CN113831664A - Large-caliber PVC pipe material and preparation method and application thereof - Google Patents
Large-caliber PVC pipe material and preparation method and application thereof Download PDFInfo
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- CN113831664A CN113831664A CN202111155489.6A CN202111155489A CN113831664A CN 113831664 A CN113831664 A CN 113831664A CN 202111155489 A CN202111155489 A CN 202111155489A CN 113831664 A CN113831664 A CN 113831664A
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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
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Rigid Pipes And Flexible Pipes (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
Abstract
The invention discloses a large-caliber PVC pipe material and a preparation method and application thereof. The large-caliber PVC pipe material comprises the following components: PVC, calcium carbonate, a calcium-zinc composite heat stabilizer, a styrene-acrylonitrile copolymer, a butyl acrylate-methyl methacrylate copolymer, titanium dioxide and an impact modifier, wherein the calcium-zinc composite heat stabilizer is a mixture of calcium stearate, zinc stearate, silane coupling agent modified fumed silica and hydroxyl-terminated pentaerythritol adipate. According to the invention, the thermal stability of the material is improved by the calcium-zinc composite heat stabilizer, the plasticizing performance of the material is improved by the butyl acrylate-methyl methacrylate copolymer, the plasticization is promoted by the styrene-acrylonitrile copolymer in a synergistic manner, the melt strength of the system can be enhanced, the flow property is increased, the prepared PVC pipe material system has excellent thermal stability, high plasticizing degree and high melt strength, and the large-caliber PVC pipe prepared by using the material system has excellent comprehensive performance.
Description
Technical Field
The invention relates to the technical field of PVC pipes, in particular to a large-caliber PVC pipe material and a preparation method and application thereof.
Background
The PVC pipeline has the advantages of excellent flame retardance, wear resistance, chemical corrosion resistance, mechanical property, electrical insulation and the like, and is widely applied to the fields of industry, building, municipal administration, agriculture and the like. However, due to the technical problems of poor thermal stability, poor plasticizing performance and the like in PVC processing, PVC pipes in the market are mainly medium and small-caliber, and large-caliber PVC pipes with the caliber of more than or equal to 315mm are few, and have poor comprehensive performance.
Because the large-caliber PVC pipe has large caliber and thicker wall thickness, the production line speed is slow, the thermal mechanical process of the melt is long, the thermal stability of a PVC pipe material system is insufficient, and PVC is easy to degrade in the processing process to influence the comprehensive performance of the pipe in the conventional production process. And because the melt strength of the large-caliber PVC pipe material system is insufficient and the plasticization degree is low, the wall thickness deviation of the produced large-caliber PVC pipe is large, and the mechanical property is reduced.
Chinese patent application CN107778700A discloses a production formula for improving plasticizing performance of a super-large-diameter PVC-U pipe, which comprises 100 parts of PVC resin, 3-8 parts of ultrafine calcium carbonate, 2-5 parts of calcium-zinc stabilizer, 0.5-3 parts of organic tin stabilizer and 0.5-3 parts of epoxidized soybean oil. However, the conventional calcium-zinc heat stabilizer is usually composed of calcium salt and zinc salt, but zinc salt is very easy to cause zinc burning in the processing process, so that the PVC material is degraded, the thermal stability of the calcium-zinc heat stabilizer is limited, the precipitation condition is serious in processing and heating, and the comparative document does not specifically disclose the plasticizing performance of the large-caliber PVC pipe. Chinese patent application CN104149354A discloses a production device and a process for a large-caliber bidirectional stretching PVC pipe, wherein a specific stretching and expanding forming device is adopted to perform annular expansion and axial stretching on the PVC pipe, so that the mechanical property of the large-caliber PVC pipe is improved. However, the PVC pipe disclosed in the prior art has complex production process, many steps, high cost, and need of using special equipment and process, and is not suitable for traditional PVC pipe manufacturers.
Therefore, it is required to develop a large-diameter PVC pipe material having good thermal stability and good plasticizing property.
