CN110964273A - PVC calendering film and preparation method thereof - Google Patents
PVC calendering film and preparation method thereof Download PDFInfo
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- C08J2327/00—Characterised by the use 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; Derivatives of such polymers
- C08J2327/02—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
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- C08K5/00—Use of organic ingredients
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- C08K5/10—Esters; Ether-esters
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- C08K5/00—Use of organic ingredients
- C08K5/56—Organo-metallic compounds, i.e. organic compounds containing a metal-to-carbon bond
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Abstract
The invention relates to a PVC calendered film, which comprises the following raw materials in parts by weight: 100 parts of PVC resin, 1-20 parts of primary plasticizer, 4-12 parts of cold-resistant plasticizer, 0-8 parts of auxiliary plasticizer, 1.2-3.5 parts of organic tin stabilizer, 0-5 parts of processing aid, 0.5-2.5 parts of lubricant and 0.05-0.5 part of anti-precipitation agent. Aiming at the precipitation problem in the production of a semi-hard organotin stable system, the invention introduces a nano-scale anti-precipitation agent, and solves the problem that the precipitation is easy to be precipitated on the surface of a calendering wheel during processing so as to influence the transparency and haze of a product; compared with the method without adding the anti-precipitation agent, the prepared PVC calendering film has the advantages that the transparency and the haze are comparable, namely the appearance of the product is not influenced, the production efficiency is improved, the times of manually cleaning the calendering roller are reduced, and the use requirement of a printing surface layer is met.
Description
Technical Field
The invention relates to a PVC (polyvinyl chloride) calendered film and a preparation method thereof, belonging to the technical field of materials.
Background
Most of the existing plastic transparent surface layers for household use are semi-hard PVC calendered films as coating surface layers of printing layers, but when the semi-hard PVC calendered films are prepared by using a calcium zinc stabilizer or a barium zinc stabilizer, the decomposition and color change of PVC at high temperature cannot be effectively solved.
The organic tin stabilizer is used in semi-hard PVC calendering film, especially products containing cold-resistant plasticizer, for a long time, but the precipitation is serious, an oily substance is formed on the surface of a calendering roller in the preparation process, the production process needs to be cleaned regularly, and the production efficiency is influenced. If the cleaning is not timely, defects such as spots, streaks and fogging can be formed on the surface of the product and reach the mucosa, so that the production efficiency and the appearance are influenced, printing, gluing and other service performances are influenced, and the production and the application of the product are limited.
Therefore, there is a need for improving the formulation and preparation method of the PVC calendered film, which can greatly reduce the small molecular substances precipitated to the calendering wheel and reduce the frequency of manual cleaning of the calendering wheel, thereby improving the appearance of the product and increasing the production efficiency, without affecting the transparency, color and other properties of the product.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the PVC calendered film and the preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: the preparation raw materials of the PVC calendered film comprise the following components in parts by weight: 100 parts of PVC resin, 1-20 parts of primary plasticizer, 4-12 parts of cold-resistant plasticizer, 0-8 parts of auxiliary plasticizer, 1.2-3.5 parts of organic tin stabilizer, 0-5 parts of processing aid, 0.5-2.5 parts of lubricant and 0.05-0.5 part of anti-precipitation agent.
As a preferred embodiment of the PVC calendered film of the present invention, the raw material for preparing the PVC calendered film comprises the following components in parts by weight: 100 parts of PVC resin, 4-10 parts of primary plasticizer, 5-8 parts of cold-resistant plasticizer, 2-4 parts of auxiliary plasticizer, 1.5-2 parts of organic tin stabilizer, 1-3 parts of processing aid, 0.8-1.5 parts of lubricant and 0.1-0.25 part of anti-precipitation agent.
In a preferred embodiment of the PVC rolled film of the present invention, the K value of the PVC resin is 60 to 70.
In a preferred embodiment of the PVC rolled film according to the present invention, the primary plasticizer is at least one of phthalate esters, terephthalate esters, phosphate esters, and polyatomic acid polyol ester polymer plasticizers.
Preferably, the primary plasticizer is diisononyl phthalate (DINP).
In a preferred embodiment of the PVC calendered film according to the present invention, the cold-resistant plasticizer is a long-chain fatty dibasic acid ester cold-resistant plasticizer.
Preferably, the cold-resistant plasticizer is dioctyl adipate (DOA).
In a preferred embodiment of the PVC rolled film according to the present invention, the auxiliary plasticizer is at least one of Epoxidized Soybean Oil (ESO) and epoxy stearate.
