CN109735022B - Preparation method of high-weather-resistance printing base film - Google Patents
Preparation method of high-weather-resistance printing base film Download PDFInfo
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- CN109735022B CN109735022B CN201811621897.4A CN201811621897A CN109735022B CN 109735022 B CN109735022 B CN 109735022B CN 201811621897 A CN201811621897 A CN 201811621897A CN 109735022 B CN109735022 B CN 109735022B
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Abstract
The invention discloses a preparation method of a high-weather-resistance printing base film, and relates to the technical field of base films. The invention comprises the following raw materials in parts by mass: 80-100 parts of PVC resin, 1-5 parts of antioxidant, 1-5 parts of weather-resistant auxiliary agent, 10-15 parts of EVA (ethylene vinyl acetate), 10-15 parts of CPE (chlorinated polyethylene), 5-10 parts of organic tin stabilizer, 4-6 parts of MBS (methyl methacrylate-butadiene-styrene) resin, 3-6 parts of internal lubricant, 4-6 parts of external lubricant and 2-4 parts of ACR (acrylate copolymer) auxiliary agent; the invention adopts SiO2Nano Ni (OH)2The film paving liquid prepared from the raw materials can form an alloying layer composite structure on the printing base film, obviously improves the weather resistance and structural strength of the printing base film, and has stronger resistance to the external severe environment.
Description
The technical field is as follows:
the invention relates to the technical field of base films, in particular to a preparation method of a high-weather-resistance printing base film.
Background art:
PVC is white powder with an amorphous structure, the branching degree is small, the relative density is about 1.4, the glass transition temperature is 77-90 ℃, decomposition starts at about 170 ℃, the stability to light and heat is poor, the PVC can be decomposed to generate hydrogen chloride at more than 100 ℃ or after long-time sunshine insolation, further the hydrogen chloride is automatically catalyzed and decomposed to cause color change, the physical and mechanical properties are also rapidly reduced, and a stabilizer must be added in practical application to improve the stability to heat and light.
The PVC floor has many excellent characteristics, such as moisture resistance, mildew resistance, water resistance, wear resistance and the like, and is not easy to age and deform when used indoors. However, the structural strength and weather resistance of the PVC floor are not significant, and when the PVC floor is subjected to severe external environments such as cold, heat, corrosion, impact, etc., the PVC floor is easily damaged, thereby affecting the use performance thereof.
The most key component of the PVC floor is a surface layer composite floor film, which plays roles of surface decoration, wear resistance, weather resistance, corrosion resistance and the like and has important influence on the service life of the floor film. At present, the floor film technology is not developed and researched in China, and is in a technical blank state. In view of this, the current companies develop great efforts to develop the technology of the key preparation technology of the floor film, and pay more attention to the development of the formula.
The invention content is as follows:
the invention aims to provide a preparation method of a high-weather-resistance printing base film which is stable in structure and has strong resistance to the external severe environment.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
the preparation method of the high-weather-resistance printing base film comprises the following steps:
(1) putting 80-100 parts of PVC resin, 1-5 parts of antioxidant, 1-5 parts of weather-resistant auxiliary agent, 10-15 parts of EVA, 10-15 parts of CPE, 5-10 parts of organic tin stabilizer, 4-6 parts of MBS resin, 3-6 parts of internal lubricant, 4-6 parts of external lubricant and 2-4 parts of ACR auxiliary agent into a mixer for mixing;
(2) banburying, rolling, cooling, rolling and warehousing and curing are carried out for 12 hours to form a printing base film;
(3) spreading a film on the printing base film, and firing in a vulcanizing machine to obtain a semi-finished product;
(4) curing the semi-finished product for 12 hours;
(5) and packaging and warehousing the finished product after the detection is qualified.
The preparation method of the weather-resistant auxiliary agent comprises the following steps: adding hydroxymethyl cellulose into deionized water, stirring at 30 deg.C for 10-15min, adding beta-hydroxybutyric acid and tetraethyl titanate, heating to reflux state, stirring for 0.5-4h while maintaining the temperature, filtering while hot, washing with deionized water to remove impurities, and drying to constant weight.
The mass ratio of the hydroxymethyl cellulose to the beta-hydroxybutyric acid to the tetraethyl titanate is 4-6: 3-5: 0.01-0.02.
The antioxidant is selected from thiodipropionic acid diester or phosphite ester.
The internal lubricant is selected from one of paraffin, stearic acid and mineral oil.
