CN112500658A - Transparent PVC colloidal particle and preparation process thereof - Google Patents
Transparent PVC colloidal particle and preparation process thereof Download PDFInfo
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- CN112500658A CN112500658A CN202011464140.6A CN202011464140A CN112500658A CN 112500658 A CN112500658 A CN 112500658A CN 202011464140 A CN202011464140 A CN 202011464140A CN 112500658 A CN112500658 A CN 112500658A
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- 239000002245 particle Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 42
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 239000003381 stabilizer Substances 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 239000011347 resin Substances 0.000 claims abstract description 17
- 229920005989 resin Polymers 0.000 claims abstract description 17
- 235000012424 soybean oil Nutrition 0.000 claims abstract description 14
- 239000003549 soybean oil Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000004605 External Lubricant Substances 0.000 claims abstract description 8
- 239000004610 Internal Lubricant Substances 0.000 claims abstract description 8
- 239000004014 plasticizer Substances 0.000 claims abstract description 8
- 238000005520 cutting process Methods 0.000 claims abstract description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 43
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 238000001354 calcination Methods 0.000 claims description 17
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical group CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 16
- 239000007790 solid phase Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- IHBCFWWEZXPPLG-UHFFFAOYSA-N [Ca].[Zn] Chemical group [Ca].[Zn] IHBCFWWEZXPPLG-UHFFFAOYSA-N 0.000 claims description 8
- 239000012188 paraffin wax Substances 0.000 claims description 8
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 108010010803 Gelatin Proteins 0.000 claims description 6
- 229920000159 gelatin Polymers 0.000 claims description 6
- 239000008273 gelatin Substances 0.000 claims description 6
- 235000019322 gelatine Nutrition 0.000 claims description 6
- 235000011852 gelatine desserts Nutrition 0.000 claims description 6
- POZPMIFKBAEGSS-UHFFFAOYSA-K trisodium;2-hydroxypropane-1,2,3-tricarboxylate;trihydrate Chemical compound O.O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O POZPMIFKBAEGSS-UHFFFAOYSA-K 0.000 claims description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 239000008117 stearic acid Substances 0.000 claims 1
- 241000894006 Bacteria Species 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229920003023 plastic Polymers 0.000 abstract description 5
- 239000004033 plastic Substances 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 55
- 229920000915 polyvinyl chloride Polymers 0.000 description 54
- 239000000243 solution Substances 0.000 description 21
- 230000000844 anti-bacterial effect Effects 0.000 description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 238000005469 granulation Methods 0.000 description 7
- 230000003179 granulation Effects 0.000 description 7
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 7
- 239000000654 additive Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 4
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000012785 packaging film Substances 0.000 description 1
- 229920006280 packaging film Polymers 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000010094 polymer processing Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
Abstract
The application relates to the technical field of PVC plastics, in particular to transparent PVC colloidal particles and a preparation process thereof. The PVC colloidal particle comprises the following components in parts by weight: 90-110 parts of PVC resin; 20-80 parts of a plasticizer; 2-4 parts of epoxidized soybean oil; 3-5 parts of an environment-friendly stabilizer; 0.4-1 part of internal lubricant; 0.2-0.8 part of external lubricant; 4-6 parts of an antibacterial agent; the preparation process comprises the following steps: s1: uniformly mixing PVC resin, a plasticizer, epoxidized soybean oil, an environment-friendly stabilizer, an internal lubricant, an external lubricant and an antibacterial agent to obtain a mixture A; s2: and heating and stirring the mixture A to a molten state, extruding the molten mixture A, cooling, and cutting the cooled mixture A to obtain the PVC colloidal particles. Compositions/products of the present application the compositions may be used in toy manufacture, which has the advantage that bacteria are not prone to growth and reproduction on the toy.
Description
Technical Field
The application relates to the technical field of PVC plastics, in particular to transparent PVC colloidal particles and a preparation process thereof.
