CN114230941A - Heat stabilizer for processing soft transparent PVC and preparation method thereof - Google Patents
Heat stabilizer for processing soft transparent PVC and preparation method thereof Download PDFInfo
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- CN114230941A CN114230941A CN202111582952.5A CN202111582952A CN114230941A CN 114230941 A CN114230941 A CN 114230941A CN 202111582952 A CN202111582952 A CN 202111582952A CN 114230941 A CN114230941 A CN 114230941A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention belongs to the technical field of PVC (polyvinyl chloride) heat stabilizers, and particularly relates to a heat stabilizer for processing soft transparent PVC and a preparation method thereof, which can solve the technical problem that the existing heat stabilizer technology cannot give consideration to both coloring at the initial stage of PVC processing and long-term heat stability. The heat stabilizer for processing the soft transparent PVC is characterized by comprising the following raw materials: zinc oleate, amino metal organic framework compounds, auxiliary heat stabilizers, plasticizers, lubricants, antioxidants and ultraviolet absorbers. The invention takes zinc oleate and amino metal organic framework compound as main stabilizers and is matched with necessary auxiliary stabilizers, compared with the traditional zinc stearate, the invention has excellent transparency and initial coloring, and is suitable for transparent PVC products.
Description
Technical Field
The invention belongs to the technical field of PVC heat stabilizers, and particularly relates to a heat stabilizer for processing soft transparent PVC and a preparation method thereof.
Background
Common products of the transparent PVC include plates, pipes, sheets and films, the hardness can be adjusted to meet the performance requirements in the fields of transparent cables, soft toys, stationery, food packaging films, artificial leather products and the like, and the development of PVC products with high transparency and low-temperature flexibility is a research hotspot in the field. The transparent PVC is added with a heat stabilizer, a plasticizer and a lubricant during processing, wherein the heat stabilizer plays an important role in the initial colorability and long-term heat stability of PVC products.
The plasticizing and decomposing temperature of PVC resin is very close, the processing temperature is usually higher than 140 ℃, and the PVC resin can be thermally decomposed at about 100 ℃ to release hydrogen chloride, and the macromolecular chain segment is degraded to generate a chromogenic conjugated polyene structure. Therefore, the transparent PVC resin must be added with a heat stabilizer during processing to prevent or reduce the problem of darkening of the product due to thermal decomposition during processing. In addition, the heat stabilizer has good compatibility with PVC and refractive index close to that of PVC, so that high transparency of PVC products is ensured.
The PVC heat stabilizer used in common use includes lead salts, organic tin, organic antimony, metallic soap, organic base and its derivatives, and composite heat stabilizer. Lead salt compounds have strong toxicity and can cause harm to human bodies and environmental safety. The organic tin compound has good thermal stability and transparency, excellent comprehensive performance and high cost. The light resistance of the organic antimony heat stabilizer itself is relatively poor. The calcium-zinc soap composite heat stabilizer is non-toxic and low in price, but has the defects of serious initial coloring, poor long-term heat stability and the like. The heat stabilizer used in the traditional PVC transparent product is calcium zinc stearate composite stabilizer, has good stability effect in the initial processing stage of PVC, but in the later processing stage, zinc stearate can be decomposed with HCl generated by heat to generateFormation of ZnCl2Which catalyzes the zipper effect promoting accelerated degradation of PVC. Therefore, the PVC processing stabilizer system needs to add an auxiliary stabilizer in addition to the main stabilizer so as to combine ZnCl in time2。
Therefore, there is a need to develop a novel heat stabilizer material to improve the initial colorability and long-term heat stability of the calcium-zinc composite heat stabilizer, and to be better applied to the field of transparent PVC processing.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a heat stabilizer for processing soft transparent PVC and a preparation method thereof, and solves the technical problem that the prior heat stabilizer technology cannot give consideration to both the initial coloring and the long-term heat stability of PVC processing.
In order to achieve the purpose, the invention adopts the following technical scheme:
the heat stabilizer for processing the soft transparent PVC comprises the following raw materials: zinc oleate, amino metal organic framework compounds, auxiliary heat stabilizers, plasticizers, lubricants, antioxidants and ultraviolet absorbers.
Preferably, the amino metal organic framework compound comprises an organic ligand and a metal salt, and the mass ratio of the organic ligand to the metal salt is 1: 1; the organic ligand is amino terephthalic acid, amino naphthalene dicarboxylic acid or 2-aminoimidazole.
Preferably, the auxiliary heat stabilizer is pentaerythritol, uracil, beta-diketone or powder phosphite ester.
