CN108864618B - High-antibacterial wear-resistant PVC resin material and preparation method thereof - Google Patents
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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
- C08L27/00—Compositions 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; Compositions of derivatives of such polymers
- C08L27/02—Compositions 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; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions 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; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L2205/00—Polymer mixtures characterised by other features
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- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention relates to the technical field of high polymer materials, and relates to a high-antibacterial wear-resistant PVC resin material and a preparation method thereof, wherein the high-antibacterial wear-resistant PVC resin material comprises the following components in parts by weight: 100 parts of PVC resin, 10-40 parts of antibacterial plasticizer, 8-12 parts of stabilizer, 1-3 parts of lubricant, 5-8 parts of antioxidant, 3-5 parts of impact modifier, 5-20 parts of filler and 1-3 parts of additive. According to the high-antibacterial wear-resistant PVC resin material and the preparation method thereof, the antibacterial functional auxiliary agent and the plasticizing-promoting modification auxiliary agent are integrated, the plasticizing effect is good, the antibacterial effect is strong, and the PVC material is matched with other components and has a synergistic effect, so that the antibacterial effect of the PVC material is good, the mechanical property and the weather resistance are excellent, and the application effect and the application field of PVC are greatly improved; in addition, the preparation method is simple, the preparation process conditions are easy to control, the preparation efficiency is high, the raw material price and the production energy consumption are low, and the method is suitable for large-scale production.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a high-antibacterial wear-resistant PVC resin material and a preparation method thereof.
Background
Pvc (pvc) thermoplastic resins obtained by polymerizing vinyl chloride under the action of an initiator are homopolymers of vinyl chloride, and homopolymers and copolymers of vinyl chloride are collectively referred to as vinyl chloride resins. The flame-retardant insulating material has the advantages of nonflammability, high chemical resistance, good electrical insulating property, stable physical and chemical properties, low price and the like, plays a very important role in industrial production, and is widely applied to the fields of industry, agriculture, traffic, buildings, electronic communication, household appliances, furniture, packaging, medical treatment and health care and the like. Also applied to products such as infusion tubes, infusion bags, oxygen masks, toys, shoes, pipelines, food packages, films and the like which are closely contacted with human bodies. Its global production is second only to polyethylene.
Because PVC is polar molecule, the interaction between molecular chains is large, the melt viscosity is high at high temperature, the thermal stability is poor, and the brittleness is large at low temperature, so the PVC without any processing aid can hardly be processed. The plasticizer is an auxiliary agent with the largest usage amount of PVC products, and makes a great contribution to large-scale industrial application of PVC. There are five hundred or more plasticizers that have been commercially produced to maximize the production and consumption of phthalates, such as dioctyl phthalate (DOP), dibutyl phthalate (DBP), and the like. However, such plasticizers are toxic and are banned from being used in children care appliances and toy products by the american Consumer Product Safety Committee (CPSC), and it is known from the new environmental protection law that the plasticizers are not toxic and are environmentally modified and the phthalate plasticizers are eliminated aiming at a wide range of PVC plastics, so that the development of novel environmentally-friendly and non-toxic plastic plasticizers becomes a hot point of plasticizer research. Meanwhile, because PVC has no antibacterial property, the surface of the product becomes dirty after a period of time, and various harmful microorganisms such as bacteria, mold, fungi and the like are bred. Particularly, harmful microorganisms are more easily propagated and spread under appropriate objective conditions such as temperature, humidity and the like, and cross infection can be caused by contact of different people, so that the PVC is a bacterial pollution source and a disease transmission source, brings harm to the health of people, and limits the application range of PVC to a certain extent. In order to enable PVC to have an antibacterial effect, some antibacterial agents are generally needed to be added, but common antibacterial agents are poor in compatibility with PVC resin and are easy to separate out in a PVC resin system like a plasticizer, so that the development of the PVC industry depends on new plasticizers and antibacterial agent products, and therefore, a PVC material with high stability, good compatibility, high mechanical strength and excellent antibacterial performance is urgently needed at present, so that the demand of people on diversification of PVC material products is met.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a high-antibacterial wear-resistant PVC resin material and a preparation method thereof, the invention integrates an antibacterial functional auxiliary agent and a plasticizing-promoting modification auxiliary agent, has good plasticizing effect and stronger antibacterial effect, and has important effects of improving material performance, increasing functions and reducing cost because the macromolecular structure ensures that the antibacterial functional auxiliary agent is not easy to precipitate in a PVC resin system; the PVC material has good antibacterial effect and excellent mechanical property and weather resistance by being matched with other components and having mutual synergistic effect, and the application effect and the application field of PVC are greatly improved; in addition, the preparation method is simple, the preparation process conditions are easy to control, the preparation efficiency is high, the raw material price and the production energy consumption are low, and the method is suitable for large-scale production.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-antibacterial wear-resistant PVC resin material is composed of the following components in parts by weight:
100 parts of PVC resin, 10-40 parts of antibacterial plasticizer, 8-12 parts of stabilizer, 1-3 parts of lubricant, 5-8 parts of antioxidant, 3-5 parts of impact modifier, 5-20 parts of filler and 1-3 parts of additive.