Background
Polyvinyl chloride (PVC), is a polymer obtained by polymerizing Vinyl Chloride Monomer (VCM) with initiators such as peroxides and azo compounds or under the action of light and heat according to a radical polymerization mechanism. Vinyl chloride homopolymers and vinyl chloride copolymers are collectively referred to as vinyl chloride resins. PVC is white powder with an amorphous structure, has small branching degree, starts to decompose at the glass transition temperature of 77-90 ℃ and about 170 ℃, has poor stability to light and heat, can decompose to generate hydrogen chloride when being exposed to the sun at the temperature of more than 100 ℃ or for a long time, further automatically catalyzes and decomposes to cause color change, and the physical and mechanical properties are also rapidly reduced. PVC has been the most widely used plastic in the world and is used in a very wide range of applications. The product has wide application in building materials, industrial products, daily necessities, floor leathers, floor tiles, artificial leathers, pipes, wires and cables, packaging films, bottles, foaming materials, sealing materials, fibers and the like.
The toy is few in the growth process of children, at present, PVC is a material frequently used in the manufacture of toys, but after children play with the toys, the toys are easily infected with microorganisms such as bacteria, so that the bacteria grow and propagate on the surfaces of the toys, when the children play with the toys next time, the bacteria are easily infected to the children, particularly, the children do not pay attention to sanitation, and often eat the toys without washing hands, so that hidden dangers are brought to the health of the children, and the improvement is needed.
Disclosure of Invention
In order to prevent bacteria from growing and propagating on toys easily, the application provides transparent PVC colloidal particles and a preparation process thereof.
First aspect, this application provides a transparent PVC micelle, adopts following technical scheme:
transparent PVC colloidal particles comprise the following components in parts by weight: 90-110 parts of PVC resin; 20-80 parts of a plasticizer; 2-4 parts of epoxidized soybean oil; 3-5 parts of an environment-friendly stabilizer;
0.4-1 part of internal lubricant; 0.2-0.8 part of external lubricant; 4-6 parts of an antibacterial agent. By adopting the technical scheme, the plasticizer can improve the performance of the high polymer material, increase the plasticity and strength of the plastic, reduce the production cost and improve the production benefit; the environment-friendly stabilizer is synthesized by using calcium salt, zinc salt, a lubricant, an antioxidant and the like as main components by adopting a special compounding process, and the environment-friendly stabilizer improves the heat stability of pvc and replaces active and unstable substituent groups; absorbing and neutralizing HCL released in the PVC processing process; the epoxidized soybean oil can play a good synergistic role with the environment-friendly stabilizer, so that the performance of the PVC colloidal particles is improved; the internal lubricant is used for reducing the internal friction force among polymer molecular chains in the polymer processing process, so that the processability is improved; the external lubricant is an additive which is added for reducing the friction between the polymer and the interface of the surface of the molding processing machine in the molding processing process, so that PVC is not easy to adhere to the machine; the use of the antibacterial agent enables the PVC colloidal particles to have antibacterial capacity, so that bacteria are not easy to grow and reproduce on toys prepared from the PVC colloidal particles, and the original color of the PVC colloidal particles is not influenced because the addition amount of the antibacterial agent is less.
Preferably, the antibacterial agent is prepared by the following steps: dissolving 10-16 parts by weight of zinc nitrate hexahydrate in 30-40 parts by weight of water, sequentially adding 1-2 parts by weight of sodium dodecyl sulfate, 12-18 parts by weight of triethylamine, 20-30 parts by weight of ethanol and 8-12 parts by weight of nano silver solution, stirring, carrying out hydrothermal reaction for a period of time, filtering, collecting a solid phase, and calcining to obtain the antibacterial agent.
By adopting the technical scheme, the triethylamine is an alkaline substance, so that zno is generated by the reaction of the zinc nitrate solution under the action of the triethylamine, and the form of zno is controlled by the sodium dodecyl sulfate and the ethanol in the generation process of zno, so that the zno and the nano-silver have good compatibility, and the antibacterial performance of the antibacterial agent is improved.
Preferably, the stirring time is 2-3h, the stirring temperature is 90-100 ℃, the calcining temperature is 400-500 ℃ and the calcining time is 1-2 h.
By adopting the technical scheme, the antibacterial agent can improve the antibacterial capability after being calcined.
Preferably, the calcination environment is an inert atmosphere.