Disclosure of Invention
In order to overcome the defects of poor plasticizing performance and poor thermal stability of the large-caliber PVC pipe material in the prior art, the invention provides the large-caliber PVC pipe material, the thermal stability of the material is improved by the calcium-zinc composite heat stabilizer, the plasticizing performance of the material is improved by the butyl acrylate-methyl methacrylate copolymer, the plasticization is promoted by the styrene-acrylonitrile copolymer in a synergistic manner, the melt strength of the system is enhanced, and the flow performance is increased, so that the prepared large-caliber PVC pipe material has excellent thermal stability and plasticizing performance, high melt strength, and uniform wall thickness and excellent mechanical performance of the PVC pipe material.
The invention also aims to provide a preparation method of the large-caliber PVC pipe material.
The invention also aims to provide application of the large-caliber PVC pipe material in preparation of a large-caliber PVC pipe material.
In order to solve the technical problems, the invention adopts the technical scheme that:
a large-caliber PVC pipe material comprises the following components in parts by weight:
100 parts of polyvinyl chloride (PVC),
5-30 parts of calcium carbonate,
8-15 parts of a calcium-zinc composite heat stabilizer,
1-3 parts of styrene-acrylonitrile copolymer,
1-3 parts of butyl acrylate-methyl methacrylate copolymer,
1-3 parts of titanium dioxide,
5 to 10 parts of an impact modifier,
the calcium-zinc composite heat stabilizer is a mixture of calcium stearate, zinc stearate, silane coupling agent modified fumed silica and hydroxyl-terminated pentaerythritol adipate.
The calcium-zinc composite heat stabilizer not only comprises calcium stearate and zinc stearate salt, but also is compounded with silane coupling agent modified fumed silica and hydroxyl-terminated pentaerythritol adipate, so that PVC degradation caused by zinc burning can be effectively avoided, the thermal stability time of a PVC material system is greatly prolonged, the melt plasticizing retention time can be further prolonged, and the plasticizing degree and the plasticizing uniformity of the PVC material system are improved. The hydroxyl-terminated pentaerythritol adipate has good compatibility with PVC, and the existence of the hydroxyl-terminated group enables oxygen atoms in the hydroxyl groups to promote zinc chloride generated by complexing zinc salts in the calcium-zinc heat stabilizer, so that the synergistic effect of the calcium-zinc heat stabilizer on the thermal stability of PVC is further improved. The silane coupling agent modified fumed silica has higher surface polarity, can quickly adsorb HCl degraded and removed by PVC, and is not easy to desorb, so that the autocatalytic degradation of PVC molecules by HCl is blocked.
The inventor researches and discovers that for a large-caliber PVC pipe, the requirement of actual production on plasticizing performance cannot be met only by improving the thermal stability of the material through the calcium-zinc composite heat stabilizer, and a synergistic effect of a styrene-acrylonitrile copolymer and a butyl acrylate-methyl methacrylate copolymer is also needed.
The butyl acrylate-methyl methacrylate copolymer can effectively improve the plasticizing performance of the material in the PVC system, and the styrene-acrylonitrile copolymer (SAN) not only synergistically promotes the plasticizing, but also can enhance the melt strength of the system and increase the flowing performance. The synergistic interaction of the styrene-acrylonitrile copolymer, the butyl acrylate-methyl methacrylate copolymer and the calcium-zinc composite heat stabilizer ensures the melt flowability and the processability of the PVC material system, and when a large-caliber PVC pipe is prepared, the material can keep good thermal stability under a longer melt thermal mechanical process, so that the mechanical property reduction caused by material degradation or component precipitation is avoided, the melt strength is improved, the plasticizing degree is high, the wall thickness of the PVC pipe is more uniform, and the comprehensive performance is excellent.
Preferably, the weight average molecular weight of the styrene-acrylonitrile copolymer is 100 to 120 ten thousand.
Preferably, the styrene-acrylonitrile copolymer contains 35-45 wt% of styrene comonomer and 55-65 wt% of acrylonitrile comonomer.
Preferably, the weight average molecular weight of the butyl acrylate-methyl methacrylate copolymer is 120-150 ten thousand.
Preferably, the butyl acrylate-methyl methacrylate copolymer has 25-35 wt.% of butyl acrylate comonomer and 65-75 wt.% of methyl methacrylate comonomer.