Further, the PVC resin is a low-polymerization-degree PVC resin containing 20-35 wt% of 800-typed medium-polymerization-degree PVC resin with an average polymerization degree of 500-typed, the particle size is 50-65 μm, 25-40 wt% of 1500-typed medium-polymerization-degree PVC resin with an average polymerization degree of 1200-typed, the particle size is 35-50 μm, 25-55 wt% of 2500-typed high-polymerization-degree PVC resin with an average polymerization degree of 2000-typed, the particle size is 10-30 μm, and the weight is based on the total weight of the PVC resin.
Further, the structural formula of the antibacterial plasticizer is as follows:
further, the stabilizer is an organic tin stabilizer or a calcium zinc stabilizer.
Further, the lubricant is prepared by compounding any two of stearic acid, glyceryl monostearate, polyethylene wax and silicone oil according to the mass ratio of 2: 1.
Further, the antioxidant is prepared by compounding an antioxidant 1076 and an antioxidant DLTDP according to the mass ratio of 3: 1.
Further, the impact modifier is one or more of chlorinated polyethylene, ACR resin and MBS resin.
Further, the filler is calcium carbonate or talcum powder which is activated by a silane coupling agent, and the particle size of the filler is 5-15 microns.
Further, the additive is borax.
A preparation method of a high-antibacterial wear-resistant PVC resin material specifically comprises the following steps:
step (I) preparation of antibacterial plasticizer:
(1) adding 1 part of phthalic anhydride and 3 parts of oleyl alcohol into a reaction container, uniformly mixing, heating to 60-70 ℃, adding a catalyst and a polymerization inhibitor, heating to 85-90 ℃ after the phthalic anhydride is melted, continuously stirring for 4-6 hours, cooling to room temperature, extracting a product with ethyl acetate, washing with water for 2-3 times, filtering, drying, and distilling under reduced pressure to remove the solvent to obtain an intermediate product;
(2) under the protection of inert gas, adding 1 part of the intermediate product in the step (1) into a reaction vessel, adding a solvent with the mass 2 times that of the intermediate product, stirring and mixing uniformly, then adding a catalyst and a polymerization inhibitor, stirring at room temperature for 1-2h, heating to 70 ℃, dissolving 3 parts of N- (4-aminophenyl) -2-hydroxybenzamide in the solvent with the mass 2 times that of the N- (4-aminophenyl) -2-hydroxybenzamide, dropwise adding the solution into the reactor, completing dropwise addition within 4h, quickly heating the reaction system to 85-90 ℃, continuously stirring for reaction for 10-15h, cooling to room temperature, washing with deionized water for 2-3 times, washing with a saturated sodium chloride solution for 2-3 times, drying an oil phase with anhydrous magnesium sulfate, decompressing and carrying out rotary evaporation to remove the solvent, thereby obtaining an antibacterial plasticizing assistant for PVC;
step (two), filler surface treatment:
adding calcium carbonate or talcum powder into the solution of silane coupling agent, and stirring and reacting for 3-4 hours at 80 ℃; then filtering, vacuum drying, grinding and sieving to obtain modified calcium carbonate or modified talcum powder; the mass of the silane coupling agent is 1-3% of that of the calcium carbonate or the talcum powder.
Step (III) preparation of PVC resin:
(1) the raw materials are stirred and mixed in a high-speed mixer according to the respective weight portion ratio, the raw materials are firstly mixed at low speed and then mixed at high speed, the mixing speed is 500-800 r/min, the temperature of the mixture is 100-110 ℃, the raw materials are stirred and mixed for 30min,
(2) discharging the mixture into a cooling mixer for cold stirring, cooling to 40 ℃, and discharging;
(3) and (3) feeding the cooled material into a double-screw extrusion granulator set, wherein the temperature of an extruder is 100-120 ℃ in the first stage, 150-165 ℃ in the second stage, 140-150 ℃ in the third stage and 180 ℃ in the head temperature, and extruding strips, and then carrying out a water-cooling granulation process and an air-cooling drying process to obtain the high-antibacterial wear-resistant PVC resin material.