Preferably, the plasticizer is epoxidized soybean oil or cyclohexane 1, 2-dicarboxylic acid diisononyl ester.
Preferably, the lubricant polyethylene wax, oxidized polyethylene wax, butyl stearate or stearic acid amide.
Preferably, the antioxidant is antioxidant 618, antioxidant 1010 or antioxidant 1076.
Preferably, the ultraviolet absorber is UV531, UV326 or UV 328.
Preferably, the raw materials are used in the following amounts: 20-30 parts of zinc oleate, 15-20 parts of amino metal organic framework compounds, 15-25 parts of auxiliary heat stabilizers, 10-15 parts of plasticizers, 4-8 parts of lubricants, 1.5-2.5 parts of antioxidants and 0.5-1.5 parts of ultraviolet absorbers.
(II) a preparation method of a heat stabilizer for processing soft transparent PVC, which comprises the following steps:
and 2, adding a plasticizer into the heated first mixture to obtain a second mixture, and sequentially heating, stirring and granulating the second mixture to obtain the heat stabilizer for processing the soft transparent PVC.
Preferably, the heating temperature in step 1 is 60-90 deg.C, and the heating temperature in step 2 is 100-120 deg.C.
The invention can produce the beneficial effects that:
1) in the composite heat stabilizer prepared by the invention, the amino metal organic framework can replace the combination of tertiary carbon group and allyl group of PVC to prevent HCl from being removed, and the porous structure and amino group of the metal organic framework compound can be combined with HCl released in processing in time to prevent the combination of HCl and zinc oleate to generate ZnCl2Can reduce the phenomenon of zinc burning, and is favorable for the long-term stability of PVC.
2) In the composite heat stabilizer prepared by the invention, zinc oleate can capture the hydrogen chloride fallen off and replace chlorine atoms in allyl chloride to generate relatively stable ester, so that an initiation source for removing HCl in a polymerization material is eliminated.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 shows the transparency results of PVC with the composite stabilizer of the present invention added.
FIG. 2 shows the results of the torque rheology of PVC with the composite stabilizer of the invention added.
FIG. 3 shows the results of oven aging tests of PVC with the composite stabilizer of the present invention added.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the respective manufacturers.
The heat stabilizer for processing the soft transparent PVC provided by the invention comprises the following raw materials: 20-30 parts of zinc oleate, 15-20 parts of amino metal organic framework compounds, 15-25 parts of auxiliary heat stabilizers, 10-15 parts of plasticizers, 4-8 parts of lubricants, 1.5-2.5 parts of antioxidants and 0.5-1.5 parts of ultraviolet absorbers.
The amino metal organic framework compound comprises an organic ligand and a metal salt, the amino metal organic framework compound is prepared from the organic ligand and the metal salt in a mass ratio of 1:1 under hydrothermal or solvothermal conditions, and the organic ligand is amino terephthalic acid, amino naphthalene dicarboxylic acid or 2-aminoimidazole.
Wherein the auxiliary heat stabilizer is pentaerythritol, uracil, beta-diketone or powder phosphite ester.
Wherein the plasticizer is epoxidized soybean oil or cyclohexane 1, 2-diisononyl phthalate.
Wherein the lubricant is polyethylene wax, oxidized polyethylene wax, butyl stearate or stearic acid amide.
Wherein the antioxidant is antioxidant 618, antioxidant 1010 or antioxidant 1076.
Wherein the ultraviolet absorbent is UV531, UV326 or UV 328.
The invention provides a preparation method of a heat stabilizer for processing soft transparent PVC, which comprises the following steps:
and 2, adding a plasticizer into the heated first mixture to obtain a second mixture, and sequentially heating, stirring and granulating the second mixture to obtain the heat stabilizer for processing the soft transparent PVC, wherein the heating temperature is 100-120 ℃, and the granulation is obtained by a granulator.
Example 1
A heat stabilizer for processing soft transparent PVC comprises the following components in parts by mass: 30 parts of zinc oleate, 15 parts of amino metal organic framework compound, 10 parts of uracil, 5 parts of beta-diketone, 10 parts of cyclohexane 1, 2-diisononyl diformate, 4 parts of polyethylene wax (AC-6A), 6181 parts of antioxidant and UV 5311 parts, wherein the amino metal organic framework compound comprises an organic ligand and a metal salt in a mass ratio of 1:1, and the organic ligand is amino terephthalic acid, amino naphthalene dicarboxylic acid or 2-aminoimidazole;
30 parts of zinc oleate, 15 parts of amino metal organic framework compounds, 10 parts of uracil, 5 parts of beta-diketone, 10 parts of cyclohexane 1, 2-diisononyl diformate, 4 parts of polyethylene wax (AC-6A), 6181 parts of antioxidant and 5311 parts of UV are mixed to obtain a first mixture, the first mixture is heated to 60 ℃, then a plasticizer is added into the heated first mixture to obtain a second mixture, the second mixture is heated to 100 ℃, the heated second mixture is uniformly stirred, and the heat stabilizer for processing the soft transparent PVC is obtained through granulation.
