CN115536915B - Low-atomization calcium-zinc stabilizer for PVC and stability test method thereof - Google Patents
Low-atomization calcium-zinc stabilizer for PVC and stability test method thereof Download PDFInfo
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Abstract
The invention discloses a low-atomization calcium zinc stabilizer for PVC and a stability test method thereof. The low-atomization calcium-zinc stabilizer for PVC comprises the following raw materials in parts by weight: 25-35 parts of zinc stearate, 15-30 parts of calcium stearate, 3-5 parts of stearoyl benzoyl methane, 10-40 parts of hydrotalcite and 10-30 parts of modified zeolite; the modified zeolite is obtained by modifying together a silane coupling agent and a cationic surfactant. The low-atomization calcium zinc stabilizer for PVC has low atomization value and good stability.
Description
Technical Field
The invention relates to the technical field of chemical stabilizers, in particular to a low-atomization calcium zinc stabilizer for PVC and a stability test method thereof.
Background
Polyvinyl chloride (PVC) has the advantages of excellent comprehensive performance, low price and the like, and is widely applied. However, the poor thermal stability of polyvinyl chloride necessitates the addition of an appropriate heat stabilizer to inhibit degradation of the polyvinyl chloride during processing. Heat stabilizers can be divided into the following categories: lead salts, metal soaps, organotin and rare earth heat stabilizers. However, the common lead salts and organotin heat stabilizers in the market have certain toxicity. The calcium zinc heat stabilizer alone cannot meet the application requirements, and an appropriate amount of auxiliary heat stabilizer, mainly polyol, beta-diketone, phosphite, epoxy compound, hydrotalcite and zeolite, is usually added for improving the heat stability.
The applicant finds that the cost of the calcium zinc heat stabilizer can be reduced by adding zeolite in the research process, but the higher water content of the zeolite can lead the atomization value of the PVC stabilizer to be higher, and the zeolite is not suitable for PVC products with the requirement on the atomization value.
Therefore, there is a need in the present application to develop a low-fogging calcium zinc stabilizer for PVC.
Disclosure of Invention
In order to reduce the atomization value of the calcium zinc stabilizer, the application provides a low-atomization calcium zinc stabilizer for PVC.
In a first aspect, the application provides a low-atomization calcium zinc stabilizer for PVC, which is realized by adopting the following technical scheme: the low-atomization calcium-zinc stabilizer for PVC comprises the following raw materials in parts by weight: 25-35 parts of zinc stearate, 15-30 parts of calcium stearate, 3-5 parts of stearoyl benzoyl methane, 10-40 parts of hydrotalcite and 10-30 parts of modified zeolite; the modified zeolite is obtained by modifying together a silane coupling agent and a cationic surfactant.
By adopting the technical scheme, the silane coupling agent and the hydroxyl groups on the surface of the zeolite are chemically bonded, so that the silicon hydroxyl groups on the surface of the zeolite are reduced, hydrophobic hydrocarbon chains are loaded on the surface of the zeolite, the cationic surfactant is easy to electrostatically adsorb with negative charges on the surface of the zeolite, so that the zeolite is hydrophobic, the silane coupling agent and the cationic surfactant are used for jointly modifying the zeolite, the water content of the zeolite is further reduced, and the atomization value of the stabilizer is reduced.
Preferably, the preparation raw materials further comprise 1-5 parts by weight of dihydropyridine or 3-7 parts by weight of 1, 3-dimethyl-6-amino uracil.
The 1, 3-dimethyl-6-amino uracil has the capability of replacing unstable chlorine atoms in PVC, and can effectively improve the stability of the low-atomization calcium zinc stabilizer for PVC. The dihydropyridine has an antioxidation effect, can improve the initial stability of the low-atomization calcium zinc stabilizer for PVC, and reduces the color difference value of the sample piece under 5min, 7min and 10 min.