The invention has the following beneficial effects:
(1) according to the high-antibacterial wear-resistant PVC resin material and the preparation method thereof, PVC resin raw materials with different polymerization degrees are selected, so that the viscosity of PVC in the processing process can be conveniently adjusted by the use of the product, PVC molecular chains with different polymerization degrees interact in the melting and blending process, the processing plasticity can be ensured, the mechanical strength of the PVC resin can be ensured, the plasticizing time is short, and the leveling property in the processing and using processes is good.
(2) According to the high-antibacterial wear-resistant PVC resin material and the preparation method thereof, the self-made antibacterial plasticizer integrates the antibacterial functional additive and the plasticizing-promoting modification additive, the plasticizing effect is good, the macromolecular structure enables the antibacterial functional additive not to be easily separated out in a PVC resin system, the important effects on material performance improvement, function increase and cost reduction are achieved, the synergistic antibacterial effect is more remarkable (the antibacterial rate can reach more than 99%) by matching with the additive borax, the sterilization spectrum is wider, the application effect and the application field of PVC are greatly improved, and the excellent antibacterial and bactericidal performance enables the PVC resin material to be applied to the fields of medical treatment, biology, aerospace and the like.
(3) According to the high-antibacterial wear-resistant PVC resin material and the preparation method thereof, the used lubricant and the impact modifier have good compatibility in PVC resin, so that the performances of the lubricant and the impact modifier are mutually compensated, the components of the composition are more uniform, the quality is more stable, the optimal cold resistance and wear resistance are generated by mutual reinforcement, and the high-antibacterial wear-resistant PVC resin material can be widely applied to fibers, packages and the like in the fields of textiles, light industry and the like.
(4) According to the high-antibacterial wear-resistant PVC resin material and the preparation method thereof, the environment-friendly organic tin or calcium zinc stabilizer is used, the stability of the PVC in the high-temperature processing process is improved, the processing fluidity of the PVC is improved, the modified filler is combined, and the modified filler, the impact modifier and the matrix resin have good interface interaction, so that the stress can be effectively transmitted, the mechanical property of a PVC system is effectively improved, the impact strength and the tensile property of the PVC are obviously improved, the processing and the forming are facilitated, and the good mechanical property can be applied to the fields of chemical engineering, rail transit, new energy, electronics and the like.
(5) The high-antibacterial wear-resistant PVC resin material and the preparation method thereof have the advantages of simple and easy operation, easily controlled preparation process conditions, environment-friendly and pollution-free process, high preparation efficiency, low raw material price and low production energy consumption, and are very suitable for large-scale production.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is an infrared spectrum of the antibacterial plasticizing adjuvant prepared according to the present invention.
FIG. 2 is a nuclear magnetic spectrum of the antibacterial plasticizing adjuvant prepared by the present invention.
Detailed Description
The present invention will now be described in further detail with reference to examples.
Example 1
A high-antibacterial wear-resistant PVC resin material is composed of the following components in parts by weight:
100 parts of PVC resin, 30 parts of antibacterial plasticizer, 10 parts of calcium-zinc stabilizer, 3 parts of lubricant compounded by stearic acid and glyceryl monostearate according to the proportion of 2:1, 5 parts of antioxidant compounded by antioxidant 1076 and antioxidant DLTDP according to the proportion of 3:1, 5 parts of ACR resin, 15 parts of modified calcium carbonate with the particle size of 5 mu m and 2 parts of borax.
The above-mentioned PVC resin is a low polymerization degree PVC resin containing 30% by weight of a medium polymerization degree PVC resin having an average polymerization degree of 600, a particle size of 60 μm, 35% by weight of a medium polymerization degree PVC resin having an average polymerization degree of 1300, a particle size of 40 μm, 35% by weight of a high polymerization degree PVC resin having an average polymerization degree of 2200, and a particle size of 20 μm, based on the total weight of the PVC resin.
