid state, so that the heat in the polyvinyl chloride is transferred, the heat reducing and temperature reducing effects are achieved, when the phase change material is in the cold environment lower than the melting point of the phase change, the temperature of the polyvinyl chloride is lower than the solidification temperature of the phase change material, the, the phase change microcapsule is formed by coating the phase change material in a wall material by a microcapsule technology to form tiny particles, the structure of the phase change microcapsule can be divided into two parts, the phase change microcapsule core material is arranged inside the phase change microcapsule, the phase change microcapsule can absorb or release a large amount of phase change latent heat in the phase change process, the particle size of the phase change microcapsule is small, the phase change microcapsule has a larger specific surface area, thereby having better heat transfer effect and effectively improving the cold resistance of polyvinyl chloride;
(2) the invention prepares a low temperature resistant polyvinyl chloride composite material by adding nano cellulose whiskers, wherein cellulose is a natural high molecular compound which is most widely distributed and rich in content in the nature, the natural cellulose is widely existed in cell walls of higher plants, some marine excystic animals, partial seaweed, fungi, bacteria and the like, compared with a synthetic high molecular compound, the cellulose also has the advantages of good biocompatibility, biodegradability, low price, renewability and the like, the cellulose is a linear polysaccharide polymer formed by combining D-glucopyranoside with beta-1, 4 glycosidic bonds, glucose units of the cellulose are not in a planar structure but in a chair conformation, in addition, each cellulose chain has direction asymmetry relative to the tail end of a molecular axis thereof, and strong hydrogen bond action is formed between cellulose macromolecular chains and inside the cellulose macromolecular chains, the surface of the nano-cellulose is chemically modified by using a silane coupling agent, a hydrophobic molecular chain segment can be grafted on the nano-cellulose, the interface between the nano-cellulose and polyvinyl chloride can be changed, the dispersibility of the nano-cellulose in the polyvinyl chloride is improved, when the polyvinyl chloride is acted by external force, the external force is transmitted to the nano-cellulose, and due to the nearly perfect arrangement of cellulose molecular chains, the structure of a crystal area in the cellulose molecular chains is compact, the contents of covalent bonds and hydrogen bonds between carbon and hydrogen oxygen in the interior are rich, so that the nano-cellulose has good mechanical properties, the crack can be effectively prevented from being further expanded, and the mechanical properties of the polyvinyl chloride are improved.
Detailed Description
Respectively weighing 10-20 parts of liquid paraffin, 5-10 parts of n-hexadecane, 5-10 parts of n-octadecane, 2-4 parts of sodium dodecyl sulfate, 12-24 parts of anhydrous calcium chloride, 8-16 parts of anhydrous sodium carbonate and 100-120 parts of deionized water according to parts by weight, adding the n-hexadecane and the n-octadecane into the liquid paraffin, stirring at the rotating speed of 200-250 r/min for 10-15 min at normal temperature to obtain a paraffin mixed solution, adding the sodium dodecyl sulfate, the anhydrous calcium chloride and the paraffin mixed solution into 1/2 deionized water, placing the mixture into a high-shear emulsifying machine, stirring at the rotating speed of 10000-12000 r/min at normal temperature for 1-2 h, placing the mixture into an ultrasonic dispersion machine, carrying out ultrasonic treatment at the power of 300-400W for 20-30 min to obtain an emulsion, adding the anhydrous sodium carbonate into the deionized water, slowly adding the mixture into the emulsion at the speed of 20-40 mL/min after uniform stirring, stirring at the normal temperature at the rotating speed of 300-350 r/min for 3-4 hours to obtain a mixed solution, placing the mixed solution in a reduced pressure filter for suction filtration, washing a filter cake for 3-5 times by using deionized water, and placing the filter cake in a drying oven at the temperature of 60-80 ℃ for drying for 1-2 hours to obtain a phase change microcapsule; respectively weighing 10-20 parts of absorbent cotton, 100-200 parts of sulfuric