The ACR processing aid commonly used in PVC pipe materials is an acrylate copolymer, which is a high polymer with a core-shell structure and is generated by emulsion polymerization of methyl methacrylate serving as a main comonomer, wherein the methyl methacrylate accounts for over 80 wt.% and is mixed with comonomers such as butyl methacrylate, ethyl methacrylate, butyl acrylate, ethyl acrylate and the like in different proportions according to performance requirements. The ACR processing aid can play a good role in plasticizing and synergizing in the PVC processing process, but due to the fact that the ACR processing aid is large in molecular weight and the weight average molecular weight is usually 150-200 ten thousand, the viscosity of a PVC material system is increased rapidly, the fluidity is reduced, and the processing is difficult.
Preferably, the mass ratio of the calcium stearate salt to the zinc stearate salt to the silane coupling agent modified fumed silica to the hydroxyl-terminated pentaerythritol adipate in the calcium-zinc composite heat stabilizer is (4-7): (3-5): (1-2): (0.5-0.8).
The hydroxyl-terminated adipic acid pentaerythritol ester is obtained by esterification reaction of hydroxyl-terminated adipic acid and pentaerythritol.
Preferably, the molar ratio of the hydroxyl-terminated adipic acid to the pentaerythritol is (1-1.5) to 2.
Preferably, the acid value of the hydroxyl-terminated pentaerythritol adipate is less than or equal to 0.5mg KOH/g, and the hydroxyl value is 70-90 mg KOH/g.
Preferably, the preparation method of the silane coupling agent modified fumed silica comprises the following steps:
dispersing the fumed silica and the silane coupling agent in an organic solvent, carrying out reflux reaction for 2-4 h at the temperature of 60-80 ℃, and carrying out post-treatment to obtain the silane coupling agent modified fumed silica.
Preferably, the mass ratio of the fumed silica to the silane coupling agent is (40-50): (20-30).
Preferably, the organic solvent is one or more of acetone, methanol, ethanol and ethyl acetate.
Preferably, the silane coupling agent is one or more of KH570, KH560 and KH 171.
Preferably, the impact modifier is Chlorinated Polyethylene (CPE) and/or methylmethacrylate-butadiene-styrene terpolymer (MBS)
The invention also provides a preparation method of the large-caliber PVC pipe material, which comprises the following steps:
mixing PVC, calcium carbonate, titanium dioxide, a calcium-zinc composite heat stabilizer, a styrene-acrylonitrile copolymer, a butyl acrylate-methyl methacrylate copolymer and an impact modifier, adding the mixture into an extruder, and performing melt blending and extrusion granulation to obtain the large-caliber PVC pipe material.
The invention also protects the application of the large-caliber PVC pipe material in the preparation of the large-caliber PVC pipe.
The caliber DN of the large-caliber PVC pipe is more than or equal to 315 mm.
The preparation method of the large-caliber PVC pipe comprises the following steps:
adding a large-caliber PVC pipe material into a double-screw extruder, and performing extrusion, molding and cutting to obtain the large-caliber PVC pipe material.
The process of the double-screw extruder comprises the following steps: the temperature of each zone of the conical double-screw extruder is 175 ℃, 160 ℃, 155 ℃ and 155 ℃, the temperature of each zone of the die head is 170 ℃, 165 ℃ and 205 ℃, and the temperature of the shaping cooling water is 25 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the invention develops a large-caliber PVC pipe material, the thermal stability of the material is improved through a calcium-zinc composite heat stabilizer, the plasticizing performance of a butyl acrylate-methyl methacrylate copolymer is improved, the plasticization is promoted by the styrene-acrylonitrile copolymer in a synergistic manner, the melt strength of a system can be enhanced, the flowing performance is increased, the prepared large-caliber PVC pipe material is excellent in thermal stability and plasticizing performance, the melt strength is high, and the prepared PVC pipe material with the caliber of more than or equal to 315mm is good in mechanical property.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The starting materials in the examples and comparative examples are all commercially available, wherein:
the silane coupling agent modified fumed silica is prepared by the following method:
dispersing the fumed silica and a silane coupling agent KH570 in acetone according to a mass ratio of 45:25, carrying out reflux heating reaction at a reaction temperature of 70 ℃ for 2h, separating and drying to obtain silane coupling agent modified fumed silica;