Preferably, the nano silver is prepared by the following method: dissolving 3-5 parts by weight of silver nitrate into 20-26 parts by weight of water, adding 4-6 parts by weight of 5% gelatin solution, 6-8 parts by weight of sodium citrate trihydrate and 2-4 parts by weight of polyethylene glycol, and fully stirring in a dark place to obtain the nano-silver solution.
By adopting the technical scheme, the sodium citrate trihydrate plays a role of a reducing agent in the process of preparing the nano-silver solution, and simultaneously plays a role of a surfactant, so that the prepared nano-silver has good antibacterial capability together with polyethylene glycol and gelatin solution, and simultaneously, in the process of preparing zno, each component in the nano-silver solution can also participate in the preparation process of zno, so that zno and the nano-silver are better combined, and the antibacterial capability of the antibacterial agent is improved.
Preferably, when the nano silver is prepared, the stirring time is 0.5-1.5h, and the stirring temperature is 20-30 ℃.
In a second aspect, the application provides a transparent PVC colloidal particle and a preparation process thereof, and the following technical scheme is adopted:
a transparent PVC colloidal particle and a preparation process thereof are disclosed, wherein the PVC colloidal particle is prepared by the following steps:
s1: uniformly mixing PVC resin, a plasticizer, epoxidized soybean oil, an environment-friendly stabilizer, an internal lubricant, an external lubricant and an antibacterial agent to obtain a mixture A;
s2: and heating and stirring the mixture A to a molten state, extruding the molten mixture A, cooling, and cutting the cooled mixture A to obtain the PVC colloidal particles.
By adopting the technical scheme, the PVC resin and various additives are uniformly mixed, and then the uniformly mixed substances are heated and melted, so that chemical reaction occurs among the components, and the PVC colloidal particles are prepared.
In summary, the present application has the following beneficial effects: 1. the use of the antibacterial agent enables the PVC colloidal particles to have antibacterial capability, so that bacteria are not easy to grow and reproduce on toys prepared from the PVC colloidal particles.
2. The zinc nitrate solution reacts under the action of triethylamine to generate zno, the form of zno is controlled by the lauryl sodium sulfate and the ethanol in the generation process of zno, so that zno and nano-silver have good compatibility, and each component in the nano-silver solution can participate in the preparation process of zno, so that zno and the nano-silver are better combined, and the antibacterial performance of the antibacterial agent is improved.
3. The PVC resin and various additives are uniformly mixed, and then the uniformly mixed substances are heated and melted to cause chemical reaction among the components, so that the PVC colloidal particles are prepared.
Detailed Description
The present application will be described in further detail with reference to examples.
The source of the raw materials for the following examples is shown in table 1:
TABLE 1
Raw materials | Manufacturer of the product |
PVC resin | Wuhanxin Xiuyi chemical Co Ltd |
Nano silver (commercially available) | Hebei Saina nano materials science and technology Co., Ltd |
Examples
Example 1
A transparent PVC colloidal particle and a preparation process thereof comprise the following steps:
s1: sequentially adding 90 parts by weight of PVC resin, 20 parts by weight of dibutyl phthalate, 2 parts by weight of epoxidized soybean oil, 3 parts by weight of calcium-zinc stabilizer, 0.4 part by weight of stearic alcohol, 0.2 part by weight of paraffin and 4 parts by weight of antibacterial agent (the antibacterial agent is commercially available nano silver, and the average particle size of the nano silver is 20nm) into a mixer, and uniformly mixing, wherein the rotating speed of the mixer is 100r/min and the mixing time is 10min during mixing, so as to obtain a mixture A;
s2: heating and blending the mixture A in a screw extruder at 160 ℃ to enable the mixture A to be heated to be molten, extruding the molten mixture A on a die head of the extruder into strips, cooling the strips in a water cooling tank, and conveying the strips to a granulator for granulation to obtain the transparent PVC colloidal particles.