Preferably, the preparation method of the modified zeolite comprises the following steps:
s1, grinding zeolite for later use;
s2, adding a silane coupling agent into isopropanol, uniformly stirring, and then adding a cationic surfactant to obtain a modified liquid;
s3, adding the ground zeolite into the modified liquid, heating and refluxing, washing with ethanol, and drying to obtain modified zeolite;
the mass ratio of the zeolite to the silane coupling agent to the cationic surfactant is 1 (0.06-0.1) (0.05-0.08).
Preferably, the mass ratio of the zeolite, the silane coupling agent and the cationic surfactant is 1:0.08:0.06.
The mass ratio of the zeolite to the silane coupling agent to the cationic surfactant is controlled to be 1 (0.06-0.1) (0.05-0.08), so that the internal pore canal and the specific surface area of the zeolite can be maintained, the stability of the low-atomization calcium-zinc stabilizer for PVC is not affected, and meanwhile, the hydrophobicity of the modified zeolite can be improved. Thereby reducing the atomization value of the low-atomization calcium zinc stabilizer for PVC. When the mass ratio of the zeolite to the silane coupling agent to the cationic surfactant is 1:0.08:0.06, the atomization value of the stabilizer is lower, and the color difference value of the sample piece is lower under 5min, 7min and 10 min.
Preferably, the silane coupling agent is a fluorine-containing silane coupling agent.
The fluorine atom is introduced into the fluorine-containing silane coupling agent, so that the hydrophobicity of the modified zeolite is further improved, and the atomization value of the low-atomization calcium-zinc stabilizer for PVC is reduced.
Preferably, the fluorine-containing silane coupling agent is heptadecafluorodecyl triethoxysilane.
The heptadecafluorodecyl triethoxysilane has low surface tension and good compounding effect with a cationic surfactant, and the carbon chain length of the heptadecafluorodecyl triethoxysilane, namely the hydrophobic chain length, improves the hydrophobicity of the modified zeolite.
Preferably, the cationic surfactant is a dialkyl quaternary ammonium salt.
Preferably, the dialkyl quaternary ammonium salt is octadecyl diester quaternary ammonium salt YH-866.
The octadecyl diester quaternary ammonium salt YH-866 not only has hygroscopicity, but also has stronger hydrophobicity of dialkyl, the carbon chain length of the octadecyl diester quaternary ammonium salt YH-866, the hydrophobic chain length, and the interaction of the octadecyl diester quaternary ammonium salt YH-866 and the heptadecafluorodecyl triethoxysilane long carbon chain reduce the water content of zeolite.
In a second aspect, the application provides a method for testing stability of a low-atomization calcium zinc stabilizer for PVC, which is realized by adopting the following technical scheme:
a method for testing the stability of a low-atomization calcium-zinc stabilizer for PVC comprises the following steps:
s1, uniformly mixing PVC, stone powder, titanium dioxide R105, stearic acid, paraffin and a low-atomization calcium zinc stabilizer for PVC to obtain a mixture;
s2, setting the temperature of an open mill to be 210 ℃, wherein the gap of a roller of the open mill is 4mm;
s3, placing the mixture into an open mill, and sampling at 3min, 5min, 7min and 10min respectively;
s4, taking the 3min sample as a standard component, and measuring the color difference values of the sample at 5min, 7min and 10min respectively.
Preferably, the mass ratio of the PVC, the stone powder, the titanium pigment, the stearic acid, the paraffin and the low-atomization calcium zinc stabilizer for PVC is 375:100:5:2.5:4:10.
The low-atomization calcium-zinc stabilizer for PVC has excellent stability, and the color difference value of the sample piece is low under 5min, 7min and 10 min.
In summary, the present application has the following beneficial effects:
1. according to the method, the zeolite is modified by the silane coupling agent and the cationic surfactant together, the silane coupling agent is chemically bonded with hydroxyl groups on the surface of the zeolite, so that the silicon hydroxyl groups on the surface of the zeolite are reduced, hydrophobic hydrocarbon chains are loaded on the surface of the zeolite, the cationic surfactant is easy to electrostatically adsorb negative charges on the surface of the zeolite to enable the zeolite to be hydrophobic, the silane coupling agent and the cationic surfactant together act, the water content of the zeolite is further reduced, and therefore the atomization value of the stabilizer is reduced.
