CN113121930A - Low-odor calendered film and preparation method thereof - Google Patents
Low-odor calendered film and preparation method thereof Download PDFInfo
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- CN113121930A CN113121930A CN202110248981.1A CN202110248981A CN113121930A CN 113121930 A CN113121930 A CN 113121930A CN 202110248981 A CN202110248981 A CN 202110248981A CN 113121930 A CN113121930 A CN 113121930A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/262—Alkali metal carbonates
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- 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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/07—Aldehydes; Ketones
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
Abstract
The invention discloses a low-odor calendered film and a preparation method thereof, and relates to the technical field of high polymer materials. The low-odor calendered film comprises the following components in parts by weight: 100 parts of PVC resin powder, 1-10 parts of a primary plasticizer, 1-10 parts of an epoxy auxiliary plasticizer, 2-5 parts of a calcium-zinc stabilizer, 0.1-5 parts of a processing aid, 0.1-5 parts of a lubricant and 0.1-4 parts of an auxiliary stabilizer. The low-odor calendering film prepared by the formula disclosed by the invention has the advantages of good stability, higher plasticizing speed and smaller odor.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a low-odor rolling film and a preparation method thereof.
Background
Currently hard calendered films typically use organotin heat stabilizers, whereas tin mercaptides are more cost effective and widely employed. However, in the actual calendering process, tin mercaptide volatilizes at high temperature to generate pungent smell, and steam stimulates nerves and skin of operators, so that the tin mercaptide is accumulated for a long time and has certain harm to health. Meanwhile, the unpleasant taste of mercaptan in the finished product also limits the rapid increase of the usage amount of the PVC calendered film in the indoor furniture industry. Although barium-zinc stabilizers can partially satisfy the requirements of stability and odor, barium is a great advantage for hindering the development of the barium as a heavy metal.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the low-odor rolling film with good stability and quick plasticization and the preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a low-odor calendered film comprises the following components in parts by weight: 100 parts of PVC resin powder, 1-10 parts of a primary plasticizer, 1-10 parts of an epoxy auxiliary plasticizer, 2-5 parts of a calcium-zinc stabilizer, 0.1-5 parts of a processing aid, 0.1-5 parts of a lubricant and 0.1-4 parts of an auxiliary stabilizer.
The invention uses an environment-friendly calcium-zinc stabilizer system, achieves the same plasticizing efficiency as organic tin by adjusting the proportion of the calcium-zinc stabilizer and the auxiliary stabilizer, and tests the residual thermal stability and the dry-wet stability of the calcium-zinc stabilizer and the auxiliary stabilizer to achieve or even exceed the level of the organic tin system, thereby reducing the pollution to the environment and the damage to the human body, and meeting the requirements of production and finished product quality.
Preferably, the low odor calendered film comprises the following ingredients in parts by weight: 100 parts of PVC resin powder, 1-5 parts of a primary plasticizer, 3-6 parts of an epoxy auxiliary plasticizer, 2-4 parts of a calcium-zinc stabilizer, 1-3 parts of a processing aid, 1-3 parts of a lubricant and 1-3 parts of an auxiliary stabilizer. Through a plurality of experiments, the inventors of the present application find that the stability of the low-odor calendered film prepared by the above proportion is the best.
Preferably, the low-odor calendered film can be added with 5-20 parts of impact resistant agent and 1-15 parts of pigment according to performance requirements.
Preferably, the primary plasticizer comprises at least one of phthalate plasticizers, terephthalate plasticizers, phosphate plasticizers, polyatomic acid polyol ester plasticizers; the epoxy auxiliary plasticizer comprises at least one of epoxidized soybean oil and epoxy stearate; the calcium zinc stabilizer is at least one of a mixture of calcium salt and zinc salt containing long-chain organic acid and a mixture of hydrotalcite calcium salt and zinc salt; the processing aid is an acrylate polymer processing aid; the lubricant comprises at least one of fatty acid glyceride, fatty acid pentaerythritol ester, PE wax and Fischer-Tropsch wax; the auxiliary stabilizer comprises at least one of an antioxidant, a light stabilizer, dibenzoyl methane, hydrotalcite, phosphite ester, polyketone, polyalcohol and carbonate.
Preferably, the epoxy-based secondary plasticizer is epoxidized soybean oil, and the secondary stabilizer comprises antioxidant 1010, dibenzoylmethane, phosphite, pentaerythritol, sorbitol, and sodium carbonate.