The external lubricant is selected from one of polyethylene wax and low molecular weight polypropylene.
The organic tin stabilizer is adopted, so that the processing stability and the thermal stability time of the product are improved; the MBS resin is taken as an additive, so that the mechanical property of the product is greatly improved; the ACR auxiliary agent improves the processing adaptability of the product; an internal lubricant to reduce friction between molecules during processing; the external lubricant reduces the friction between the PVC resin and equipment in the processing process and improves the demoulding performance.
The polymerization degree of the PVC resin is 1000-1300.
Further, the preparation method of the membrane spreading solution for spreading the membrane in the step (3) comprises the following steps:
(1) modification of flexible graphite: adding flexible graphite into deionized water, stirring uniformly, adding a silane coupling agent and a chain extender, heating to a reflux state, keeping the temperature and stirring for 0.5-2h, filtering while hot, washing the obtained solid with deionized water to remove impurities, drying at the temperature of 110 ℃ to constant weight, sealing and standing at the temperature of-3-0 ℃, the temperature of 20-25 ℃, the temperature of 3-5 ℃, and standing for 30-50min each time;
(2) preparing a composite liquid: mixing nano SiO2And nano Ni (OH)2Adding the powder into absolute ethyl alcohol, and performing ultrasonic dispersion for 30-50 min;
(3) mixing: and (2) adding the modified flexible graphite in the step (1) into the composite liquid, and performing ultrasonic dispersion for 0.5-1.5h to obtain a membrane spreading liquid.
The mass ratio of the flexible graphite to the silane coupling agent to the chain extender is 3-5: 0.3-0.5: 0.02-0.04.
The nano SiO2Nano Ni (OH)2The mass ratio of the powder to the absolute ethyl alcohol is 10-15: 6-10: 60-80.
Further, the nanometer Ni (OH)2The concentration of the powder is 1-8g/L, and the particle size is 70-120 nm.
The invention has the beneficial effects that:
(1) the invention adopts SiO2Nano Ni (OH)2The film paving liquid prepared from the raw materials can form an alloying layer composite structure on the printing base film, so that the weather resistance and the structural strength of the printing base film are obviously improved, and the printing base film has stronger resistance to the external severe environment;
(2) the silane coupling agent is coupled under the action of the chain extender and is adsorbed in the small holes of the flexible graphite, so that the flexible graphite is modified, the film layer can be firmly adsorbed on the printing base film and the binding material and cannot fall off or crack, and the weather resistance and the mechanical strength of the printing base film are further enhanced;
(3) the weather-resistant auxiliary agent prepared by taking the hydroxymethyl cellulose and the beta-hydroxybutyric acid as raw materials can enhance the tightness of a film layer and a floor due to the cohesive property and the reaction activity of the structure of the weather-resistant auxiliary agent, and meanwhile, the weather-resistant auxiliary agent is added into a printing base film, so that the connectivity among the raw materials can be improved, and further the weather resistance of the printing base film is improved.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
Preparation of high-weather-resistance printing base film:
(1) putting 80 parts of PVC resin, 2 parts of thiodipropionic acid diester, 4 parts of weather-resistant additive, 10 parts of EVA (ethylene vinyl acetate), 12 parts of CPE (chlorinated polyethylene) compound, 6 parts of organic tin stabilizer, 5 parts of MBS (methyl methacrylate-butadiene-styrene) resin, 4 parts of stearic acid, 5 parts of polyethylene wax and 2 parts of ACR (acrylate copolymer) additive into a mixer for mixing;
(2) banburying, rolling, cooling, rolling and warehousing and curing are carried out for 12 hours to form a printing base film;
(3) spreading a film on the printing base film, and firing in a vulcanizing machine to obtain a semi-finished product;
(4) curing the semi-finished product for 12 hours;
(5) and packaging and warehousing the finished product after the detection is qualified.
Preparing a weather-resistant auxiliary agent: adding 4 parts of hydroxymethyl cellulose into deionized water, stirring for 10min at 30 ℃, then adding 3 parts of beta-hydroxybutyric acid and 0.01 part of tetraethyl titanate, heating to a reflux state, keeping the temperature and stirring for 2h, filtering while hot, washing with deionized water to remove impurities, and drying to constant weight.