In a preferred embodiment of the PVC calendered film of the present invention, the organotin stabilizer is at least one of tin monoalkyl-dialkyl mercaptide and tin alkyl organic acid.
Preferably, the organotin stabilizer is tin methyl mercaptide.
As a preferred embodiment of the PVC calendered film of the present invention, the processing aid is an acrylate polymer processing aid, the lubricant is at least one of fatty acid glyceride, fatty acid pentaerythritol ester, PE wax, and fischer-tropsch wax, and the anti-precipitation agent is at least one of nano-silica and nano-calcium carbonate.
Preferably, the processing aid is ACR and the lubricant is stearic acid monoglyceride.
Preferably, the thickness of the PVC calendering film is 0.03-0.10 mm.
In a second aspect, the invention provides a preparation method of the PVC calendered film, comprising the following steps: adding the raw materials into a high-speed stirrer according to a ratio, uniformly mixing, plasticizing by a planetary extruder and a double-roll open mill in sequence, filtering impurity particles by a filter, embossing by a calender, cooling and rolling to obtain the PVC calendered film.
As a preferred embodiment of the preparation method of the PVC calendered film, the mixing temperature is not higher than 100 ℃, the temperature of the filter is not higher than 180 ℃, the temperature of the calendering roller in the calender is 160-215 ℃, the speed of the calendering wheel in the calender is 5-70 m/min, the winding speed is 0-150 m/min, and the cooling temperature is 10-50 ℃.
Compared with the prior art, the invention has the beneficial effects that: aiming at the precipitation problem in the production of a semi-hard organotin stable system, the invention introduces a nano-scale anti-precipitation agent, and solves the problem that the precipitation is easy to be precipitated on the surface of a calendering wheel during processing so as to influence the transparency and haze of a product; compared with the method without adding the anti-precipitation agent, the prepared PVC calendering film has the advantages that the transparency and the haze are comparable, namely the appearance of the product is not influenced, the production efficiency is improved, the times of manually cleaning the calendering roller are reduced, and the use requirement of a printing surface layer is met.
Drawings
FIG. 1 is a process flow diagram of the preparation method of the present invention.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
Example 1
The preparation raw materials of the PVC calendered film comprise the following components in parts by weight: 100 parts of PVC resin, 9 parts of DINP, 6 parts of DOA, 2 parts of ESO, 1.5 parts of methyl tin mercaptide, 1.2 parts of ACR, 1 part of stearic acid monoglyceride and 0.2 part of nano silicon dioxide, wherein the K value of the PVC resin is 60.
The preparation method of the PVC calendered film of this example includes the following steps: the PVC calendering film is prepared by adding the raw materials into a high-speed stirrer according to a ratio, uniformly mixing, sequentially plasticizing by a planetary extruder and a double-roll open mill, filtering impurity particles by a filter, embossing by a calender, cooling and rolling, wherein the mixing temperature is not higher than 100 ℃, the temperature of the filter is not higher than 180 ℃, the temperature of a calender roll in the calender is 200 ℃, the speed of a calender wheel in the calender is 50m/min, the rolling speed is 70m/min, and the cooling temperature is 30 ℃. The process flow diagram of the preparation method of the embodiment is shown in fig. 1.
Example 2
The preparation raw materials of the PVC calendered film comprise the following components in parts by weight: 100 parts of PVC resin, 1 part of terephthalate plasticizer, 12 parts of cold-resistant plasticizer n-nonyl phthalate, 38 parts of epoxy stearate auxiliary plasticizing ED, MT-8001.2 parts of monoalkyl mercaptan carboxylate tin, 0.5 part of fatty acid pentaerythritol ester and 0.05 part of nano calcium carbonate, wherein the K value of the PVC resin is 65.
The preparation method of the PVC calendered film of this example includes the following steps: the PVC calendering film is prepared by adding the raw materials into a high-speed stirrer according to a ratio, uniformly mixing, sequentially plasticizing by a planetary extruder and a double-roll open mill, filtering impurity particles by a filter, embossing by a calender, cooling and rolling, wherein the mixing temperature is not higher than 100 ℃, the temperature of the filter is not higher than 180 ℃, the temperature of a calender roll in the calender is 160 ℃, the speed of a calender wheel in the calender is 70m/min, the rolling speed is 150m/min, and the cooling temperature is 10 ℃.
Example 3
The preparation raw materials of the PVC calendered film comprise the following components in parts by weight: 100 parts of PVC resin, 20 parts of phosphate plasticizer TCP, 4 parts of long-chain fatty dibasic acid ester cold-resistant plasticizer DOS, 3.5 parts of methyl tin mercaptide, 2.5 parts of PE wax and 0.5 part of nano calcium carbonate, wherein the K value of the PVC resin is 70.