2. The application adopts the heptadecafluorodecyl triethoxysilane, the surface tension is low, the compounding effect of the heptadecafluorodecyl triethoxysilane and the cationic surfactant is good, and the carbon chain length of the heptadecafluorodecyl triethoxysilane, namely the hydrophobic chain length, improves the hydrophobicity of the modified zeolite.
3. The application not only has hygroscopicity, but also has stronger hydrophobicity of dialkyl through the octadecyl diester quaternary ammonium salt YH-866, and the carbon chain length, hydrophobic chain length and interaction of the octadecyl diester quaternary ammonium salt YH-866 and heptadecafluorodecyl triethoxysilane long carbon chain reduce the water content of zeolite.
Detailed Description
The present application is described in further detail below with reference to examples.
Preparation example
Preparation examples 1 to 6 provide a modified zeolite, and preparation example 1 is given as an example.
The preparation method of the modified zeolite provided in preparation example 1 comprises the following preparation steps:
s1, grinding 10g of 4A zeolite to a particle size not larger than 100 meshes for later use;
s2, adding 0.6g of silane coupling agent KH-550 into 200mL of isopropanol, uniformly stirring, and adding 0.5g of cetyltrimethylammonium bromide to obtain a modified liquid;
s3, adding the ground zeolite into the modified liquid, heating and refluxing for 2 hours at 90 ℃, washing with ethanol three times, and drying for 6 hours at 100 ℃ to obtain the modified zeolite.
Preparation examples 2 to 3 differ from preparation example 1 only in that: the quality of each preparation raw material of the modified zeolite is different, and the specific quality is shown in table 1.
TABLE 1 preparation examples 1-3 modified zeolite mass/g of each preparation raw material
Preparation example 4 differs from preparation example 3 only in that: the silane coupling agent KH-550 is replaced by trifluoropropane trimethoxysilane with equal mass.
Preparation 5 differs from preparation 3 only in that: the silane coupling agent KH-550 is replaced by heptadecafluorodecyl triethoxysilane with equal mass.
Preparation 6 differs from preparation 5 only in that: cetyl trimethylammonium bromide is replaced by octadecyl diester-based quaternary ammonium salt YH-866 (purchased from Zhengzhou Yi and Fine chemical Co., ltd.).
Preparation of comparative example
Comparative example 1 was prepared, differing from preparation example 1 only in that: the silane coupling agent KH-550 is replaced by hexadecyl trimethyl ammonium bromide with equal mass.
Comparative example 2 was prepared, differing from preparation example 1 only in that: the equal mass of cetyl trimethyl ammonium bromide is replaced by a silane coupling agent KH-550.
Examples
Examples 1-9 provide a low-fogging calcium zinc stabilizer for PVC, and are described below by way of example 1.
The preparation method of the low-atomization calcium zinc stabilizer for PVC provided in the embodiment 1 comprises the following steps:
mixing 35g zinc stearate, 15g calcium stearate, 5g stearoyl benzoyl methane, 15g hydrotalcite, 25g modified zeolite (from preparation example 1) and 5g dihydropyridine uniformly to obtain the low-atomization calcium zinc stabilizer for PVC.
Examples 2-4 differ from example 1 only in that: the low-atomization calcium zinc stabilizer for PVC has different quality of raw materials for preparation, and is specifically shown in Table 2.
TABLE 2 EXAMPLES 1-4 Low-fogging calcium Zinc stabilizers for PVC mass/g of raw materials for each preparation
Examples 5-9 differ from example 3 only in that: the sources of the modified zeolite are different and are shown in Table 3.