Preparing a membrane laying liquid:
(1) modification of flexible graphite: adding 4 parts of flexible graphite into deionized water, stirring uniformly, adding 0.3 part of silane coupling agent KH550 and 0.02 part of trimethylolpropane, heating to a reflux state, keeping the temperature and stirring for 1h, filtering while hot, washing the obtained solid with deionized water to remove impurities, drying at the temperature of 100 ℃ plus 110 ℃ to constant weight, sealing and standing at the temperature of-3 ℃, 22 ℃ and 3 ℃, wherein the standing time is 30min each time;
(2) preparing a composite liquid: mixing 12 parts of nano SiO2And 8 parts of nano Ni (OH)2Adding the powder into 70 parts of absolute ethyl alcohol, and performing ultrasonic dispersion for 40 min;
(3) mixing: and (3) adding the modified flexible graphite in the step (1) into the composite liquid, and performing ultrasonic dispersion for 1h to obtain a membrane spreading liquid.
Example 2
Preparation of high-weather-resistance printing base film:
(1) 100 parts of PVC resin, 4 parts of phosphite ester, 4 parts of weather-resistant additive, 12 parts of EVA (ethylene vinyl acetate), 12 parts of CPE (chlorinated polyethylene), 7 parts of organic tin stabilizer, 5 parts of MBS (methyl methacrylate-butadiene-styrene) resin, 6 parts of stearic acid, 5 parts of polyethylene wax and 4 parts of ACR (acrylate copolymer) additive are put into a mixer for mixing;
(2) banburying, rolling, cooling, rolling and warehousing and curing are carried out for 12 hours to form a printing base film;
(3) spreading a film on the printing base film, and firing in a vulcanizing machine to obtain a semi-finished product;
(4) curing the semi-finished product for 12 hours;
(5) and packaging and warehousing the finished product after the detection is qualified.
Preparing a weather-resistant auxiliary agent: adding 4 parts of hydroxymethyl cellulose into deionized water, stirring for 10min at 30 ℃, then adding 3 parts of beta-hydroxybutyric acid and 0.01 part of tetraethyl titanate, heating to a reflux state, keeping the temperature and stirring for 2h, filtering while hot, washing with deionized water to remove impurities, and drying to constant weight.
Preparing a membrane laying liquid:
(1) modification of flexible graphite: adding 4 parts of flexible graphite into deionized water, stirring uniformly, adding 0.3 part of silane coupling agent KH550 and 0.02 part of trimethylolpropane, heating to a reflux state, keeping the temperature and stirring for 1h, filtering while hot, washing the obtained solid with deionized water to remove impurities, drying at the temperature of 100 ℃ plus 110 ℃ to constant weight, sealing and standing at the temperature of-3 ℃, 22 ℃ and 3 ℃, wherein the standing time is 30min each time;
(2) preparing a composite liquid: mixing 12 parts of nano SiO2And 8 parts of nano Ni (OH)2Adding the powder into 70 parts of absolute ethyl alcohol, and performing ultrasonic dispersion for 40 min;
(3) mixing: and (3) adding the modified flexible graphite in the step (1) into the composite liquid, and performing ultrasonic dispersion for 1h to obtain a membrane spreading liquid.
Comparative example 1
Preparation of high-weather-resistance printing base film:
(1) putting 80 parts of PVC resin, 2 parts of thiodipropionic acid diester, 4 parts of weather-resistant additive, 10 parts of EVA (ethylene vinyl acetate), 12 parts of CPE (chlorinated polyethylene) compound, 6 parts of organic tin stabilizer, 5 parts of MBS (methyl methacrylate-butadiene-styrene) resin, 4 parts of stearic acid, 5 parts of polyethylene wax and 2 parts of ACR (acrylate copolymer) additive into a mixer for mixing;
(2) banburying, rolling, cooling, rolling and warehousing and curing are carried out for 12 hours to form a printing base film;
(3) spreading a film on the printing base film, and firing in a vulcanizing machine to obtain a semi-finished product;
(4) curing the semi-finished product for 12 hours;
(5) and packaging and warehousing the finished product after the detection is qualified.
Preparing a membrane laying liquid:
(1) modification of flexible graphite: adding 4 parts of flexible graphite into deionized water, stirring uniformly, adding 0.3 part of silane coupling agent KH550 and 0.02 part of trimethylolpropane, heating to a reflux state, keeping the temperature and stirring for 1h, filtering while hot, washing the obtained solid with deionized water to remove impurities, drying at the temperature of 100 ℃ plus 110 ℃ to constant weight, sealing and standing at the temperature of-3 ℃, 22 ℃ and 3 ℃, wherein the standing time is 30min each time;
(2) preparing a composite liquid: mixing 12 parts of nano SiO2Adding 8 parts of nano aluminum hydroxide powder into 70 parts of absolute ethyl alcohol, and performing ultrasonic dispersion for 40 min;
(3) mixing: and (3) adding the modified flexible graphite in the step (1) into the composite liquid, and performing ultrasonic dispersion for 1h to obtain a membrane spreading liquid.