Example 2
A heat stabilizer for processing soft transparent PVC comprises the following components in parts by mass: 25 parts of zinc oleate, 18 parts of amino metal organic framework compound, 10 parts of uracil, 5 parts of pentaerythritol, 10 parts of epoxidized soybean oil, 6 parts of polyethylene wax (AC-6A), 10101 parts of antioxidant and UV 3261 parts, wherein the amino metal organic framework compound comprises an organic ligand and a metal salt in a mass ratio of 1:1, and the organic ligand is amino terephthalic acid, amino naphthalene dicarboxylic acid or 2-aminoimidazole;
30 parts of zinc oleate, 15 parts of amino metal organic framework compounds, 10 parts of uracil, 5 parts of beta-diketone, 10 parts of cyclohexane 1, 2-diisononyl diformate, 4 parts of polyethylene wax (AC-6A), 6181 parts of antioxidant and 5311 parts of UV are mixed to obtain a first mixture, the first mixture is heated to 90 ℃, then a plasticizer is added into the heated first mixture to obtain a second mixture, the second mixture is heated to 120 ℃, the heated second mixture is uniformly stirred, and the heat stabilizer for processing the soft transparent PVC is obtained through granulation.
Example 3
A heat stabilizer for processing soft transparent PVC comprises the following components in parts by mass: 20 parts of zinc oleate, 20 parts of amino metal organic framework compound, 10 parts of uracil, 5 parts of powder phosphite ester, 12 parts of cyclohexane 1, 2-diisononyl diformate, 8 parts of polyethylene wax (AC-6A), 10761 parts of antioxidant and UV 3281 parts, wherein the amino metal organic framework compound comprises an organic ligand and a metal salt in a mass ratio of 1:1, and the organic ligand is amino terephthalic acid, amino naphthalene dicarboxylic acid or 2-aminoimidazole;
30 parts of zinc oleate, 15 parts of amino metal organic framework compounds, 10 parts of uracil, 5 parts of beta-diketone, 10 parts of cyclohexane 1, 2-diisononyl diformate, 4 parts of polyethylene wax (AC-6A), 6181 parts of antioxidant and 5311 parts of UV are mixed to obtain a first mixture, the first mixture is heated to 60 ℃, then a plasticizer is added into the heated first mixture to obtain a second mixture, the second mixture is heated to 100 ℃, the heated second mixture is uniformly stirred, and the heat stabilizer for processing the soft transparent PVC is obtained through granulation.
Comparative example 1
PVC calcium zinc stabilizer heat stabilizer sold in China is used as comparison
Under the same conditions, the heat stabilizers for processing soft transparent PVC prepared in the above examples and comparative example 1 were prepared into PVC transparent sheets, and the specific formulation is shown in table 1:
TABLE 1PVC formulation
| Raw material | Examples | Comparative example |
| PVC (SG-5, Wenzhou Zhengbang chemical Co., Ltd.) | 100g | 100g |
| Plasticizer | 30g | 30g |
| The invention relates to a composite heat stabilizer for transparent PVC | 3g | / |
| Traditional calcium-zinc stabilizer for transparent PVC (polyvinyl chloride) | / | 3g |
The preparation process of the PVC transparent sheet comprises the following steps: respectively and uniformly mixing by a small high-speed mixer, plasticating the mixture on an open mill for 5min at 180 ℃, and preparing a test piece with the thickness of 1mm for later use.
The following description of the test procedures and test results for the preparation of PVC articles according to the examples and comparative examples is as follows:
1. light transmittance
The transparent sheet samples prepared in comparative examples and examples according to the formulation components of table 1 were cut into a size of 5 × 5cm, and the transmittance was measured, and the average value was taken 3 times for each sample. The results are shown in FIG. 1.
As shown in figure 1, the transparency of the transparent sheet made by using the heat stabilizer for processing soft transparent PVC disclosed by the invention can reach 89%, and the transparent sheet has better transparency compared with a PVC calcium-zinc heat stabilizer sold in China.