Example 2
A transparent PVC colloidal particle and a preparation process thereof comprise the following steps:
s1: sequentially adding 90 parts by weight of PVC resin, 20 parts by weight of dibutyl phthalate, 2 parts by weight of epoxidized soybean oil, 3 parts by weight of calcium-zinc stabilizer, 0.4 part by weight of stearic alcohol, 0.2 part by weight of paraffin and 4 parts by weight of antibacterial agent into a mixer, and uniformly mixing, wherein the rotating speed of the mixer is 100r/min and the mixing time is 10min during mixing, thus obtaining a mixture A;
s2: heating and blending the mixture A in a screw extruder at 160 ℃ to enable the mixture A to be heated to be molten, extruding the molten mixture A on a die head of the extruder into strips, cooling the strips in a water cooling tank, and conveying the strips to a granulator for granulation to obtain the transparent PVC colloidal particles.
The antibacterial agent is prepared by the following steps:
dissolving 10 parts by weight of zinc nitrate hexahydrate in 30 parts by weight of water, sequentially adding 1 part by weight of sodium dodecyl sulfate, 12 parts by weight of triethylamine, 20 parts by weight of ethanol and 0.8 part by weight of nano silver (sold in the market) with the average particle size of 20nm, stirring for 2 hours at 90 ℃ by using a magnetic stirrer at the rotating speed of 400 rpm, then putting the mixed solution into an autoclave, carrying out hydrothermal reaction for 12 hours at 140 ℃, filtering, collecting a solid phase, washing the solid phase by using acetone and water, putting the solid phase into a muffle furnace, and calcining for 1 hour at the calcining temperature of 400 ℃ under the nitrogen atmosphere environment to obtain the antibacterial agent.
Example 3
A transparent PVC colloidal particle and a preparation process thereof comprise the following steps:
s1: sequentially adding 90 parts by weight of PVC resin, 20 parts by weight of dibutyl phthalate, 2 parts by weight of epoxidized soybean oil, 3 parts by weight of calcium-zinc stabilizer, 0.4 part by weight of stearic alcohol, 0.2 part by weight of paraffin and 4 parts by weight of antibacterial agent into a mixer, and uniformly mixing, wherein the rotating speed of the mixer is 100r/min and the mixing time is 10min during mixing, thus obtaining a mixture A;
s2: heating and blending the mixture A in a screw extruder at 160 ℃ to enable the mixture A to be heated to be molten, extruding the molten mixture A on a die head of the extruder into strips, cooling the strips in a water cooling tank, and conveying the strips to a granulator for granulation to obtain the transparent PVC colloidal particles.
The antibacterial agent is prepared by the following steps:
dissolving 10 parts by weight of zinc nitrate hexahydrate in 30 parts by weight of water, sequentially adding 1 part by weight of sodium dodecyl sulfate, 12 parts by weight of triethylamine, 20 parts by weight of ethanol and 0.8 part by weight of nano silver solution with the average particle size of 20nm, stirring for 2 hours at 90 ℃ by using a magnetic stirrer, wherein the rotating speed of a stirrer is 400 revolutions per minute, then putting the mixed solution into an autoclave, carrying out hydrothermal reaction for 12 hours at 140 ℃, then filtering, collecting a solid phase, washing the solid phase by using acetone and water, putting the solid phase into a muffle furnace, and calcining for 1 hour at the calcining temperature of 400 ℃ in a nitrogen atmosphere environment to obtain the antibacterial agent.
The nano silver solution is prepared by the following steps:
dissolving 3 parts by weight of silver nitrate in 20 parts by weight of water, adding 4 parts by weight of 5% gelatin solution, 6 parts by weight of sodium citrate trihydrate and 2 parts by weight of polyethylene glycol 400, stirring for 0.5 hour in a dark place, and then stirring at the temperature of 20 ℃ to obtain the nano-silver solution.
Example 4
A transparent PVC colloidal particle and a preparation process thereof comprise the following steps:
s1: sequentially adding 110 parts by weight of PVC resin, 50 parts by weight of dibutyl phthalate, 3 parts by weight of epoxidized soybean oil, 4 parts by weight of calcium-zinc stabilizer, 0.7 part by weight of stearic alcohol, 0.8 part by weight of paraffin and 5 parts by weight of antibacterial agent into a mixer, and uniformly mixing, wherein the rotating speed of the mixer is 100r/min and the mixing time is 10min during mixing, thus obtaining a mixture A;
s2: and heating and blending the mixture A in a screw extruder at 180 ℃ to enable the mixture A to be heated to be molten, extruding the molten mixture A on a die head of the extruder into strips, cooling the strips in a water cooling tank, and conveying the strips to a granulator for granulation to obtain the transparent PVC colloidal particles.