A preparation method of a high-antibacterial wear-resistant PVC resin material specifically comprises the following steps:
step (I) preparation of antibacterial plasticizer:
(1) adding 1 part of phthalic anhydride and 3 parts of oleyl alcohol into a reaction container, uniformly mixing, heating to 60-70 ℃, adding a catalyst and a polymerization inhibitor, heating to 90 ℃ after the phthalic anhydride is melted, continuously stirring for 6 hours, cooling to room temperature, extracting a product with ethyl acetate, washing with water for 2-3 times, filtering, drying, and distilling under reduced pressure to remove the solvent to obtain an intermediate product;
(2) under the protection of inert gas, adding 1 part of the intermediate product in the step (1) into a reaction vessel, adding a solvent with the mass 2 times that of the intermediate product, stirring and mixing uniformly, then adding a catalyst and a polymerization inhibitor, stirring at room temperature for 1-2h, heating to 70 ℃, dissolving 3 parts of N- (4-aminophenyl) -2-hydroxybenzamide in the solvent with the mass 2 times that of the N- (4-aminophenyl) -2-hydroxybenzamide, dropwise adding the solution into the reactor, dripping within 4h, quickly heating the reaction system to 90 ℃, continuously stirring for reaction for 15h, cooling to room temperature, washing with deionized water for 2-3 times, washing with a saturated sodium chloride solution for 2-3 times, drying an oil phase with anhydrous magnesium sulfate, decompressing and rotary steaming to remove the solvent, thereby obtaining the antibacterial plasticizing assistant for PVC;
FTIR(KBr)：3433cm-1is a characteristic peak of hydroxyl group, 1716cm-1Is a stretching vibration absorption peak of ester carbonyl of 2925cm-1And 2854cm-1Is a characteristic peak of methyl and methylene on the molecular chain of the auxiliary agent, 1654cm-1Is an amide bond characteristic peak, a C-N characteristic peak of 1288cm-1，1600cm-1No peak of carbon-carbon double bond appears, which indicates that the double bond reaction is complete, and the stretching vibration peak of the benzene ring in the infrared spectrogram is obvious, as shown in the infrared spectrogram of figure 1.
The nuclear magnetic spectrum is shown in figure 1, and the nuclear magnetic test result is as follows:
1H-NMR(400MHz,DMSO-d6)δ11.13(p，2H)，9.93(n，2H)，8.05(m，2H)，7.89(l，2H),7.71(k，2H)，7.42(r，6H)，6.95(j，4H)，6.77(i，4H)，4.57(g，2H),4.33(f，4H),2..41(e，2H),1.78(d，4H),1.43(k，12H),7.71(b，22H),7.71(a，6H)。
step (two), filler surface treatment:
adding calcium carbonate or talcum powder into the solution of silane coupling agent, and stirring and reacting for 3-4 hours at 80 ℃; then filtering, vacuum drying, grinding and sieving to obtain modified calcium carbonate or modified talcum powder; the mass of the silane coupling agent is 3% of that of the calcium carbonate or the talcum powder.
Step (III) preparation of PVC resin:
(1) the raw materials are stirred and mixed in a high-speed mixer according to the respective weight portion ratio, the raw materials are firstly mixed at low speed and then mixed at high speed, the mixing speed is 500-800 r/min, the temperature of the mixture is 100-110 ℃, the raw materials are stirred and mixed for 30min,
(2) discharging the mixture into a cooling mixer for cold stirring, cooling to 40 ℃, and discharging;
(3) and (3) feeding the cooled material into a double-screw extrusion granulator set, wherein the temperature of an extruder is 100-120 ℃ in the first stage, 150-165 ℃ in the second stage, 140-150 ℃ in the third stage and 180 ℃ in the head temperature, and extruding strips, and then carrying out a water-cooling granulation process and an air-cooling drying process to obtain the high-antibacterial wear-resistant PVC resin material.
Examples 2-5 and comparative examples 1-4 differ from example 1 as indicated in table 1:
TABLE 1
The preparation method of the high antibacterial and wear-resistant PVC resin material of the examples 2-5 and the comparative examples 1-4 is the same as that of the example 1.
And (3) performance detection: the tests were carried out on the high antibacterial and abrasion-resistant PVC resin materials obtained in examples 1 to 5 and comparative examples 1 to 4, and the results of the respective performance tests are shown in Table 2:
table 2 performance analysis data
As can be seen from the performance analysis data in Table 2, the PVC resin material with high antibacterial and wear-resistant performances prepared by the embodiment of the invention has the advantages of obvious plasticizing effect, good cold resistance and wear resistance, high tensile strength, good antibacterial performance, antibacterial rate of more than 99%, antifouling performance of 4 grade, and obvious deterioration of the performance of the PVC resin material due to the loss of core components in the comparative example.