the hydroxyl-terminated pentaerythritol adipate is prepared by the following method:
under the action of a concentrated sulfuric acid catalyst, adding hydroxyl-terminated adipic acid and pentaerythritol into a round-bottom flask with a stirring device according to a molar ratio of 1:2, and carrying out esterification reaction under a vacuum condition, wherein the esterification reaction temperature is 150 ℃, and the reaction time is 4 hours, so as to obtain hydroxyl-terminated pentaerythritol adipate, the acid value of which is 0.2mgKOH/g, and the hydroxyl value of which is 90 mgKOH/g;
styrene-acrylonitrile copolymer a was purchased from japanese chemistry and has a weight average molecular weight of 100 ten thousand, with 35 wt.% styrene comonomer and 65 wt.% acrylonitrile comonomer;
styrene-acrylonitrile copolymer B was purchased from japanese chemistry with a weight average molecular weight of 120 ten thousand, with 45 wt.% styrene comonomer and 55 wt.% acrylonitrile comonomer;
butyl acrylate-methyl methacrylate copolymer a was purchased from japanese chemistry with a weight average molecular weight of 120 ten thousand, with 25 wt.% butyl acrylate comonomer and 75 wt.% methyl methacrylate comonomer;
butyl acrylate-methyl methacrylate copolymer B was purchased from japanese chemistry with a weight average molecular weight of 150 ten thousand, with 35 wt.% butyl acrylate comonomer and 65 wt.% methyl methacrylate comonomer;
ACR processing aids were purchased from national chemistry.
Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Examples 1 to 13
Examples 1 to 13 respectively provide a large-diameter PVC pipe material and a PVC pipe manufactured therefrom, wherein the contents of the components of the large-diameter PVC pipe material are shown in table 1,
the preparation method of the large-caliber PVC pipe material comprises the following steps: uniformly mixing the components according to the table 1, adding the mixture into a double-screw extruder, and carrying out melt blending and extrusion granulation to obtain a large-caliber PVC pipe material;
the preparation method of the PVC pipe comprises the following steps:
adding a large-caliber PVC pipe material into a double-screw extruder, and performing melt extrusion, mold forming, cooling and cutting to obtain the PVC pipe material with the DN caliber of 400 mm.
TABLE 1 component contents (parts by weight) of large-diameter PVC pipe materials of examples 1 to 8
Comparative examples 1 to 5
Comparative examples 1 to 5 respectively provide a PVC pipe material and a PVC pipe material prepared therefrom, the contents of the components of the PVC pipe material are shown in Table 2,
the preparation method of the PVC pipe material comprises the following steps: uniformly mixing the components according to the table 2, adding the mixture into a double-screw extruder, and carrying out melt blending and extrusion granulation to obtain a PVC pipe material;
the preparation method of the PVC pipe comprises the following steps:
adding a PVC pipe material into a double-screw extruder, and performing melt extrusion, mold forming, cooling and cutting to obtain the PVC pipe with the DN diameter of 400 mm.
TABLE 2 component contents (parts by weight) of PVC pipe materials of comparative examples 1 to 5
Performance testing
The PVC pipe material and the PVC pipe material prepared in the above examples and comparative examples are subjected to performance tests, and the test methods are as follows:
thermal stability performance: performing dynamic thermal stability test on each material formula system by using a torque rheometer, sampling every 5min, and performing color test until the color changes, wherein the length of thermal stability time represents the thermal stability of the material system;
wall thickness deviation: the wall thickness deviation is [ (maximum wall thickness-minimum wall thickness)/nominal wall thickness ] × 100%, the nominal wall thickness refers to GB/T10002.1-2006, the maximum wall thickness and the minimum wall thickness are 20 points randomly tested along the circumference of the pipe wall, and the maximum value and the minimum value are respectively taken;
tensile yield strength: the test method is determined according to GB/T8804.2-2003;
breakage rate of drop hammer impact test: the test method is determined according to GB/T14152-2001, and the breakage rate is (number of broken samples/total number of samples) × 100%.
The test results of examples and comparative examples are shown in tables 3 and 4.