The antibacterial agent is prepared by the following steps:
dissolving 16 parts by weight of zinc nitrate hexahydrate in 40 parts by weight of water, sequentially adding 1.5 parts by weight of sodium dodecyl sulfate, 15 parts by weight of triethylamine, 25 parts by weight of ethanol and 12 parts by weight of nano silver solution, stirring for 2.5 hours at 100 ℃ by using a magnetic stirrer, wherein the rotating speed of a stirrer is 400 revolutions per minute, then putting the mixed solution into an autoclave, carrying out hydrothermal reaction for 16 hours at 150 ℃, then filtering, collecting a solid phase, washing with acetone and water, calcining the solid phase in a muffle furnace for 2 hours in a nitrogen atmosphere environment, and obtaining the antibacterial agent at the calcining temperature of 450 ℃.
The nano silver solution is prepared by the following steps:
dissolving 4 parts by weight of silver nitrate in 26 parts by weight of water, adding 5 parts by weight of 5% gelatin solution, 7 parts by weight of sodium citrate trihydrate and 4 parts by weight of polyethylene glycol 400, stirring for 1.5 hours in a dark place, and then stirring at the temperature of 25 ℃ to obtain the nano-silver solution.
Example 5
A transparent PVC colloidal particle and a preparation process thereof comprise the following steps:
s1: sequentially adding 100 parts by weight of PVC resin, 80 parts by weight of dibutyl phthalate, 4 parts by weight of epoxidized soybean oil, 5 parts by weight of calcium-zinc stabilizer, 1 part by weight of stearic alcohol, 0.5 part by weight of paraffin and 6 parts by weight of antibacterial agent into a mixer, and uniformly mixing, wherein the rotating speed of the mixer is 100r/min and the mixing time is 10min during mixing, thus obtaining a mixture A;
s2: heating and blending the mixture A in a screw extruder at 170 ℃ to enable the mixture A to be heated to be molten, extruding the molten mixture A on a die head of the extruder into strips, cooling the strips in a water cooling tank, and conveying the strips to a granulator for granulation to obtain the transparent PVC colloidal particles.
The antibacterial agent is prepared by the following steps:
dissolving 13 parts by weight of zinc nitrate hexahydrate in 30 parts by weight of water, sequentially adding 2 parts by weight of sodium dodecyl sulfate, 18 parts by weight of triethylamine, 30 parts by weight of ethanol and 10 parts by weight of nano silver solution, stirring for 3 hours at 95 ℃ by using a magnetic stirrer, wherein the rotation speed of a stirrer is 400 revolutions per minute, then putting the mixed solution into an autoclave, carrying out hydrothermal reaction for 14 hours at 160 ℃, filtering, collecting a solid phase, washing with acetone and water, calcining the solid phase in a muffle furnace for 1.5 hours in a nitrogen atmosphere environment, and obtaining the antibacterial agent at the calcining temperature of 500 ℃.
The nano silver solution is prepared by the following steps:
dissolving 5 parts by weight of silver nitrate in 23 parts by weight of water, adding 6 parts by weight of 5% gelatin solution, 8 parts by weight of sodium citrate trihydrate and 3 parts by weight of polyethylene glycol 400, stirring for 1 hour in a dark place, and then stirring at the temperature of 30 ℃ to obtain the nano-silver solution.
