CN108503976B - Modified polyvinyl chloride material and preparation method thereof - Google Patents
Modified polyvinyl chloride material and preparation method thereof Download PDFInfo
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- 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
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C08K3/24—Acids; Salts thereof
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Abstract
The invention relates to a preparation method of a modified polyvinyl chloride material, which comprises the following steps: mixing titanium dioxide and carbon black, heating to 60-80 ℃, adding a titanate coupling agent, stirring for 10-20 min, drying, and grinding to obtain a weather-resistant auxiliary agent with the particle size of less than 100nm, wherein the mass ratio of the titanium dioxide to the carbon black to the titanate coupling agent is 4-7: 2-5: 1; and uniformly mixing the polyvinyl chloride, the auxiliary material and the weather-resistant auxiliary agent, and then extruding and molding to obtain the modified polyvinyl chloride material. According to the invention, through pretreatment, titanium dioxide, carbon black and a titanate coupling agent can be better dispersed and combined with polyvinyl chloride, the synergistic uvioresistant effect of the titanium dioxide and the carbon black can be improved, and simultaneously, a carbonate coupling agent is more beneficial to the combination of the titanium dioxide, the carbon black and the polyvinyl chloride than other coupling agents, so that the ultraviolet resistance of the modified polyvinyl chloride material is improved, the modified polyvinyl chloride material is not easy to decompose, age and change color, the mechanical property change is small, the excellent weather resistance is obtained, and the modified polyvinyl chloride material is particularly suitable for preparing various PVC pipes.
Description
Technical Field
The invention relates to the field of materials, in particular to a modified polyvinyl chloride material and a preparation method thereof.
Background
Polyvinyl chloride (PVC)) The PVC is white powder with an amorphous structure, the branching degree is small, the molecular weight of PVC produced in industry is generally within the range of 5-12 ten thousand, the PVC has no fixed melting point, the PVC begins to soften at 80-85 ℃, becomes a viscoelastic state at 130 ℃, begins to change into a viscous state at 160-180 ℃, has good mechanical property, the tensile strength is about 60MPa, and the impact strength is 5-10 kJ/m2It has excellent dielectric performance and fire resistance, and is stable to organic and inorganic acids, alkalis and salts. Therefore, PVC is an important building engineering material and is widely applied to the fields of building materials, light industry, agriculture and the like, and products of the PVC are mainly applied to the aspects of pipes such as drainage pipes, electric power threading pipes and the like.
However, when a general PVC material is used outdoors, it is easily decomposed by ultraviolet irradiation to generate hydrogen chloride, and further, it is decomposed by auto-catalysis to cause aging and discoloration, and the physical and mechanical properties are rapidly decreased, which affects the use of customers.
Disclosure of Invention
Therefore, it is necessary to provide a method for preparing a modified polyvinyl chloride material which is not easy to age and discolor and has small change of mechanical properties.
A preparation method of a modified polyvinyl chloride material comprises the following steps:
mixing titanium dioxide and carbon black, heating to 60-80 ℃, adding a titanate coupling agent, stirring for 10-20 min, drying, and grinding to obtain a weather-resistant auxiliary agent with the particle size of less than 100nm, wherein the mass ratio of the titanium dioxide to the carbon black to the titanate coupling agent is 4-7: 2-5: 1;
and uniformly mixing the polyvinyl chloride, the auxiliary material and the weather-resistant auxiliary agent, and then extruding and molding to obtain the modified polyvinyl chloride material.
In one embodiment, the mass ratio of the titanium dioxide to the carbon black to the titanate coupling agent is 6:3: 1.
In one embodiment, the polyvinyl chloride is 100 parts by weight, the weather-resistant auxiliary agent is 2-10 parts by weight, and the auxiliary material is 14-41 parts by weight.
In one embodiment, the polyvinyl chloride is 100 parts by weight, the weather-resistant auxiliary agent is 5-7 parts by weight, and the auxiliary material is 14-41 parts by weight.