TABLE 3 sources of modified zeolites examples 3, 5-9
| Group of | Example 3 | Example 5 | Example 6 | Example 7 | Example 8 | Example 9 |
| Modified zeolite source | Preparation example 1 | Preparation example 2 | Preparation example 3 | Preparation example 4 | Preparation example 5 | Preparation example 6 |
Comparative example
Comparative example 1 differs from example 4 only in that: the modified zeolite was derived from the preparation of comparative example 1.
Comparative example 2 differs from example 4 only in that: the modified zeolite was derived from preparation comparative example 2.
Comparative example 3 differs from example 4 only in that: the quality of the modified zeolite is replaced by 4A zeolite.
Atomization performance test
For the low fogging calcium zinc stabilizers for PVC prepared in examples 1-9 and comparative examples 1-3 of the present application, fogging condensate values were recorded according to the PV3015 standard, and the test results are shown in Table 4.
Table 4 atomization test data
Wherein the tin-cloud organotin stabilizer YT181 is purchased from Zibo & Yue trade Co.
The test data of table 4 are described in detail below.
From the experimental data of example 4 and comparative example 3, it is understood that the modification of zeolite 4A herein reduces the haze condensate number of the stabilizer, as the modified zeolite reduces the water content of the zeolite.
From the experimental data of example 4 and comparative examples 1 and 2, it is understood that the silane coupling agent and the cationic surfactant together modify the zeolite to reduce the water content of the zeolite, thereby reducing the atomization value of the stabilizer.
From the experimental data of examples 3, 5 and 6, the haze condensate value of the low-fogging calcium zinc stabilizer for PVC is lower when the mass ratio of zeolite, silane coupling agent and cationic surfactant is 1:0.08:0.06.
From the experimental data of examples 6, 7 and 8, it is understood that example 6 is silane coupling agent KH-550, example 7 is trifluoropropane trimethoxysilane, example 8 is heptadecafluorodecyl triethoxysilane, and the haze condensate value of the corresponding stabilizer of example 8 is significantly lower than that of example 7 and lower than that of example 6. This is because the heptadecafluorodecyl triethoxysilane has low surface tension and good compounding effect with the cationic surfactant, and the carbon chain length of the heptadecafluorodecyl triethoxysilane, namely the hydrophobic chain length, improves the hydrophobicity of the modified zeolite.
From the experimental data of examples 8 and 9, it is understood that example 8 is cetyltrimethylammonium bromide, example 9 is octadecyl diester quaternary ammonium salt YH-866, and the misting condensate value of the corresponding stabilizer of example 9 is significantly lower than that of the corresponding stabilizer of example 8. This is because the octadecyl diester quaternary ammonium salt YH-866 not only has hygroscopicity, but also has stronger hydrophobicity of dialkyl, the carbon chain length of the octadecyl diester quaternary ammonium salt YH-866, the hydrophobic chain length, and the interaction of the octadecyl diester quaternary ammonium salt YH-866 and the heptadecafluorodecyl triethoxysilane long carbon chain reduces the water content of zeolite.
Stability test
For the low-atomization calcium zinc stabilizer for PVC prepared in examples 1-9 and comparative examples 1-3, stability test was performed, the test results are shown in Table 5, and the test steps are as follows:
s1, uniformly mixing PVC, stone powder, titanium dioxide R105, stearic acid, paraffin and a low-atomization calcium zinc stabilizer for PVC according to a mass ratio of 375:100:5:2.5:4:10 to obtain a mixture;
s2, setting the temperature of an open mill to be 210 ℃, wherein the gap of a roller of the open mill is 4mm;
s3, placing the mixture into an open mill, and sampling at 3min, 5min, 7min and 10min respectively;
s4, taking the 3min sample as a standard component, and measuring delta E values of the sample at 5min, 7min and 10min respectively by using a color difference meter.
TABLE 5 stability test results
The test data of table 5 are used in the following to describe the present application in detail.
The low-atomization calcium-zinc stabilizer for PVC, which is prepared by the application, has low atomization value, excellent stability and low color difference value of sample pieces under 5min, 7min and 10 min.