Comparative example
Comparative example 1
A transparent PVC colloidal particle and a preparation process thereof comprise the following steps:
s1: sequentially adding 90 parts by weight of PVC resin, 20 parts by weight of dibutyl phthalate, 2 parts by weight of epoxidized soybean oil, 3 parts by weight of calcium-zinc stabilizer, 0.4 part by weight of stearic alcohol and 0.2 part by weight of paraffin into a mixer, and uniformly mixing, wherein the rotating speed of the mixer is 100r/min and the mixing time is 10min during mixing, thus obtaining a mixture A;
s2: heating and blending the mixture A in a screw extruder at 160 ℃ to enable the mixture A to be heated to be molten, extruding the molten mixture A on a die head of the extruder into strips, cooling the strips in a water cooling tank, and conveying the strips to a granulator for granulation to obtain the transparent PVC colloidal particles.
Comparative example 2
Example 2
A transparent PVC colloidal particle and a preparation process thereof comprise the following steps:
s1: sequentially adding 90 parts by weight of PVC resin, 20 parts by weight of dibutyl phthalate, 2 parts by weight of epoxidized soybean oil, 3 parts by weight of calcium-zinc stabilizer, 0.4 part by weight of stearic alcohol, 0.2 part by weight of paraffin and 4 parts by weight of additive into a mixer, and uniformly mixing, wherein the rotating speed of the mixer is 100r/min and the mixing time is 10min during mixing, thus obtaining a mixture A;
s2: heating and blending the mixture A in a screw extruder at 160 ℃ to enable the mixture A to be heated to be molten, extruding the molten mixture A on a die head of the extruder into strips, cooling the strips in a water cooling tank, and conveying the strips to a granulator for granulation to obtain the transparent PVC colloidal particles.
The additive is prepared by the following steps:
dissolving 10 parts by weight of zinc nitrate hexahydrate in 30 parts by weight of water, sequentially adding 1 part by weight of sodium dodecyl sulfate, 12 parts by weight of triethylamine and 20 parts by weight of ethanol, stirring for 2 hours at 90 ℃ by using a magnetic stirrer, wherein the rotating speed of a stirrer is 400 revolutions per minute, then putting the mixed solution into a high-pressure kettle, carrying out hydrothermal reaction for 12 hours at 140 ℃, then filtering, collecting a solid phase, washing the solid phase by using acetone and water, putting the solid phase into a muffle furnace, and calcining for 1 hour in a nitrogen atmosphere environment at the calcining temperature of 400 ℃ to obtain the additive.
TABLE 2 amounts of the components in examples 1-5, comparative examples 1-2 in parts by weight
Performance test
The same PVC rubber particles as those obtained in examples 1 to 5 and comparative examples 1 to 2 were prepared to obtain toys, and the PVC rubber particles obtained in examples 1 to 5 and comparative examples 1 to 2 were tested by using the method for testing the antibacterial property of antibacterial plastics of QB/T2591-2003 as a test standard.
TABLE 3 antibacterial Properties test
Escherichia coli (kill rate/%) | Staphylococcus aureus (kill rate.%) and its preparation method | |
Example 1 | 96 | 96 |
Example 2 | 90 | 90 |
Example 3 | 99 | 99 |
Example 4 | 99 | 99 |
Example 5 | 97 | 97 |
Comparative example 1 | 0 | 0 |
Comparative example 2 | 0 | 0 |
It can be seen from the combination of example 1, comparative example 2 and table 3 that the number of bacteria on the surface of the toy is greatly reduced when the nano silver is added to the PVC rubber particles, which indicates that the PVC rubber particles prepared in example 1 have good antibacterial effect, probably because the bacteria on the surface of the toy are killed due to the existence of the nano silver and the nano silver has good antibacterial effect on the bacteria after the nano silver is added to the PVC rubber particles, so that the bacteria are not easy to grow and propagate on the surface of the toy.
It can be seen from the combination of example 1 and example 3 and table 3 that, when nano silver is combined into zinc oxide, the antibacterial ability of the toy prepared from pvc colloidal particles is greatly enhanced, probably because zno prepared in the present application and nano silver have a good synergistic effect, so that the antibacterial ability of nano silver is stronger, and the antibacterial ability of the toy is greatly enhanced.
It can be seen from the combination of example 1 and example 2 and table 3 that, although the antibacterial ability of example 1 is stronger than that of example 2, which may be due to the more added amount of nano silver in example 1, the cost of nano silver is expensive, so if too much nano silver is used, the production cost is greatly increased, thereby reducing the competitiveness of the product.