In one embodiment, the step of uniformly mixing the polyvinyl chloride, the auxiliary material and the weather-resistant auxiliary agent specifically comprises the following steps: mixing polyvinyl chloride, auxiliary materials and the weather-resistant auxiliary agent to obtain a mixture, stirring at 1200-1500 r/min until the temperature of the mixture reaches 110-130 ℃, and then stirring at 400-600 r/min until the temperature of the mixture is reduced to 40-50 ℃.
In one embodiment, the auxiliary materials comprise 3-6 parts by weight of a stabilizer, 10-30 parts by weight of a filler and 1-5 parts by weight of a lubricant.
In one embodiment, the stabilizer is a calcium zinc stabilizer.
In one embodiment, the filler is light calcium carbonate or activated calcium carbonate.
In one embodiment, the lubricant is an internal lubricant and an external lubricant.
The invention also provides a modified polyvinyl chloride material prepared by the preparation method of the modified polyvinyl chloride material.
The invention mixes titanium dioxide, carbon black and titanate coupling agent according to a specific proportion, stirs, dries and grinds at high temperature to obtain weather-proof auxiliary agent with grain diameter below 100nm, then mixes the weather-proof auxiliary agent, polyvinyl chloride and auxiliary material evenly and extrudes and forms to obtain the modified polyvinyl chloride material. Therefore, titanium dioxide, carbon black and titanate coupling agent can be better dispersed and combined with polyvinyl chloride through pretreatment, the synergistic uvioresistant effect of the titanium dioxide and the carbon black can be improved, and meanwhile, the carbonate coupling agent is more favorable for the combination of the titanium dioxide, the carbon black and the polyvinyl chloride than other coupling agents, so that the ultraviolet resistance of the modified polyvinyl chloride material is improved, the modified polyvinyl chloride material is not easy to decompose, age and change color, the mechanical property change is small, the excellent weather resistance is obtained, the service life of the product under outdoor conditions is prolonged, and the modified polyvinyl chloride material is particularly suitable for preparing various PVC pipes.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The preparation method of the modified polyvinyl chloride material of one embodiment of the invention comprises the following steps of S1-S2:
s1, mixing titanium dioxide and carbon black, heating to 60-80 ℃, adding a titanate coupling agent, stirring for 10-20 min, drying, and grinding to obtain the weather-resistant auxiliary agent with the particle size of less than 100nm, wherein the mass ratio of the titanium dioxide to the carbon black to the titanate coupling agent is 4-7: 2-5: 1.
In one embodiment, the mass ratio of the titanium dioxide to the carbon black to the titanate coupling agent is 6:3:1, the ratio can obtain better performance compared with other ratios, and the carbon black and the titanium dioxide have a synergistic effect, but excessive carbon black is not suitable to be added, otherwise the mechanical property of the modified polyvinyl chloride material is easily reduced.
And S2, uniformly mixing the polyvinyl chloride, the auxiliary materials and the weather-resistant auxiliary agent, and then extruding and molding to obtain the modified polyvinyl chloride material.
Specifically, uniformly mixing the polyvinyl chloride, the auxiliary materials and the weather-resistant auxiliary agent specifically comprises the following steps: mixing polyvinyl chloride, auxiliary materials and weather-resistant auxiliary agents to obtain a mixture, stirring at 1200-1500 r/min until the temperature of the mixture reaches 110-130 ℃, and then stirring at 400-600 r/min until the temperature of the mixture is reduced to 40-50 ℃. In the process of uniformly mixing, materials generate heat through high-speed friction in high-speed stirring equipment, and the temperature control is very important.
In one embodiment, the polyvinyl chloride is 100 parts by weight, the weather-resistant auxiliary agent is 2-10 parts by weight, and the auxiliary material is 14-41 parts by weight.