The preparation method of the PVC calendered film of this example includes the following steps: the PVC calendering film is prepared by adding the raw materials into a high-speed stirrer according to a ratio, uniformly mixing, sequentially plasticizing by a planetary extruder and a double-roll open mill, filtering impurity particles by a filter, embossing by a calender, cooling and rolling, wherein the mixing temperature is not higher than 100 ℃, the temperature of the filter is not higher than 180 ℃, the temperature of a calender roll in the calender is 215 ℃, the speed of a calender wheel in the calender is 5m/min, the rolling speed is 30m/min, and the cooling temperature is 50 ℃.
Comparative example 1
The preparation raw materials of the PVC calendered film comprise the following components in parts by weight: 100 parts of PVC resin, 9 parts of DINP, 6 parts of DOA, 2 parts of ESO, 1.5 parts of tin methyl mercaptide, 1.2 parts of ACR and 1 part of stearic acid monoglyceride, wherein the K value of the PVC resin is 60.
The preparation method of the PVC calendered film of this example includes the following steps: the PVC calendering film is prepared by adding the raw materials into a high-speed stirrer according to a ratio, uniformly mixing, sequentially plasticizing by a planetary extruder and a double-roll open mill, filtering impurity particles by a filter, embossing by a calender, cooling and rolling, wherein the mixing temperature is not higher than 100 ℃, the temperature of the filter is not higher than 180 ℃, the temperature of a calender roll in the calender is 200 ℃, the speed of a calender wheel in the calender is 50m/min, the rolling speed is 70m/min, and the cooling temperature is 30 ℃.
Effect example 1
The performance of the PVC calendered film prepared in examples 1 to 3 and comparative example 1 was tested, including the precipitation, transmittance, haze, etc. during the preparation process. The anti-precipitation test method is characterized in that continuous production effect judgment is adopted, precipitation time of the calendering roller and precipitation conditions of the roller surface during continuous production are observed, the detection standard of transmittance is ANSI-26.1, and the detection standard of haze is ASTM D1003. The test results are shown in table 1.
TABLE 1
| Resistance to precipitation test | Transmittance of light | Haze degree | |
| Example 1 | After continuous production for 8hr, trace precipitation occurs at the edge of the roller | 90.56％ | 49.14％ |
| Example 2 | After continuous production for 6hr, micro precipitation is generated at the edge of the roller | 91.55％ | 49.00％ |
| Example 3 | After continuous production for 7hr, micro precipitation is generated at the edge of the roller | 90.50％ | 49.35％ |
| Comparative example 1 | Precipitating for 2hr to cover the whole roller length | 90.63％ | 48.90％ |
As can be seen from table 1, in examples 1 to 3, within the scope of the present invention, the PVC calendered film prepared has good transmittance and haze, and the precipitation is greatly improved during the production process. In contrast, in comparative example 1, no anti-precipitation agent was added, and the precipitation in the production process was severe.
Effect example 2
In order to investigate the influence of the weight parts of the raw materials on the effect of the invention, test groups 1-5 and control groups 1-2 were set. In test groups 1 to 5 and control groups 1 to 2, only the weight parts of the respective raw materials were different, the selection of the raw materials and the preparation method were the same, and the weight parts of the respective raw materials are shown in table 2. Meanwhile, the performance of the PVC calendered film prepared by the test groups 1-5 and the control groups 1-2 is tested, and the test results are shown in Table 2.