Preferably, in the auxiliary stabilizer, the mass ratio of the antioxidant 1010, dibenzoylmethane, phosphite ester, pentaerythritol, sorbitol and sodium carbonate is as follows: antioxidant 1010: dibenzoylmethane: phosphite ester: pentaerythritol: sorbitol: sodium carbonate is 1:0.5 to 1.5:0.5 to 2.0:0.5 to 1.5:0.2 to 0.5.
Preferably, the thickness of the low-odor calendered film is 0.05-0.40 mm.
Meanwhile, the invention also discloses a preparation method of the low-odor calendered film, which comprises the following steps: adding the materials into a mixing machine for mixing, plasticating by a planetary extruder, mixing by a double-roll open mill, filtering by a filter, calendering by a calendering roll, embossing by an embossing roll, cooling, slitting and rolling to obtain the low-odor calendered film.
Preferably, the material mixing temperature is not higher than 100 ℃, the filtering temperature is not higher than 180 ℃, the temperature of the calendering roll is 160-215 ℃, the rotating speed of the calendering roll is 5-70 m/min, and the temperature of the cooling roll is 10-50 ℃.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, the calcium-zinc stabilizer is selected and assisted by dibenzoyl methane, polyhydric alcohol, antioxidant, phosphite ester and sodium carbonate, so that the prepared calendering film has good stability, less smell and more environmental friendliness. In addition, the proportion of each component is selected, so that the plasticizing time is shortened, and the processing time is reduced. Compared with the traditional calendered film taking organic tin as a stabilizing agent, the calendered film prepared by the formula has better comprehensive performance.
Drawings
Fig. 1 is a flow diagram of the preparation of a low odor calendered film 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.
Examples 1 to 9
In the examples of the low-odor calendered film of the invention, the formula of the low-odor calendered film of examples 1 to 9 is shown in table 1, and the preparation method comprises the following steps: adding all the raw materials into a mixer, uniformly mixing, plasticating in a planetary extruder, mixing in a double-roll mill, filtering in a filter, calendering by using a calendering roll, embossing by using an embossing roll, cooling, slitting and rolling to obtain the low-odor calendered film. Wherein the mixing temperature is controlled to be 80 +/-5 ℃, the filtering temperature is controlled to be 150 +/-5 ℃, the temperature of a calendering roller is 180 +/-5 ℃, the rotating speed of the calendering roller is 30m/min, and the temperature of a cooling roller is 25 +/-3 ℃.
Comparative example 1
A low odor calendered film made in the same manner as in example 1 except that the heat stabilizer was replaced with an organotin heat stabilizer from a calcium zinc stabilizer and no dibenzoylmethane.
TABLE 1 recipe table (parts by weight)
Performance testing
(1) Plasticizing time: after the materials are weighed and stirred and mixed uniformly, the powder is poured into a laboratory double-roller machine with constant temperature, a double roller is started, timing is started, the materials are turned and plasticized, when the materials are completely melted and can form pieces on the roller, the timing is stopped, and the time is the plasticizing time.
(2) And (3) testing dynamic stability: continuously plasticating the plasticized material, sampling according to a set thickness, sampling again after 30min, visually observing the color change of the sample, and comparing the yellowing index YI and the DeltE value of the sample.
(3) And (3) testing the dry stability of the finished product: DIN 1272170 ℃.
(4) Testing the wet stability of the finished product: DIN 1272270 ℃.
(5) Odor: and (3) performing smell evaluation on the finished product in the sample preparation process and after the sample preparation, putting a quantitative sample into a glass sealed bottle during the finished product test, heating the glass sealed bottle in a 60 ℃ oven for 4 hours, taking out the glass sealed bottle, standing the glass sealed bottle at room temperature for 0.5 hour, and judging the product according to the grade 1-5. The odor irritation gradually increases from 1 to 5.
The results of the performance tests are shown in Table 2.
TABLE 2
As can be seen from table 2, the low odor calendered films prepared from the formulations of the present invention plasticize faster; in addition, the calcium-zinc stabilizer and other stabilizers are compounded, so that compared with an organic tin heat stabilizer, the prepared PVC calendered film has smaller smell.