In one embodiment, the polyvinyl chloride is 100 parts by weight, the weather-resistant auxiliary agent is 5-7 parts by weight, and the auxiliary material is 14-41 parts by weight. With the gradually increased addition amount of the weather-resistant auxiliary agent, the color difference change of the modified polyvinyl chloride material is gradually reduced, and simultaneously the tensile yield strength is gradually reduced, namely the weather resistance of the product is gradually improved, but the tensile yield strength of the product is influenced by the excessive addition amount, so the proportion range is more preferable.
In one embodiment, the auxiliary materials comprise 3-6 parts by weight of a stabilizer, 10-30 parts by weight of a filler and 1-5 parts by weight of a lubricant.
Optionally, the polyvinyl chloride has an average degree of polymerization of 800 to 1200. Alternatively, the stabilizer is a calcium zinc stabilizer, the filler is light calcium carbonate or activated calcium carbonate, and the lubricant is an internal lubricant and an external lubricant, which are not limited thereto and may be selected as desired.
The invention also provides a modified polyvinyl chloride material prepared by the preparation method of the modified polyvinyl chloride material.
The invention mixes titanium dioxide, carbon black and titanate coupling agent according to a specific proportion, stirs, dries and grinds at high temperature to obtain weather-proof auxiliary agent with grain diameter below 100nm, then mixes the weather-proof auxiliary agent, polyvinyl chloride and auxiliary material evenly and extrudes and forms to obtain the modified polyvinyl chloride material. Therefore, titanium dioxide, carbon black and titanate coupling agent can be better dispersed and combined with polyvinyl chloride through pretreatment, the synergistic uvioresistant effect of the titanium dioxide and the carbon black can be improved, and meanwhile, the carbonate coupling agent is more favorable for the combination of the titanium dioxide, the carbon black and the polyvinyl chloride than other coupling agents, so that the ultraviolet resistance of the modified polyvinyl chloride material is improved, the modified polyvinyl chloride material is not easy to decompose, age and change color, the mechanical property change is small, the excellent weather resistance is obtained, the service life of the product under outdoor conditions is prolonged, and the modified polyvinyl chloride material is particularly suitable for preparing various PVC pipes.
The following are specific examples.
Example 1
Adding 6kg of titanium dioxide and 3kg of carbon black into high-speed stirring equipment, stirring, gradually heating to 70 ℃, adding 1kg of titanate coupling agent, stirring for 10-20 min, taking out, drying, and grinding in a grinding machine to obtain the weather-resistant auxiliary agent with the particle size of less than 100 nm.
Stirring 2kg of weather-resistant auxiliary agent and 100kg of PVC in a high-speed mixer at a low speed (below 100 r/min) for 5min, then adding 4kg of calcium-zinc stabilizer, 15kg of active calcium carbonate, 2kg of internal lubricant and external lubricant to obtain a mixture, stirring at 1200-1500 r/min until the temperature of the mixture reaches 120 ℃, then placing the mixture into a cold mixing device, stirring at 500r/min until the temperature of the mixture is reduced to 40-50 ℃, and extruding and molding through an extruder to obtain the modified polyvinyl chloride material pipe.
Example 2
Adding 6kg of titanium dioxide and 3kg of carbon black into high-speed stirring equipment, stirring, gradually heating to 70 ℃, adding 1kg of titanate coupling agent, stirring for 10-20 min, taking out, drying, and grinding in a grinding machine to obtain the weather-resistant auxiliary agent with the particle size of less than 100 nm.
Stirring 6kg of weather-resistant auxiliary agent and 100kg of PVC in a high-speed mixer at a low speed (below 100 r/min) for 5min, then adding 4kg of calcium-zinc stabilizer, 15kg of active calcium carbonate, 2kg of internal lubricant and external lubricant to obtain a mixture, stirring at 1200-1500 r/min until the temperature of the mixture reaches 120 ℃, then placing the mixture into a cold mixing device, stirring at 500r/min until the temperature of the mixture is reduced to 40-50 ℃, and extruding and molding through an extruder to obtain the modified polyvinyl chloride material pipe.