acid with the mass fraction of 40%, 4-8 parts of vinyl trimethoxy silane and 100-200 parts of deionized water, adding the absorbent cotton and the vinyl trimethoxy silane into the sulfuric acid, stirring for 30-40 min at the rotating speed of 160-180 r/min under the water bath condition of 60-70 ℃, adding the deionized water, dropwise adding a sodium hydroxide solution with the mass fraction of 1% to adjust the pH to 7 to obtain a mixed suspension, placing the mixed suspension in a centrifuge, centrifugally separating for 10-20 min at the rotating speed of 5000-6000 r/min at normal temperature, taking a lower layer of solid, and centrifugally washing for 3-5 times by using the deionized water to obtain the modified nano cellulose whisker; respectively weighing 80-100 parts by weight of polyvinyl chloride powder, 20-25 parts by weight of phase change microcapsule, 16-20 parts by weight of modified nano cellulose whisker, 8-10 parts by weight of sodium stearate, 4-5 parts by weight of glycerol and 0.4-0.5 part by weight of antioxidant 1010, placing the polyvinyl chloride powder, the phase change microcapsule, the modified nano cellulose whisker, the sodium stearate, the glycerol and the antioxidant 1010 in a high-speed stirrer, stirring at the normal temperature at the rotating speed of 800-1000 r/min for 20-30 min to obtain a mixture, placing the mixture in a double-roller open mill, performing triangular wrapping at the temperature of 160-170 ℃ for 6-8 times, mixing for 10-15 min, and cooling at the normal temperature to obtain the low-temperature polyvinyl chloride composite material.
Example 1
Respectively weighing 10 parts of liquid paraffin, 5 parts of n-hexadecane, 5 parts of n-octadecane, 2 parts of sodium dodecyl sulfate, 12 parts of anhydrous calcium chloride, 8 parts of anhydrous sodium carbonate and 100 parts of deionized water, adding the n-hexadecane and the n-octadecane into the liquid paraffin, stirring for 10min at the normal temperature at the rotating speed of 200r/min to obtain a paraffin mixed solution, adding the sodium dodecyl sulfate, the anhydrous calcium chloride and the paraffin mixed solution into 1/2 deionized water, placing the mixture into a high-shear emulsifying machine, stirring for 1h at the rotating speed of 10000r/min at the normal temperature, placing the mixture into an ultrasonic dispersion machine, carrying out ultrasonic treatment for 20min at the power of 300W to obtain an emulsion, adding the anhydrous sodium carbonate into the deionized water, slowly dripping the anhydrous sodium carbonate into the emulsion at the speed of 20mL/min after uniform stirring, stirring for 3h at the rotating speed of 300r/min at the normal temperature to obtain a mixed solution, placing the mixed solution into a vacuum suction filtration machine, washing the filter cake with deionized water for 3 times, and drying in an oven at 60 ℃ for 1h to obtain phase change microcapsules; respectively weighing 10 parts of absorbent cotton, 100 parts of sulfuric acid with the mass fraction of 40%, 4 parts of vinyl trimethoxy silane and 100 parts of deionized water according to parts by weight, adding the absorbent cotton and the vinyl trimethoxy silane into the sulfuric acid, stirring for 30min at the rotating speed of 160r/min under the water bath condition of 60 ℃, adding the deionized water, dropwise adding a sodium hydroxide solution with the mass fraction of 1% to adjust the pH to 7 to obtain a mixed suspension, placing the mixed suspension into a centrifuge, centrifugally separating for 10min at the rotating speed of 5000r/min at normal temperature, taking a lower-layer solid, and centrifugally washing for 3 times by using the deionized water to obtain modified nano-cellulose whiskers; respectively weighing 80 parts of polyvinyl chloride powder, 20 parts of phase change microcapsule, 16 parts of modified nano cellulose whisker, 8 parts of sodium stearate, 4 parts of glycerol and 0.4 part of antioxidant 1010 according to parts by weight, placing the polyvinyl chloride powder, the phase change microcapsule, the modified nano cellulose whisker, the sodium stearate, the glycerol and the antioxidant 1010 in a high-speed stirrer, stirring at the normal temperature at the rotating speed of 800r/min for 20min to obtain a mixture, placing the mixture in a double-roller open mill, performing triangular wrapping at 160 ℃ for 6 times, mixing for 10min, and cooling at the normal temperature to obtain the low-temperature polyvinyl chloride composite material.