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 has been 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 (9)
1. The low-odor calendered film is characterized by comprising the following components in parts by weight: 100 parts of PVC resin powder, 1-10 parts of a primary plasticizer, 1-10 parts of an epoxy auxiliary plasticizer, 2-5 parts of a calcium-zinc stabilizer, 0.1-5 parts of a processing aid, 0.1-5 parts of a lubricant and 0.1-4 parts of an auxiliary stabilizer.
2. The low odor calendered film of claim 1 comprising the following parts by weight of ingredients: 100 parts of PVC resin powder, 1-5 parts of a primary plasticizer, 3-6 parts of an epoxy auxiliary plasticizer, 2-4 parts of a calcium-zinc stabilizer, 1-3 parts of a processing aid, 1-3 parts of a lubricant and 1-3 parts of an auxiliary stabilizer.
3. The low odor calendered film of claim 1 further comprising 5 to 20 parts of a fire retardant and 1 to 15 parts of a pigment.
4. The low odor calendered film of claim 1 wherein the primary plasticizer comprises at least one of a phthalate-based plasticizer, a terephthalate-based plasticizer, a phosphate-based plasticizer, a polyatomic acid polyol-based plasticizer; the epoxy auxiliary plasticizer comprises at least one of epoxidized soybean oil and epoxy stearate; the calcium zinc stabilizer is at least one of a mixture of calcium salt and zinc salt containing long-chain organic acid and a mixture of hydrotalcite calcium salt and zinc salt; the processing aid is an acrylate polymer processing aid; the lubricant comprises at least one of fatty acid glyceride, fatty acid pentaerythritol ester, PE wax and Fischer-Tropsch wax; the auxiliary stabilizer comprises at least one of an antioxidant, a light stabilizer, dibenzoyl methane, hydrotalcite, phosphite ester, polyketone, polyalcohol and carbonate.
5. The low odor calendered film of claim 4 wherein the epoxy-based secondary plasticizer is epoxidized soybean oil and wherein the secondary stabilizer comprises antioxidant 1010, dibenzoylmethane, a phosphite, pentaerythritol, sorbitol and sodium carbonate.
6. The low odor calendered film of claim 5 wherein the secondary stabilizer comprises antioxidant 1010, dibenzoylmethane, phosphite, pentaerythritol, sorbitol, and sodium carbonate in the mass ratio of: antioxidant 1010: dibenzoylmethane: phosphite ester: pentaerythritol: sorbitol: sodium carbonate is 1:0.5 to 1.5:0.5 to 2.0:0.5 to 1.5:0.2 to 0.5.
7. The low-odor calendered film of any of claims 1 to 6 wherein the low-odor calendered film has a thickness of from 0.05 to 0.40 mm.
8. A method of making a low odor calendered film according to any of claims 1 to 7, wherein the method comprises: adding the materials into a mixing machine for mixing, plasticating by a planetary extruder, mixing by a double-roll open mill, filtering by a filter, calendering by a calendering roll, embossing by an embossing roll, cooling, slitting and rolling to obtain the low-odor calendered film.
9. The method of producing a low-odor calendered film according to claim 8, wherein the mixing temperature is not higher than 100 ℃, the filtration temperature is not higher than 180 ℃, the temperature of the calendering roll is 160 to 215 ℃, the rotation speed of the calendering roll is 5 to 70m/min, and the temperature of the cooling roll is 10 to 50 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110248981.1A CN113121930B (en) | 2021-03-05 | 2021-03-05 | Low-odor calendered film and preparation method thereof |
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| CN202110248981.1A CN113121930B (en) | 2021-03-05 | 2021-03-05 | Low-odor calendered film and preparation method thereof |
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| CN113121930B CN113121930B (en) | 2022-03-22 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113943466A (en) * | 2021-10-25 | 2022-01-18 | 江苏新丰之星膜材料有限公司 | Formula for producing middle-layer film in decorative film |
| CN116589807A (en) * | 2023-07-17 | 2023-08-15 | 广州雷诺丽特塑料有限公司 | Heat-resistant PVC film and preparation method and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113943466A (en) * | 2021-10-25 | 2022-01-18 | 江苏新丰之星膜材料有限公司 | Formula for producing middle-layer film in decorative film |
| CN116589807A (en) * | 2023-07-17 | 2023-08-15 | 广州雷诺丽特塑料有限公司 | Heat-resistant PVC film and preparation method and application thereof |
| CN116589807B (en) * | 2023-07-17 | 2023-11-17 | 广州雷诺丽特塑料有限公司 | Heat-resistant PVC film and preparation method and application thereof |
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