Example 3
Adding 6kg of titanium dioxide and 3kg of carbon black into high-speed stirring equipment, stirring, gradually heating to 70 ℃, adding 1kg of titanate coupling agent, stirring for 10-20 min, taking out, drying, and grinding in a grinding machine to obtain the weather-resistant auxiliary agent with the particle size of less than 100 nm.
Stirring 10kg of weather-resistant auxiliary agent and 100kg of PVC in a high-speed mixer at a low speed (below 100 r/min) for 5min, then adding 4kg of calcium-zinc stabilizer, 15kg of light calcium carbonate, 2kg of internal lubricant and external lubricant to obtain a mixture, stirring at 1200-1500 r/min until the temperature of the mixture reaches 120 ℃, then placing the mixture into a cold mixing device, stirring at 500r/min until the temperature of the mixture is reduced to 40-50 ℃, and extruding and molding through an extruder to obtain the modified polyvinyl chloride material pipe.
Example 4
Adding 4kg of titanium dioxide and 5kg of carbon black into high-speed stirring equipment, stirring, gradually heating to 70 ℃, adding 1kg of titanate coupling agent, stirring for 10-20 min, taking out, drying, and grinding in a grinding machine to obtain the weather-resistant auxiliary agent with the particle size of less than 100 nm.
Stirring 2kg of weather-resistant auxiliary agent and 100kg of PVC in a high-speed mixer at a low speed (below 100 r/min) for 5min, then adding 4kg of calcium-zinc stabilizer, 15kg of active calcium carbonate, 2kg of internal lubricant and external lubricant to obtain a mixture, stirring at 1200-1500 r/min until the temperature of the mixture reaches 120 ℃, then placing the mixture into a cold mixing device, stirring at 500r/min until the temperature of the mixture is reduced to 40-50 ℃, and extruding and molding through an extruder to obtain the modified polyvinyl chloride material pipe.
Comparative example 1
Adding 8kg of titanium dioxide and 1kg of carbon black into high-speed stirring equipment, stirring, gradually heating to 70 ℃, adding 1kg of titanate coupling agent, stirring for 10-20 min, taking out, drying, and grinding in a grinding machine to obtain the weather-resistant auxiliary agent with the particle size of less than 100 nm.
Stirring 2kg of weather-resistant auxiliary agent and 100kg of PVC in a high-speed mixer at a low speed (below 100 r/min) for 5min, then adding 4kg of calcium-zinc stabilizer, 15kg of active calcium carbonate, 2kg of internal lubricant and external lubricant to obtain a mixture, stirring at 1200-1500 r/min until the temperature of the mixture reaches 120 ℃, then placing the mixture into a cold mixing device, stirring at 500r/min until the temperature of the mixture is reduced to 40-50 ℃, and extruding and molding through an extruder to obtain the modified polyvinyl chloride material pipe.
Comparative example 2
100kg of PVC, 4kg of calcium-zinc stabilizer, 15kg of active calcium carbonate, 2kg of internal lubricant and external lubricant, 6kg of titanium dioxide (with the particle size of less than 100 nm), 3kg of carbon black (with the particle size of less than 100 nm) and 1kg of titanate coupling agent are put into a high-speed mixer to obtain a mixture, the mixture is stirred under the condition of 1200-1500 r/min until the temperature of the mixture reaches 120 ℃, then the mixture is put into cold mixing equipment and stirred under the condition of 500r/min until the temperature of the mixture is reduced to 40-50 ℃, and then the mixture is extruded and molded by an extruder to obtain the modified polyvinyl chloride material pipe.
Comparative example 3
Adding 6kg of titanium dioxide and 3kg of carbon black into high-speed stirring equipment, stirring, gradually heating to 70 ℃, adding 1kg of silane coupling agent, stirring for 10-20 min, taking out, drying, and grinding in a grinding machine to obtain the weather-resistant auxiliary agent with the particle size of less than 100 nm.