It can be seen from the combination of example 2 and example 3 and table 3 that when the nano silver is added as the nano silver prepared in the present application during the preparation of the antibacterial agent, the antibacterial ability of the toy is greatly improved, probably because zno prepared in the present application has better compatibility with the nano silver prepared in the present application, so that the antibacterial ability of the nano silver is improved under the action of zno.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. The transparent PVC colloidal particle is characterized by comprising the following components in parts by weight:
90-110 parts of PVC resin;
20-80 parts of a plasticizer;
2-4 parts of epoxidized soybean oil;
3-5 parts of an environment-friendly stabilizer;
0.4-1 part of internal lubricant;
0.2-0.8 part of external lubricant;
4-6 parts of an antibacterial agent.
2. Transparent PVC rubber grain according to claim 1, characterized in that: the antibacterial agent is prepared by the following steps:
dissolving 10-16 parts by weight of zinc nitrate hexahydrate in 30-40 parts by weight of water, sequentially adding 1-2 parts by weight of sodium dodecyl sulfate, 12-18 parts by weight of triethylamine, 20-30 parts by weight of ethanol and 8-12 parts by weight of nano silver solution, stirring, carrying out hydrothermal reaction for a period of time, filtering, collecting a solid phase, and calcining to obtain the antibacterial agent.
3. Transparent PVC rubber grain according to claim 2, characterized in that: the stirring time is 2-3h, the stirring temperature is 90-100 ℃, the reaction time is 12-16h, the reaction temperature is 140-.
4. Transparent PVC rubber grain according to claim 2, characterized in that: during calcination, the calcination environment is inert atmosphere.
5. Transparent PVC rubber grain according to claim 2, characterized in that: the nano silver is prepared by the following method: dissolving 3-5 parts by weight of silver nitrate into 20-26 parts by weight of water, adding 4-6 parts by weight of 5% gelatin solution, 6-8 parts by weight of sodium citrate trihydrate and 2-4 parts by weight of polyethylene glycol, and fully stirring in a dark place to obtain the nano-silver solution.
6. Transparent PVC colloidal particles according to claim 5, characterized in that: when the nano silver is prepared, the stirring time is 0.5-1.5h, and the stirring temperature is 20-30 ℃.
7. Transparent PVC rubber grain according to claim 1, characterized in that: the plasticizer is dibutyl phthalate, the environment-friendly stabilizer is a calcium-zinc stabilizer, the internal lubricant is stearic acid alcohol, and the external lubricant is paraffin.
8. Transparent PVC colloidal particles and process for their preparation according to any of claims 1 to 7, characterized in that: the PVC colloidal particle is prepared by the following steps:
s1: uniformly mixing PVC resin, a plasticizer, epoxidized soybean oil, an environment-friendly stabilizer, an internal lubricant, an external lubricant and an antibacterial agent to obtain a mixture A;
s2: and heating and stirring the mixture A to a molten state, extruding the molten mixture A, cooling, and cutting the cooled mixture A to obtain the PVC colloidal particles.
9. The transparent PVC colloidal particle and the preparation process thereof according to claim 1, wherein the transparent PVC colloidal particle comprises the following steps: in the step S2, the heating temperature is 160-180 ℃.
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CN113549286A (en) * | 2021-08-05 | 2021-10-26 | 东莞鼎信实业有限公司 | Heat-resistant PVC colloidal particle and preparation method thereof |
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Cited By (4)
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CN113248844A (en) * | 2021-06-03 | 2021-08-13 | 浙江德首新型建材有限公司 | Environment-friendly PVC pipe and production process thereof |
CN113248844B (en) * | 2021-06-03 | 2022-07-05 | 浙江德首新型建材有限公司 | Environment-friendly PVC pipe and production process thereof |
CN113549285A (en) * | 2021-08-05 | 2021-10-26 | 东莞鼎信实业有限公司 | Anti-aging PVC colloidal particle and preparation process thereof |
CN113549286A (en) * | 2021-08-05 | 2021-10-26 | 东莞鼎信实业有限公司 | Heat-resistant PVC colloidal particle and preparation method thereof |
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