Comparative example 2
Preparation of high-weather-resistance printing base film:
(1) putting 80 parts of PVC resin, 2 parts of thiodipropionic acid diester, 4 parts of weather-resistant additive, 10 parts of EVA (ethylene vinyl acetate), 12 parts of CPE (chlorinated polyethylene) compound, 6 parts of organic tin stabilizer, 5 parts of MBS (methyl methacrylate-butadiene-styrene) resin, 4 parts of stearic acid, 5 parts of polyethylene wax and 2 parts of ACR (acrylate copolymer) additive into a mixer for mixing;
(2) banburying, rolling, cooling, rolling and warehousing and curing are carried out for 12 hours to form a printing base film;
(3) spreading a film on the printing base film, and firing in a vulcanizing machine to obtain a semi-finished product;
(4) curing the semi-finished product for 12 hours;
(5) and packaging and warehousing the finished product after the detection is qualified.
Preparing a weather-resistant auxiliary agent: adding 4 parts of hydroxymethyl cellulose into deionized water, stirring for 10min at 30 ℃, then adding 3 parts of beta-hydroxybutyric acid and 0.01 part of tetraethyl titanate, heating to a reflux state, keeping the temperature and stirring for 2h, filtering while hot, washing with deionized water to remove impurities, and drying to constant weight.
Preparing a membrane laying liquid:
(1) preparing a composite liquid: mixing 12 parts of nano SiO2Adding 8 parts of nano aluminum hydroxide powder into 70 parts of absolute ethyl alcohol, and performing ultrasonic dispersion for 40 min;
(2) mixing: and adding 4 parts of flexible graphite into the composite liquid, and performing ultrasonic dispersion for 1 hour to obtain a membrane spreading liquid.
Comparative example 3
Preparation of high-weather-resistance printing base film:
(1) putting 80 parts of PVC resin, 2 parts of thiodipropionic acid diester, 4 parts of weather-resistant additive, 10 parts of EVA (ethylene vinyl acetate), 12 parts of CPE (chlorinated polyethylene) compound, 6 parts of organic tin stabilizer, 5 parts of MBS (methyl methacrylate-butadiene-styrene) resin, 4 parts of stearic acid, 5 parts of polyethylene wax and 2 parts of ACR (acrylate copolymer) additive into a mixer for mixing;
(2) banburying, rolling, cooling, rolling and warehousing and curing are carried out for 12 hours to form a printing base film;
(3) spreading a film on the printing base film, and firing in a vulcanizing machine to obtain a semi-finished product;
(4) curing the semi-finished product for 12 hours;
(5) and packaging and warehousing the finished product after the detection is qualified.
Preparing a weather-resistant auxiliary agent: adding 4 parts of hydroxymethyl cellulose into deionized water, stirring for 10min at 30 ℃, then adding 3 parts of beta-hydroxybutyric acid and 0.01 part of tetraethyl titanate, heating to a reflux state, keeping the temperature and stirring for 2h, filtering while hot, washing with deionized water to remove impurities, and drying to constant weight.
The base films were prepared by printing according to examples 1 to 2 and comparative examples 1 to 3, and the weather resistance thereof was measured, and the results are shown in Table 1.