Stirring 2kg of weather-resistant auxiliary agent and 100kg of PVC in a high-speed mixer at a low speed (below 100 r/min) for 5min, then adding 4kg of calcium-zinc stabilizer, 15kg of active calcium carbonate, 2kg of internal lubricant and external lubricant to obtain a mixture, stirring at 1200-1500 r/min until the temperature of the mixture reaches 120 ℃, then placing the mixture into a cold mixing device, stirring at 500r/min until the temperature of the mixture is reduced to 40-50 ℃, and extruding and molding through an extruder to obtain the modified polyvinyl chloride material pipe.
Comparative example 4
Adding 9kg of titanium dioxide into high-speed stirring equipment, gradually heating to 70 ℃, adding 1kg of titanate coupling agent, stirring for 10-20 min, taking out, drying, and grinding in a grinding machine to obtain the weather-resistant auxiliary agent with the particle size of less than 100 nm.
Stirring 2kg of weather-resistant auxiliary agent and 100kg of PVC in a high-speed mixer at a low speed (below 100 r/min) for 5min, then adding 4kg of calcium-zinc stabilizer, 15kg of active calcium carbonate, 2kg of internal lubricant and external lubricant to obtain a mixture, stirring at 1200-1500 r/min until the temperature of the mixture reaches 120 ℃, then placing the mixture into a cold mixing device, stirring at 500r/min until the temperature of the mixture is reduced to 40-50 ℃, and extruding and molding through an extruder to obtain the modified polyvinyl chloride material pipe.
Comparative example 5
Adding 9kg of carbon black into high-speed stirring equipment, gradually heating to 70 ℃, adding 1kg of titanate coupling agent, stirring for 10-20 min, taking out, drying, and grinding in a grinder to obtain the weather-resistant auxiliary agent with the particle size of less than 100 nm.
Stirring 2kg of weather-resistant auxiliary agent and 100kg of PVC in a high-speed mixer at a low speed (below 100 r/min) for 5min, then adding 4kg of calcium-zinc stabilizer, 15kg of active calcium carbonate, 2kg of internal lubricant and external lubricant to obtain a mixture, stirring at 1200-1500 r/min until the temperature of the mixture reaches 120 ℃, then placing the mixture into a cold mixing device, stirring at 500r/min until the temperature of the mixture is reduced to 40-50 ℃, and extruding and molding through an extruder to obtain the modified polyvinyl chloride material pipe.
The dn110 drain pipes prepared in examples 1-4 and comparative examples 1-5 were subjected to ultraviolet aging for 1000 hours, and the results of comparing the pipe color difference change condition and the tensile yield strength condition are shown in tables 1 and 2, respectively.
From the change of color difference, the examples 1 to 4 are all smaller than the comparative examples 1 to 4 in the change trend, wherein the example 3 is better than the example 2, the example 2 is better than the example 1, the example 1 is better than the example 4, and the comparative example 5 has small change of color difference because the product is black. From the aspect of tensile yield strength, the tensile yield strength of each example is smaller than that of the comparative example, wherein the tensile property of example 1 is better than that of examples 2-4. According to examples 1 to 4, when the addition amount of the weather-resistant auxiliary agent is gradually increased, the color difference change is gradually reduced, the weather resistance of the product is gradually improved, but when the addition amount is excessive, the tensile yield strength of the product is gradually reduced. According to the example 1, the comparative example 4 and the comparative example 5, when the titanium dioxide and the carbon black are added simultaneously, the change of the tensile yield strength of the product is better than that of the product obtained by independently adding the titanium dioxide or the carbon black (the total mass is the same), which shows that the titanium dioxide and the carbon black are added simultaneously to have a synergistic effect. According to the embodiment 3 and the comparative example 2, the titanium dioxide, the carbon black and the titanate coupling agent are pretreated to prepare the weather-resistant auxiliary agent for product production, and under the condition of the same addition amount, the product has obvious advantages in the aspects of tensile yield strength change and color difference change, which shows that the treatment processing technology can bring obvious beneficial effects.
