CN114181446B - Polymer waterproof sheet, preparation method thereof and polymer waterproof coiled material - Google Patents
Polymer waterproof sheet, preparation method thereof and polymer waterproof coiled material Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/06—Polyethene
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08J2471/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
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Abstract
The application relates to the technical field of waterproof coiled materials, and particularly discloses a high-molecular waterproof sheet, a preparation method thereof and a high-molecular waterproof coiled material. The high-molecular waterproof sheet comprises high-density polyethylene, thermoplastic plastics, thermoplastic elastomers, coupling agents, compatilizers, anti-aging agents, flame retardants, fillers, white oil and polymers containing phenolic hydroxyl groups. The preparation method comprises the following steps: (1) Firstly, uniformly mixing a coupling agent and a filler, then adding a polymer containing phenolic hydroxyl groups, uniformly mixing, finally adding a compatilizer, an anti-aging agent, a flame retardant and white oil, and uniformly mixing to obtain powder; (2) Uniformly mixing high-density polyethylene, thermoplastic plastics and thermoplastic elastomer to obtain granules; (3) And (3) performing blending extrusion molding, cooling and shaping on the powder and the granules to obtain the macromolecular waterproof sheet. The polymer waterproof roll comprises the polymer waterproof sheet. This application has improved the waterproof sheet rigidity of polymer under the prerequisite of guaranteeing the pliability of waterproof sheet of polymer.
Description
Technical Field
The application relates to the technical field of waterproof rolls, in particular to a high-polymer waterproof sheet, a preparation method thereof and a high-polymer waterproof roll.
Background
High Density Polyethylene (HDPE) is one of the most common polyethylenes, has the characteristics of high crystallinity, non-polarity and the like, and is widely applied. In recent years, with the development of polymer self-adhesive film waterproof rolls, self-adhesive film waterproof rolls using HDPE as a main material have been rapidly developed. The high-molecular self-adhesive film waterproof roll is mainly made of HDPE (high-density polyethylene) serving as a main material, a self-adhesive reaction layer with a certain thickness is coated on the surface of the HDPE, and an isolating film is coated on the surface of the HDPE to form the waterproof roll. However, HDPE has high rigidity and poor impact resistance, and a single HDPE material is difficult to meet the performance requirements of the building waterproof coiled material in practical application, so the HDPE material needs to be toughened and modified.
The most important method for toughening the polymer is to add an elastomer into the polymer and prepare the elastomer into a polymer/elastomer or polymer/elastomer/filler multiphase composite material. However, elastomers generally used as toughening agents are low-modulus, low-strength materials, and their addition in large amounts leads to a decrease in the rigidity of the materials.
Disclosure of Invention
In order to improve the rigidity of a high-molecular waterproof sheet on the premise of ensuring the flexibility of the high-molecular waterproof sheet, the application provides the high-molecular waterproof sheet, a preparation method thereof and a high-molecular waterproof coiled material.
In a first aspect, the present application provides a waterproof polymer sheet, which adopts the following technical scheme:
a high-molecular waterproof sheet comprises the following raw materials in parts by weight: 30 to 70 parts of high-density polyethylene, 10 to 20 parts of thermoplastic plastics, 10 to 20 parts of thermoplastic elastomer, 0.01 to 0.5 part of coupling agent, 1 to 5 parts of compatilizer, 0.01 to 0.5 part of anti-aging agent, 1 to 5 parts of flame retardant, 5 to 10 parts of filler and 0 to 10 parts of white oil, wherein the polymer contains phenolic hydroxyl groups;
wherein the polymer containing phenolic hydroxyl is obtained by polymerization reaction of cardanol, hydroquinone and formaldehyde under an acid catalyst; 7-9 parts of cardanol, 1-3 parts of hydroquinone, 2-4 parts of formaldehyde and 0.01-0.1 part of acid catalyst.
Optionally, the thermoplastic is selected from the group consisting of low density polyethylene, ultra low density polyethylene, and ethylene vinyl acetate.
Optionally, the thermoplastic elastomer is a polyethylene octene co-elastomer. The polyethylene octene co-elastomer is metallocene polyolefin, has good elasticity, can increase the flexibility of high-density polyethylene, and ensures the molding of the hydrophobic groove of the high-molecular waterproof sheet in the molding processing process.
Optionally, the coupling agent is selected from titanate coupling agents and silane coupling agents. Preferably, the coupling agent is a titanate coupling agent.
Optionally, the compatibilizer is selected from the group consisting of maleic anhydride grafted polyethylene wax, high density oxidized polyethylene wax, and AClyn low relative molecular mass ionomer.
Optionally, the aging inhibitor is selected from the group consisting of antioxidants (e.g., antioxidant B215) and light stabilizers. Preferably, the anti-ageing agent is an antioxidant, such as: antioxidant B215.
Optionally, the flame retardant is selected from inorganic flame retardants and organic flame retardants.
Optionally, the filler is selected from talc and light calcium. Preferably, the filler is talc, for example: 600-1000 meshes of talcum powder.
Optionally, the acidic catalyst is selected from oxalic acid, hydrochloric acid and sulfuric acid. Preferably, the acidic catalyst is oxalic acid.
Optionally, the reaction temperature of the polymerization reaction is 90-100 ℃. Preferably, the reaction temperature of the polymerization reaction is 95 ℃.
Optionally, the weight average molecular weight of the polymer containing phenolic hydroxyl groups is 5000-10000. Preferably, the weight average molecular weight of the phenolic hydroxyl group-containing polymer is 6000 to 9000. More preferably, the weight average molecular weight of the phenolic hydroxyl group-containing polymer is 7500 to 8000.