Table 1 performance testing of printed base films
Weather resistance test the encapsulating material was evaluated according to astm d2244-93, "standard test method for color difference of color coordinates measured by a computer". The encapsulant was placed in a QUV uv weatherometer and the color characteristics (L, a, and b parameters) of each sample were measured using a color guide 45/0BYK Gardner unit with UVB uv radiation for 200 hours of irradiation. The change in color (Δ E) was calculated using astm d 2244.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (1)
1. The preparation method of the high-weather-resistance printing base film is characterized by comprising the following steps of:
(1) putting 80-100 parts of PVC resin, 1-5 parts of antioxidant, 1-5 parts of weather-resistant auxiliary agent, 10-15 parts of EVA, 10-15 parts of CPE, 5-10 parts of organic tin stabilizer, 4-6 parts of MBS resin, 3-6 parts of internal lubricant, 4-6 parts of external lubricant and 2-4 parts of ACR auxiliary agent into a mixer for mixing;
(2) banburying, rolling, cooling, rolling and warehousing and curing are carried out for 12 hours to form a printing base film;
(3) spreading the printing base film with a film spreading liquid, and firing in a vulcanizing machine to obtain a semi-finished product;
(4) curing the semi-finished product for 12 hours;
(5) packaging and warehousing the finished product after the detection is qualified;
the preparation method of the membrane spreading liquid in the step (3) comprises the following steps:
(1) modification of flexible graphite: adding flexible graphite into deionized water, stirring uniformly, adding a silane coupling agent and a chain extender, heating to a reflux state, keeping the temperature and stirring for 0.5-2h, filtering while hot, washing the obtained solid with deionized water to remove impurities, drying at the temperature of 110 ℃ to constant weight, sealing and standing at the temperature of-3-0 ℃, the temperature of 20-25 ℃, the temperature of 3-5 ℃, and standing for 30-50min each time;
(2) preparing a composite liquid: mixing nano SiO2And nano Ni (OH)2Adding the powder into absolute ethyl alcohol, and performing ultrasonic dispersion for 30-50 min;
(3) mixing: adding the modified flexible graphite in the step (1) into the composite liquid, and performing ultrasonic dispersion for 0.5-1.5h to obtain a membrane spreading liquid;
the mass ratio of the flexible graphite to the silane coupling agent to the chain extender is 3-5: 0.3-0.5: 0.02-0.04;
the nano SiO2Nano Ni (OH)2The mass ratio of the powder to the absolute ethyl alcohol is 10-15: 6-10: 60-80 parts;
the preparation method of the weather-resistant auxiliary agent comprises the following steps: adding hydroxymethyl cellulose into deionized water, stirring at 30 deg.C for 10-15min, adding beta-hydroxybutyric acid and tetraethyl titanate, heating to reflux state, stirring for 0.5-4 hr under heat preservation, filtering while hot, washing with deionized water to remove impurities, and drying to constant weight;
the mass ratio of the hydroxymethyl cellulose to the beta-hydroxybutyric acid to the tetraethyl titanate is 4-6: 3-5: 0.01-0.02.
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| JP3822425B2 (en) * | 2000-08-25 | 2006-09-20 | エスケー化研株式会社 | Floor coating method |
| CN103481517A (en) * | 2013-08-28 | 2014-01-01 | 南京美高美新材料有限公司 | Production technology of polyvinyl chloride (PVC) plastic floor |
| CN104196197A (en) * | 2014-08-11 | 2014-12-10 | 江阴华东装饰材料有限公司 | Damp-proof and inflaming-retarding PVC polymer floor film |
| CN107698890A (en) * | 2017-10-18 | 2018-02-16 | 安徽嘉阳新材料科技有限公司 | A kind of processing technology of floor film |
| CN108532905A (en) * | 2018-04-18 | 2018-09-14 | 江苏华俊新材料有限公司 | A kind of multi-functional high-elastic floor film |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924850A (en) * | 2012-11-20 | 2013-02-13 | 苏州奥凯材料技术有限公司 | Polyvinyl chloride transparent weather-resistant sheet |
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- 2018-12-28 CN CN201811621897.4A patent/CN109735022B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3822425B2 (en) * | 2000-08-25 | 2006-09-20 | エスケー化研株式会社 | Floor coating method |
| CN103481517A (en) * | 2013-08-28 | 2014-01-01 | 南京美高美新材料有限公司 | Production technology of polyvinyl chloride (PVC) plastic floor |
| CN104196197A (en) * | 2014-08-11 | 2014-12-10 | 江阴华东装饰材料有限公司 | Damp-proof and inflaming-retarding PVC polymer floor film |
| CN107698890A (en) * | 2017-10-18 | 2018-02-16 | 安徽嘉阳新材料科技有限公司 | A kind of processing technology of floor film |
| CN108532905A (en) * | 2018-04-18 | 2018-09-14 | 江苏华俊新材料有限公司 | A kind of multi-functional high-elastic floor film |
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Denomination of invention: Preparation method of high weather resistance printing base film Effective date of registration: 20210923 Granted publication date: 20210326 Pledgee: Anhui Science and technology Financing Guarantee Co.,Ltd. Jieshou branch Pledgor: ANHUI JIAYANG NEW MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2021980009726 |