TABLE 3 test results of examples 1 to 8
TABLE 4 test results for comparative examples 1 to 5
As can be seen from the test results in Table 3, the large-caliber PVC pipe material system prepared in each embodiment of the invention has excellent thermal stability, the dynamic thermal stability time is more than or equal to 35min, and the requirement of long thermal mechanical process in the production of the large-caliber PVC pipe material can be met; and the plasticizing performance is excellent, so that the wall thickness deviation of the prepared large-caliber PVC pipe is less than or equal to 1.5 percent, the wall thickness is uniform, and the mechanical property is excellent.
According to the test results in table 4, in comparative example 1, under the condition of not adding modified fumed silica and hydroxyl-terminated pentaerythritol adipate, the thermal stability of the PVC material system is poor, and PVC can be degraded in the processing process, so that the mechanical property of the PVC pipe is reduced. Compared with the comparative examples 2 and 3, when the butyl acrylate-methyl methacrylate copolymer processing aid or the styrene-acrylonitrile copolymer processing aid is used alone, the requirements for improving the melt plasticizing performance and the flow performance cannot be met simultaneously, so that the wall thickness deviation of the PVC pipe is large, and the mechanical property is reduced. In comparative example 4, the ACR processing aid is used, and the tensile yield strength of the PVC pipe is only 42 MPa. In comparative example 5, the amount of processing aid used was small, resulting in a decrease in the overall performance of the PVC pipe.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The large-caliber PVC pipe material is characterized by comprising the following components in parts by weight:
100 parts of PVC, 5-30 parts of calcium carbonate, 8-15 parts of a calcium-zinc composite heat stabilizer, 1-3 parts of a styrene-acrylonitrile copolymer, 1-3 parts of a butyl acrylate-methyl methacrylate copolymer, 1-3 parts of titanium dioxide and 5-10 parts of an impact modifier, wherein the calcium-zinc composite heat stabilizer is a mixture of calcium stearate, zinc stearate, silane coupling agent modified fumed silica and pentaerythritol terminated hydroxyadipate.
2. The large-caliber PVC pipe material according to claim 1, wherein the weight average molecular weight of the styrene-acrylonitrile copolymer is 100-120 ten thousand.
3. A large bore PVC pipe material according to claim 1 or 2, wherein the styrene-acrylonitrile copolymer has 35-45 wt.% styrene comonomer and 55-65 wt.% acrylonitrile comonomer.
4. The large-caliber PVC pipe material according to claim 1, wherein the weight-average molecular weight of the butyl acrylate-methyl methacrylate copolymer is 120-150 ten thousand.
5. A large caliber PVC pipe material according to claim 1 or 4, wherein the butyl acrylate-methyl methacrylate copolymer has 25-35 wt.% butyl acrylate comonomer and 65-75 wt.% methyl methacrylate comonomer.
6. The large-caliber PVC pipe material according to claim 1, wherein the mass ratio of calcium stearate, zinc stearate, silane coupling agent modified fumed silica and hydroxyl-terminated pentaerythritol adipate in the calcium-zinc composite heat stabilizer is (4-7): (3-5): (1-2): (0.5-0.8).
7. A preparation method of a large-caliber PVC pipe material according to any one of claims 1 to 6, characterized by comprising the following steps:
mixing PVC, calcium carbonate, titanium dioxide, a calcium-zinc composite heat stabilizer, a styrene-acrylonitrile copolymer, a butyl acrylate-methyl methacrylate copolymer and an impact modifier, adding the mixture into an extruder, and performing melt blending and extrusion granulation to obtain the large-caliber PVC pipe material.
8. Use of a large caliber PVC pipe material according to any one of claims 1 to 6 for the preparation of a large caliber PVC pipe.
9. The application of claim 8, wherein the caliber DN of the large-caliber PVC pipe is more than or equal to 315 mm.
10. The application of claim 8, wherein the preparation method of the large-caliber PVC pipe comprises the following steps:
the large-caliber PVC pipe material as claimed in any one of claims 1 to 6 is added into a double-screw extruder, and is subjected to extrusion, forming and cutting to obtain the large-caliber PVC pipe.
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| CN114854144A (en) * | 2022-04-26 | 2022-08-05 | 海南联塑科技实业有限公司 | Large-diameter PVC-U pipe and preparation method thereof |
| 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 |
| CN116178792B (en) * | 2022-12-05 | 2023-11-28 | 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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Application publication date: 20211224 |