TABLE 2
| Test group 1 | Test group 2 | Test group 3 | Test group 4 | Test group 5 | Control group 1 | Control group 2 | |
| PVC resin | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
| Primary plasticizer | 1 | 4 | 7 | 10 | 20 | 10 | 22 |
| Cold-resistant plasticizer | 4 | 5 | 6 | 8 | 10 | 12 | 3 |
| Auxiliary plasticizer | 0 | 2 | 3 | 4 | 8 | 2 | 4 |
| Organotin stabilizers | 1.2 | 1.5 | 2 | 2 | 3.5 | 5 | 4 |
| Processing aid | 0 | 1 | 2 | 3 | 5 | 1 | 3 |
| Lubricating agent | 0.5 | 0.8 | 1.0 | 1.5 | 2.5 | 3 | 3 |
| Anti-precipitation agent | 0.05 | 0.1 | 0.2 | 0.25 | 0.5 | 0.4 | 0.6 |
| Resistance to precipitation test | Precipitating for 7hr | Precipitating for 7.5hr | Precipitating for 7hr | Precipitating for 8hr | Precipitating for 6hr | Precipitating for 5hr | Precipitating for 4hr |
| Transmittance of light | 89.01％ | 89.88％ | 90.20％ | 90.88％ | 87.65％ | 85.33％ | 83.86％ |
| Haze degree | 43.25％ | 44.00％ | 45.99％ | 45.50％ | 40.38％ | 35..76％ | 33.05％ |
As can be seen from Table 2, the PVC calendered film prepared by the test groups 1-5 with the weight parts of the raw materials within the range of the invention has good transmittance and haze, and the precipitation condition is greatly improved in the production process; the weight parts of the raw materials of the control groups 1-2 are not all in the range of the invention, and the transmittance and haze of the prepared PVC calendered film are inferior to those of the invention. The PVC calendered film prepared by the test groups 2-4 has better transmittance and haze, and the precipitation condition in the production process is better improved; namely, when the preparation raw material comprises the following components in parts by weight: the invention has better effect when 100 parts of PVC resin, 4-10 parts of main plasticizer, 5-8 parts of cold-resistant plasticizer, 2-4 parts of auxiliary plasticizer, 1.5-2 parts of organic tin stabilizer, 1-3 parts of processing aid, 0.8-1.5 parts of lubricant and 0.1-0.25 part of anti-precipitation agent.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The PVC calendered film is characterized in that the preparation raw materials of the PVC calendered film comprise the following components in parts by weight: 100 parts of PVC resin, 1-20 parts of primary plasticizer, 4-12 parts of cold-resistant plasticizer, 0-8 parts of auxiliary plasticizer, 1.2-3.5 parts of organic tin stabilizer, 0-5 parts of processing aid, 0.5-2.5 parts of lubricant and 0.05-0.5 part of anti-precipitation agent.
2. The calendered PVC film of claim 1 wherein the raw materials for the preparation of the calendered PVC film comprise the following components in parts by weight: 100 parts of PVC resin, 4-10 parts of primary plasticizer, 5-8 parts of cold-resistant plasticizer, 2-4 parts of auxiliary plasticizer, 1.5-2 parts of organic tin stabilizer, 1-3 parts of processing aid, 0.8-1.5 parts of lubricant and 0.1-0.25 part of anti-precipitation agent.
3. The PVC calendered film of claim 1 or 2 wherein the PVC resin has a K value of from 60 to 70.
4. The calendered PVC film of claim 1 or 2 wherein the primary plasticizer is at least one of phthalate esters, terephthalate esters, phosphate esters, and polymeric plasticizers based on polyatomic acid polyol esters.
5. The PVC calendered film of claim 1 or 2 wherein the cold-resistant plasticizer is a long chain fatty dibasic acid ester cold-resistant plasticizer.
6. The PVC calendered film of claim 1 or 2 wherein the secondary plasticizer is at least one of epoxidized soybean oil, and epoxidized stearate.
7. The PVC calendered film of claim 1 or 2 wherein the organotin stabilizer is at least one of a tin mono-and bis-alkyl mercaptide carboxylate and a tin alkyl organate.
8. The PVC calendered film of claim 1 or 2 wherein the processing aid is an acrylate polymer processing aid, the slip agent is at least one of a fatty acid glyceride, a fatty acid pentaerythritol ester, a PE wax, and a fischer-tropsch wax, and the anti-bleed agent is at least one of a nano-silica and a nano-calcium carbonate.
9. The method for preparing a PVC calendered film according to any of the claims 1 to 8, comprising the following steps: adding the raw materials into a high-speed stirrer according to a ratio, uniformly mixing, plasticizing by a planetary extruder and a double-roll open mill in sequence, filtering impurity particles by a filter, embossing by a calender, cooling and rolling to obtain the PVC calendered film.
10. The method for preparing a PVC calendered film according to claim 9, wherein in the step, the mixing temperature is not higher than 100 ℃, the temperature of the filter is not higher than 180 ℃, the temperature of the calender roll in the calender is 160 to 215 ℃, the speed of the calender roll in the calender is 5 to 70m/min, the winding speed is 0 to 150m/min, and the cooling temperature is 10 to 50 ℃.
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| CN111393766A (en) * | 2020-04-27 | 2020-07-10 | 山东沃尔新材料有限公司 | Production formula and preparation method of middle-layer PVC printing film for SPC floor |
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| CN112812462A (en) * | 2020-12-31 | 2021-05-18 | 河北晨升塑胶制品有限公司 | Flexible odorless low-temperature-resistant PVC material and preparation method thereof |
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