Example 2
Respectively weighing 15 parts of liquid paraffin, 8 parts of n-hexadecane, 8 parts of n-octadecane, 3 parts of sodium dodecyl sulfate, 18 parts of anhydrous calcium chloride, 12 parts of anhydrous sodium carbonate and 110 parts of deionized water, adding the n-hexadecane and the n-octadecane into the liquid paraffin, stirring at the normal temperature at the rotating speed of 225r/min for 12min to obtain a paraffin mixed solution, adding the sodium dodecyl sulfate, the anhydrous calcium chloride and the paraffin mixed solution into 1/2 deionized water, placing the mixture into a high-shear emulsifying machine, stirring at the rotating speed of 11000r/min for 1h at the normal temperature, placing the mixture into an ultrasonic dispersion machine, carrying out ultrasonic treatment at the power of 350W for 25min to obtain an emulsion, adding the anhydrous sodium carbonate into the deionized water, slowly dripping the anhydrous sodium carbonate into the emulsion at the speed of 30mL/min after uniformly stirring, stirring at the rotating speed of 325r/min at the normal temperature for 3h to obtain a mixed solution, placing the mixed solution into a reduced-pressure suction filter, washing the filter cake with deionized water for 4 times, and drying in an oven at 70 ℃ for 1h to obtain phase change microcapsules; respectively weighing 15 parts of absorbent cotton, 150 parts of sulfuric acid with the mass fraction of 40%, 6 parts of vinyl trimethoxy silane and 150 parts of deionized water, adding the absorbent cotton and the vinyl trimethoxy silane into the sulfuric acid, stirring for 35min at the rotating speed of 170r/min under the water bath condition of 65 ℃, adding the deionized water, dropwise adding a sodium hydroxide solution with the mass fraction of 1% to adjust the pH to 7 to obtain a mixed suspension, placing the mixed suspension into a centrifuge, centrifugally separating for 15min at the rotating speed of 5500r/min at normal temperature, taking a lower-layer solid, and centrifugally washing for 4 times by using the deionized water to obtain modified nano-cellulose whiskers; and respectively weighing 90 parts of polyvinyl chloride powder, 22 parts of phase change microcapsule, 18 parts of modified nano cellulose whisker, 9 parts of sodium stearate, 4 parts of glycerol and 0.4 part of antioxidant 1010 according to parts by weight, placing the polyvinyl chloride powder, the phase change microcapsule, the modified nano cellulose whisker, the sodium stearate, the glycerol and the antioxidant 1010 in a high-speed stirrer, stirring at the rotating speed of 900r/min for 25min at normal temperature to obtain a mixture, placing the mixture in a double-roller open mill, performing triangular wrapping for 7 times at 165 ℃, mixing for 12min, and cooling at normal temperature to obtain the low-temperature polyvinyl chloride composite material.
Example 3
Respectively weighing 20 parts of liquid paraffin, 10 parts of n-hexadecane, 10 parts of n-octadecane, 4 parts of sodium dodecyl sulfate, 24 parts of anhydrous calcium chloride, 16 parts of anhydrous sodium carbonate and 120 parts of deionized water, adding the n-hexadecane and the n-octadecane into the liquid paraffin, stirring for 15min at the normal temperature at the rotating speed of 250r/min to obtain a paraffin mixed solution, adding the sodium dodecyl sulfate, the anhydrous calcium chloride and the paraffin mixed solution into 1/2 deionized water, placing the mixture into a high-shear emulsifying machine, stirring for 2h at the rotating speed of 12000r/min at the normal temperature, placing the mixture into an ultrasonic dispersion machine, carrying out ultrasonic treatment for 30min at the power of 400W to obtain an emulsion, adding the anhydrous sodium carbonate into the deionized water, slowly dripping the anhydrous sodium carbonate into the emulsion at the speed of 40mL/min after uniform stirring, stirring for 4h at the rotating speed of 350r/min at the normal temperature to obtain a mixed solution, placing the mixed solution into a decompression suction filter, washing the filter cake with deionized water for 5 times, and drying in an oven at 80 ℃ for 2h to obtain phase change microcapsules; respectively weighing 