2. Static thermal stability
The transparent sheets made in the comparative examples and examples prepared according to the formulation components of table 1 were subjected to oven aging tests to investigate the static thermal stability, and the photographs were taken every 10 minutes, and the results are shown in fig. 2.
As can be seen from FIG. 2, the static thermal stability time of the transparent sheet made by using the heat stabilizer for processing soft transparent PVC disclosed by the present invention is about 90min, which means that the addition of the heat stabilizer for processing soft transparent PVC disclosed by the present invention has better static thermal stability than the conventional calcium-zinc heat stabilizer.
3. Dynamic thermal stability
The comparative examples and examples, prepared according to the formulation components of table 1, were tested for dynamic thermal stability of PVC using a torque rheometer and the results are shown in fig. 3.
As can be seen from FIG. 3, the dynamic thermal stability of the transparent sheet made by using the heat stabilizer for processing soft transparent PVC disclosed by the invention can reach 90min, i.e. the dynamic thermal stability time of PVC plastics can be obviously prolonged by using the heat stabilizer for processing soft transparent PVC disclosed by the invention.
The invention takes zinc oleate and amino metal organic framework compound as main stabilizers and is matched with necessary auxiliary stabilizers, compared with the traditional zinc stearate, the invention has excellent transparency and initial coloring, and is suitable for transparent PVC products. The zinc oleate has better compatibility with PVC, and is beneficial to the initial coloring of PVC products. The abundant porous structure and amino side chain structure of the metal organic framework compound can effectively absorb HCl released during PVC hot processing, and the metal organic framework compound has excellent static and long-term stable effects, and added lubricant, antioxidant, ultraviolet absorbent and plasticizer have excellent synergistic effect and easy processability during PVC processing.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A heat stabilizer for processing soft transparent PVC is characterized by comprising the following raw materials: zinc oleate, amino metal organic framework compounds, auxiliary heat stabilizers, plasticizers, lubricants, antioxidants and ultraviolet absorbers.
2. The thermal stabilizer for processing soft transparent PVC according to claim 1, wherein the amino metal organic framework compound comprises an organic ligand and a metal salt, the mass ratio of the organic ligand to the metal salt is 1: 1;
the organic ligand is amino terephthalic acid, amino naphthalene dicarboxylic acid or 2-aminoimidazole.
3. The heat stabilizer for processing soft transparent PVC according to claim 1, wherein the auxiliary heat stabilizer is pentaerythritol, uracil, beta-diketone or powder phosphite.
4. Heat stabilizer for the processing of flexible transparent PVC according to claim 1, characterized in that the plasticizer is epoxidized soybean oil or cyclohexane 1, 2-dicarboxylic acid diisononyl ester.
5. Heat stabilizer for the processing of soft transparent PVC according to claim 1, characterized in that the lubricant polyethylene wax, oxidized polyethylene wax, butyl stearate or stearamide.
6. The heat stabilizer for processing soft transparent PVC according to claim 1, wherein the antioxidant is antioxidant 618, antioxidant 1010 or antioxidant 1076.
7. Heat stabilizer for the processing of soft transparent PVC according to claim 1, characterized in that the ultraviolet absorber is UV531, UV326 or UV 328.
8. The heat stabilizer for processing soft transparent PVC according to claim 1, wherein the raw materials are used in the following amounts: 20-30 parts of zinc oleate, 15-20 parts of amino metal organic framework compounds, 15-25 parts of auxiliary heat stabilizers, 10-15 parts of plasticizers, 4-8 parts of lubricants, 1.5-2.5 parts of antioxidants and 0.5-1.5 parts of ultraviolet absorbers.
9. A preparation method of a heat stabilizer for processing soft transparent PVC is characterized by comprising the following steps:
step 1, mixing zinc oleate, an amino metal organic framework compound, an auxiliary heat stabilizer, a lubricant, an antioxidant and an ultraviolet absorber to obtain a first mixture, and heating the first mixture;
and 2, adding a plasticizer into the heated first mixture to obtain a second mixture, and sequentially heating, stirring and granulating the second mixture to obtain the heat stabilizer for processing the soft transparent PVC.
10. The method for preparing heat stabilizer for processing flexible transparent PVC according to claim 9, wherein the heating temperature in step 1 is 60-90 ℃ and the heating temperature in step 2 is 100-120 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116178792A (en) * | 2022-12-05 | 2023-05-30 | 茂名联塑建材有限公司 | Calcium-zinc MOFs composite heat stabilizer and preparation method and application thereof |
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