TABLE 1
TABLE 2
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the modified polyvinyl chloride material is characterized by comprising the following steps:
mixing titanium dioxide and carbon black, heating to 60-80 ℃, adding a titanate coupling agent, stirring for 10-20 min, drying, and grinding to obtain a weather-resistant auxiliary agent with the particle size of less than 100nm, wherein the mass ratio of the titanium dioxide to the carbon black to the titanate coupling agent is 6:3: 1;
and uniformly mixing the polyvinyl chloride, the auxiliary material and the weather-resistant auxiliary agent, and then extruding and molding to obtain the modified polyvinyl chloride material.
2. The method for preparing a modified polyvinyl chloride material according to claim 1, wherein the polyvinyl chloride has an average degree of polymerization of 800 to 1200.
3. The preparation method of the modified polyvinyl chloride material according to claim 1, wherein the polyvinyl chloride is 100 parts by weight, the weather-resistant auxiliary agent is 2-10 parts by weight, and the auxiliary material is 14-41 parts by weight.
4. The preparation method of the modified polyvinyl chloride material according to claim 3, wherein the polyvinyl chloride is 100 parts by weight, the weather-resistant auxiliary agent is 5-7 parts by weight, and the auxiliary material is 14-41 parts by weight.
5. The preparation method of the modified polyvinyl chloride material according to claim 1, wherein the step of uniformly mixing the polyvinyl chloride, the auxiliary material and the weather-resistant auxiliary agent specifically comprises the following steps: mixing polyvinyl chloride, auxiliary materials and the weather-resistant auxiliary agent to obtain a mixture, stirring at 1200-1500 r/min until the temperature of the mixture reaches 110-130 ℃, and then stirring at 400-600 r/min until the temperature of the mixture is reduced to 40-50 ℃.
6. The method for preparing the modified polyvinyl chloride material according to any one of claims 1 to 5, wherein the auxiliary materials comprise 3 to 6 parts by weight of the stabilizer, 10 to 30 parts by weight of the filler and 1 to 5 parts by weight of the lubricant.
7. The method for preparing a modified polyvinyl chloride material according to claim 6, wherein the stabilizer is a calcium zinc stabilizer.
8. The method for preparing a modified polyvinyl chloride material according to claim 6, wherein the filler is light calcium carbonate or activated calcium carbonate.
9. The method for preparing a modified polyvinyl chloride material according to claim 6, wherein the lubricant is an internal lubricant and an external lubricant.
10. A modified polyvinyl chloride material prepared by the method of any one of claims 1 to 9.
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| CN113603979A (en) * | 2021-06-25 | 2021-11-05 | 杭州联通管业有限公司 | Weather-resistant polyvinyl chloride pipe and preparation method thereof |
| CN113969030A (en) * | 2021-12-07 | 2022-01-25 | 广东红波新材料集团有限公司 | Method for manufacturing photovoltaic matched PVC tile by using weather-resistant reinforced modified filler |
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| CN102838964B (en) * | 2012-08-29 | 2014-01-08 | 浙江大学 | High-weather-fastness polysulfide sealant |
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Effective date of registration: 20201229 Address after: 7 Yuanhe Road, Wuqing District, Tianjin Patentee after: RiFeng enterprise (Tianjin) Co.,Ltd. Address before: Block 2, No.19, area D, Sanshui Industrial Park, Foshan, Guangdong 528000 Patentee before: RIFENG TECHNOLOGY Co.,Ltd. Patentee before: RIFENG ENTERPRISE GROUP Co.,Ltd. Patentee before: FOSHAN RIFENG ENTERPRISE Co.,Ltd. |