20 parts of absorbent cotton, 200 parts of sulfuric acid with the mass fraction of 40%, 8 parts of vinyl trimethoxy silane and 200 parts of deionized water according to parts by weight, adding the absorbent cotton and the vinyl trimethoxy silane into the sulfuric acid, stirring for 40min at the rotating speed of 180r/min under the water bath condition of 70 ℃, adding the deionized water, dropwise adding a sodium hydroxide solution with the mass fraction of 1% to adjust the pH to 7 to obtain a mixed suspension, placing the mixed suspension into a centrifuge, centrifugally separating for 20min at the rotating speed of 6000r/min at normal temperature, taking a lower-layer solid, and centrifugally washing for 5 times by using the deionized water to obtain modified nano-cellulose whiskers; and then respectively weighing 100 parts of polyvinyl chloride powder, 25 parts of phase change microcapsule, 20 parts of modified nano cellulose whisker, 10 parts of sodium stearate, 5 parts of glycerol and 0.5 part of antioxidant 1010 according to parts by weight, placing the polyvinyl chloride powder, the phase change microcapsule, the modified nano cellulose whisker, the sodium stearate, the glycerol and the antioxidant 1010 in a high-speed stirrer, stirring for 30min at the normal temperature at the rotating speed of 1000r/min to obtain a mixture, placing the mixture in a double-roller open mill, performing triangular bag packing for 8 times at the temperature of 170 ℃, mixing for 15min, and cooling at the normal temperature to obtain the low-temperature polyvinyl chloride composite material.
Comparative example: polyvinyl chloride composite material manufactured by Dongguan company.
The polyvinyl chloride composite materials prepared in the examples and the comparative examples are detected, and the specific detection is as follows:
tensile property: according to the GB/T1004-2006 standard, an electronic material universal testing machine is adopted to test the tensile strength and the elongation at break of the material, and the tensile speed is 50 mm/min.
Low-temperature impact: and testing the low-temperature impact strength of the sample by using a simple beam impact tester according to the GB/T2843-2008 standard.
The specific test results are shown in table 1.
Table 1 comparative table of property characterization
| Detecting items | Example 1 | Example 2 | Example 3 | Comparative example |
| Tensile strength/MPa | 21 | 21.5 | 22 | 15 |
| Elongation at break/% | 340 | 345 | 330 | 250 |
| Low temperature impact strength/kJ/m2 | 36.7 | 37 | 38 | 24.3 |
As can be seen from Table 1, the polyvinyl chloride composite material prepared by the invention has good mechanical properties and low-temperature impact strength.
Claims (10)
1. The preparation method of the low-temperature-resistant polyvinyl chloride composite material is characterized by comprising the following specific preparation steps:
(1) placing polyvinyl chloride powder, phase-change microcapsules, modified nano cellulose whiskers, sodium stearate, glycerol and an antioxidant 1010 in a high-speed stirrer, and stirring at the normal temperature at the rotating speed of 800-1000 r/min for 20-30 min to obtain a mixture;
(2) and (3) placing the mixture into a double-roller open mill, performing triangular bag making under the condition of 160-170 ℃, mixing for 10-15 min, and cooling at normal temperature to obtain the low-temperature polyvinyl chloride composite material.
2. The preparation method of the low-temperature-resistant polyvinyl chloride composite material according to claim 1, wherein the polyvinyl chloride powder, the phase-change microcapsule, the modified nanocellulose whisker, the sodium stearate, the glycerol and the antioxidant 1010 are 80-100 parts by weight of the polyvinyl chloride powder, 20-25 parts by weight of the phase-change microcapsule, 16-20 parts by weight of the modified nanocellulose whisker, 8-10 parts by weight of the sodium stearate, 4-5 parts by weight of the glycerol and 0.4-0.5 part by weight of the antioxidant 1010.
3. The method for preparing a low temperature resistant polyvinyl chloride composite material according to claim 1, wherein the triangular wrapping times in the step (2) are 6-8.