In light of the above-described embodiments of the present invention, it is clear that many modifications and variations can be made by the worker skilled in the art without departing from the scope of the present invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (9)
1. The high-antibacterial wear-resistant PVC resin material is characterized in that: the composition comprises the following components in parts by weight:
100 parts of PVC resin, 10-40 parts of antibacterial plasticizer, 8-12 parts of stabilizer, 1-3 parts of lubricant, 5-8 parts of antioxidant, 3-5 parts of impact modifier, 5-20 parts of filler and 1-3 parts of additive;
the structural formula of the antibacterial plasticizer is as follows:
2. the highly antibacterial and wear-resistant PVC resin material as claimed in claim 1, wherein: the PVC resin is low-polymerization-degree PVC resin with 20-35 wt% of average polymerization degree of 500-800, and the particle size is 50-65 μm; 25-40 wt% of medium polymerization degree PVC resin with average polymerization degree of 1200-1500, and the particle size is 35-50 μm; 25-55 wt% of high polymerization degree PVC resin with average polymerization degree of 2000-2500, and the particle size is 10-30 μm based on the total weight of the PVC resin.
3. The highly antibacterial and wear-resistant PVC resin material as claimed in claim 1, wherein: the stabilizer is organic tin or calcium zinc stabilizer.
4. The highly antibacterial and wear-resistant PVC resin material as claimed in claim 1, wherein: the lubricant is prepared by compounding any two of stearic acid, glyceryl monostearate, polyethylene wax and silicone oil according to the mass ratio of 2: 1.
5. The highly antibacterial and wear-resistant PVC resin material as claimed in claim 1, wherein: the antioxidant is compounded by antioxidant 1076 and antioxidant DLTDP according to the mass ratio of 3: 1.
6. The highly antibacterial and wear-resistant PVC resin material as claimed in claim 1, wherein: the impact modifier is one or more of chlorinated polyethylene, ACR resin and MBS resin.
7. The highly antibacterial and wear-resistant PVC resin material as claimed in claim 1, wherein: the filler is calcium carbonate or talcum powder subjected to activation treatment by a silane coupling agent, and the particle size of the filler is 5-15 micrometers.
8. The highly antibacterial and wear-resistant PVC resin material as claimed in claim 1, wherein: the additive is borax.
9. A method for preparing the highly antibacterial and wear-resistant PVC resin material as claimed in any one of claims 1 to 8, comprising the steps of:
step (I) preparation of antibacterial plasticizer:
(1) adding 1 part of phthalic anhydride and 3 parts of oleyl alcohol into a reaction container, uniformly mixing, heating to 60-70 ℃, adding a catalyst and a polymerization inhibitor, heating to 85-90 ℃ after the phthalic anhydride is melted, continuously stirring for 4-6 hours, cooling to room temperature, extracting a product with ethyl acetate, washing with water for 2-3 times, filtering, drying, and distilling under reduced pressure to remove the solvent to obtain an intermediate product;
(2) under the protection of inert gas, adding 1 part of the intermediate product in the step (1) into a reaction vessel, adding a solvent with the mass 2 times that of the intermediate product, stirring and mixing uniformly, then adding a catalyst and a polymerization inhibitor, stirring at room temperature for 1-2h, heating to 70 ℃, dissolving 3 parts of N- (4-aminophenyl) -2-hydroxybenzamide in the solvent with the mass 2 times that of the N- (4-aminophenyl) -2-hydroxybenzamide, dropwise adding the solution into the reactor, completing dropwise addition within 4h, quickly heating the reaction system to 85-90 ℃, continuously stirring for reaction for 10-15h, cooling to room temperature, washing with deionized water for 2-3 times, washing with a saturated sodium chloride solution for 2-3 times, drying an oil phase with anhydrous magnesium sulfate, decompressing and carrying out rotary evaporation to remove the solvent, thereby obtaining an antibacterial plasticizing assistant for PVC;
step (two), filler surface treatment:
adding calcium carbonate or talcum powder into the solution of silane coupling agent, and stirring and reacting for 3-4 hours at 80 ℃; then filtering, vacuum drying, grinding and sieving to obtain modified calcium carbonate or modified talcum powder; the mass of the silane coupling agent is 1-3% of that of the calcium carbonate or the talcum powder;
step (III) preparation of PVC resin:
(1) the raw materials are stirred and mixed in a high-speed mixer according to the respective weight portion ratio, the raw materials are firstly mixed at low speed and then mixed at high speed, the mixing speed is 500-800 r/min, the temperature of the mixture is 100-110 ℃, the raw materials are stirred and mixed for 30min,
(2) discharging the mixture into a cooling mixer for cold stirring, cooling to 40 ℃, and discharging;
(3) and (3) feeding the cooled material into a double-screw extrusion granulator set, wherein the temperature of an extruder is 100-120 ℃ in the first stage, 150-165 ℃ in the second stage, 140-150 ℃ in the third stage and 180 ℃ in the head temperature, and extruding strips, and then carrying out a water-cooling granulation process and an air-cooling drying process to obtain the high-antibacterial wear-resistant PVC resin material.
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