From the experimental data of example 4 and comparative examples 1, 2 and 3, it is understood that the modification of zeolite by the silane coupling agent and the cationic surfactant does not decrease the stability of the low-atomizing calcium-zinc stabilizer for PVC, but rather improves the stability, and the color difference value of the sample is low in 5min, 7min and 10 min.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (5)
1. The low-atomization calcium-zinc stabilizer for PVC is characterized by comprising the following raw materials in parts by weight: 25-35 parts of zinc stearate, 15-30 parts of calcium stearate, 3-5 parts of stearoyl benzoyl methane, 10-40 parts of hydrotalcite and 10-30 parts of modified zeolite;
the preparation raw materials also comprise 1-5 parts of dihydropyridine or 3-7 parts of 1, 3-dimethyl-6-amino uracil;
the modified zeolite is obtained by modifying together a silane coupling agent and a cationic surfactant;
the preparation method of the modified zeolite comprises the following steps:
s1, grinding zeolite for later use;
s2, adding a silane coupling agent into isopropanol, uniformly stirring, and then adding a cationic surfactant to obtain a modified liquid;
s3, adding the ground zeolite into the modified liquid, heating and refluxing, washing with ethanol, and drying to obtain modified zeolite;
the mass ratio of the zeolite to the silane coupling agent to the cationic surfactant is 1:0.08:0.06;
the silane coupling agent is a fluorine-containing silane coupling agent;
the cationic surfactant is a dialkyl quaternary ammonium salt.
2. The low-atomizing calcium zinc stabilizer for PVC according to claim 1, wherein the fluorine-containing silane coupling agent is heptadecafluorodecyl triethoxysilane.
3. A low atomizing calcium zinc stabilizer for PVC according to claim 1, wherein the dialkyl quaternary ammonium salt is octadecyl diester quaternary ammonium salt YH-866.
4. The method for testing the stability of the low-atomization calcium-zinc stabilizer for PVC is characterized by comprising the following steps of:
s1, uniformly mixing PVC, stone powder, titanium dioxide R105, stearic acid, paraffin and the low-atomization calcium zinc stabilizer for PVC according to claim 1 to obtain a mixture;
s2, setting the temperature of an open mill to be 210 ℃, wherein the gap of a roller of the open mill is 4mm;
s3, placing the mixture into an open mill, and sampling at 3min, 5min, 7min and 10min respectively;
s4, taking the 3min sample as a standard component, and measuring the color difference values of the sample at 5min, 7min and 10min respectively.
5. The method for testing the stability of the low-atomizing calcium zinc stabilizer for the PVC according to claim 1, wherein the mass ratio of the PVC, the stone powder, the titanium pigment, the stearic acid, the paraffin wax to the low-atomizing calcium zinc stabilizer for the PVC is 375:100:5:2.5:4:10.
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| CN103212384B (en) * | 2013-04-01 | 2015-04-22 | 上海师范大学 | Preparation method of poly siloxane quaternary ammonium modified zeolite and application thereof |
| CN105778338B (en) * | 2016-03-25 | 2017-07-28 | 上海天原集团胜德塑料有限公司 | Environment-friendly type soft polyvinyl chloride granules |
| CN107200869A (en) * | 2017-07-01 | 2017-09-26 | 武汉金牛经济发展有限公司 | A kind of Ca-Zn composite heat stabilizer and its application and preparation method |
| CN110982194A (en) * | 2019-12-18 | 2020-04-10 | 惠州市兴邦新材料科技有限公司 | Calcium-zinc stabilizer for PVC (polyvinyl chloride) and preparation method thereof |
| CN112759867A (en) * | 2021-04-12 | 2021-05-07 | 广讯检测（广东）有限公司 | Calcium-zinc stabilizer for PVC-UH (polyvinyl chloride-ultra high-temperature) pipe and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109825002A (en) * | 2019-02-18 | 2019-05-31 | 杭州凌洲塑胶科技有限公司 | A kind of PVC Environment-friendlycalcium calcium zinc stabilizer |
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