4. The preparation method of low temperature resistant polyvinyl chloride composite material according to claim 1, wherein the modified nanocellulose whiskers in step (1) are prepared by the following specific steps:
(1) adding absorbent cotton and vinyl trimethoxy silane into sulfuric acid, stirring for 30-40 min at a rotating speed of 160-180 r/min under a water bath condition of 60-70 ℃, adding deionized water, and adjusting the pH value to 7 to obtain a mixed suspension;
(2) and placing the mixed suspension in a centrifuge, centrifuging and separating at the normal temperature at the rotating speed of 5000-6000 r/min for 10-20 min, taking the lower-layer solid, and centrifuging and washing for 3-5 times by using deionized water to obtain the modified nano cellulose whisker.
5. The method for preparing the low-temperature-resistant polyvinyl chloride composite material according to claim 4, wherein the absorbent cotton, the sulfuric acid, the vinyltrimethoxysilane, 10-20 parts of the deionized water, 100-200 parts of the sulfuric acid with the mass fraction of 40%, 4-8 parts of the vinyltrimethoxysilane and 100-200 parts of the deionized water.
6. The method for preparing low temperature resistant polyvinyl chloride composite material according to claim 4, wherein the pH adjustment in step (1) is 1% sodium hydroxide solution by mass.
7. The method for preparing the low temperature resistant polyvinyl chloride composite material according to claim 1, wherein the phase change microcapsules in the step (1) are prepared by the following steps:
(1) adding n-hexadecane and n-octadecane into liquid paraffin, and stirring at the normal temperature at the rotating speed of 200-250 r/min for 10-15 min to obtain paraffin mixed liquid;
(2) adding a mixed solution of sodium dodecyl sulfate, anhydrous calcium chloride and paraffin into 1/2 deionized water, placing the mixture into a high-shear emulsifying machine, stirring the mixture for 1 to 2 hours at the normal temperature at the rotating speed of 10000 to 12000r/min, and placing the mixture into an ultrasonic dispersion machine to perform ultrasonic treatment for 20 to 30 minutes at the power of 300 to 400W to obtain an emulsion;
(3) adding anhydrous sodium carbonate into deionized water, stirring uniformly, slowly dripping into the emulsion, and stirring at the rotating speed of 300-350 r/min for 3-4 h at normal temperature to obtain a mixed solution;
(4) and (3) placing the mixed solution into a decompression suction filter for suction filtration, washing the filter cake with deionized water for 3-5 times, and placing the filter cake into a drying oven at the temperature of 60-80 ℃ for drying for 1-2 hours to obtain the phase-change microcapsule.
8. The method for preparing a low temperature resistant polyvinyl chloride composite material according to claim 7, wherein the liquid paraffin, n-hexadecane, n-octadecane, sodium dodecyl sulfate, anhydrous calcium chloride, anhydrous sodium carbonate, and deionized water are 10-20 parts by weight of liquid paraffin, 5-10 parts by weight of n-hexadecane, 5-10 parts by weight of n-octadecane, 2-4 parts by weight of sodium dodecyl sulfate, 12-24 parts by weight of anhydrous calcium chloride, 8-16 parts by weight of anhydrous sodium carbonate, and 100-120 parts by weight of deionized water.
9. The preparation method of the low temperature resistant polyvinyl chloride composite material according to claim 7, wherein the power of the ultrasonic treatment in the step (2) is 300-400W.
10. The method for preparing the low temperature resistant polyvinyl chloride composite material according to claim 7, wherein the dropping rate of the sodium carbonate solution in the step (3) is 20-40 mL/min.
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| CN112574719A (en) * | 2020-12-29 | 2021-03-30 | 凯盛石墨碳材料有限公司 | Preparation method of phase change energy storage material based on calcium carbonate nano vesicles |
| CN112848020A (en) * | 2020-12-31 | 2021-05-28 | 富思特新材料科技发展股份有限公司 | Method for reinforcing substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112574719A (en) * | 2020-12-29 | 2021-03-30 | 凯盛石墨碳材料有限公司 | Preparation method of phase change energy storage material based on calcium carbonate nano vesicles |
| CN112848020A (en) * | 2020-12-31 | 2021-05-28 | 富思特新材料科技发展股份有限公司 | Method for reinforcing substrate |
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