Optionally, the formaldehyde is prepared into a formaldehyde aqueous solution with a weight percentage concentration of 30-50 wt% by using distilled water, for example: 40 percent by weight concentration of formaldehyde aqueous solution.
Optionally, the polymer waterproof sheet may be a planar sheet with the same thickness, or the polymer waterproof sheet is provided with a plurality of hydrophobic grooves arranged along the width direction of the polymer waterproof sheet.
Optionally, the thickness of the polymer waterproof sheet is 0.8-1.8 mm.
In a second aspect, the present application provides a method for preparing a polymer waterproof sheet, which adopts the following technical scheme:
a preparation method of a high-molecular waterproof sheet comprises the following steps:
(1) Firstly, uniformly mixing a coupling agent and a filler, then adding a polymer containing phenolic hydroxyl groups, uniformly mixing, finally adding a compatilizer, an anti-aging agent, a flame retardant and white oil, and uniformly mixing to obtain powder;
(2) Uniformly mixing high-density polyethylene, thermoplastic plastics and thermoplastic elastomer to obtain granules;
(3) And (3) performing blending extrusion molding, cooling and shaping on the powder and the granules to obtain the macromolecular waterproof sheet.
In a third aspect, the present application provides a polymer waterproof roll, which adopts the following technical scheme:
a macromolecule waterproof coiled material comprises the macromolecule waterproof sheet.
Optionally, the polymer waterproof roll further comprises an adhesive layer and an isolation layer.
Optionally, the thickness of the adhesive layer is 0.25 to 0.50mm.
Optionally, the material of the bonding layer may be an adhesive resin, such as: adhesive resin KT-YH1.
Optionally, the isolation layer may be a release film or a gravel layer.
In summary, the present application has the following beneficial effects:
firstly, the flexibility of the high-density polyethylene is improved by adopting thermoplastic plastics (low-density polyethylene, ultra-low-density polyethylene and ethylene-vinyl acetate copolymer) so as to ensure the molding processing of the high-molecular waterproof sheet.
Secondly, the rigidity of the high-molecular waterproof sheet can be improved by adding the polymer containing phenolic hydroxyl provided by the application, and the flexibility of the high-molecular waterproof sheet is further improved.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation of Polymer containing phenolic hydroxyl group
Preparation examples 1 to 3 and preparation comparative examples 1 to 4
TABLE 1 compounding tables of preparation examples 1 to 3 and preparation comparative examples 1 to 4 of polymers containing phenolic hydroxyl groups
The concrete preparation methods of the polymers containing a phenolic hydroxyl group of preparation examples 1 to 3 and preparation comparative examples 1 to 4 include the steps of: firstly, adding cardanol, hydroquinone, resorcinol, catechol and oxalic acid into a reaction kettle under the condition of stirring, and then heating to 95 ℃; then dripping 40 percent formaldehyde water solution within 1 hour, continuing the heat preservation reaction after finishing dripping until the weight average molecular weight of the polymer containing phenolic hydroxyl reaches 7500, stopping heating and cooling to room temperature, then using 500mL of distilled water at 50-60 ℃ to soak and wash for 30 minutes, repeating the soaking and washing for 10 times, and drying to obtain the cardanol-based polymer.
Examples of Polymer Water-repellent sheets
The raw material sources in the preparation of the polymer waterproof sheet are shown in table 2.
TABLE 2 sources of raw materials
Wherein the density of the high-density polyethylene 5000S is 0.948-0.954 g/cm 3 The melt index MI @190 ℃ is 0.9g/10min under 2.16 kg;
the density of the low density polyethylene 2420F is 0.923g/cm 3 The melt index MI @190 ℃ is 0.8g/10min under 2.16 kg;
the density of the ultra-low density polyethylene is 0.900g/cm 3 The melt index MI @190 ℃ is 0.7g/10min at 2.16 kg;
the melt index MI @190 ℃ of the ethylene-vinyl acetate copolymer 6110M is 5.6-6.4 g/10min at 2.16kg, and the content of vinyl acetate is 25.6-28.4 wt%;
polyethylene octene co-elastomer 8480 having a density of 0.860g/cm 3 And a melt index MI @190 ℃ of 1.2g/10min at 2.16 kg.
The polymer waterproof sheet of this application can be for the plane sheet of thickness such as, perhaps be provided with a plurality of hydrophobic recesses that are provided with along its width direction on the polymer waterproof sheet. The following embodiments are described by taking the polymer waterproof sheet as a planar sheet with equal thickness.
Preparation of high-molecular waterproof sheet
The preparation method of the polymer waterproof sheet specifically comprises the following steps:
(1) Firstly, uniformly mixing a coupling agent and a filler, then adding a polymer containing phenolic hydroxyl groups, uniformly mixing, finally adding a compatilizer, an anti-aging agent, a flame retardant and white oil, uniformly mixing, and heating to obtain powder at 105-110 ℃;
(2) Uniformly mixing high-density polyethylene, thermoplastic plastics and thermoplastic elastomer, and heating to obtain granules at 105-110 ℃;
(3) And (3) mixing and extruding the powder at the temperature of 105-110 ℃ and the granules at the temperature of 105-110 ℃ (a single-screw extruder, the extrusion temperature is set to be 190 ℃, the rotation speed is set to be 200 rpm), and cooling and shaping to obtain the macromolecular waterproof sheet with the thickness of 1 mm.
Performance test of waterproof polymer sheet
Tensile property: according to GB/T328.9-2007 test method for waterproof coiled materials for buildings, part 9: and (3) detecting by using a method A in the Polymer waterproof sheet tensile property.
Heat resistance: according to GB/T328.11-2007 test method for waterproof roll for building part 11: and (4) detecting by using a method B in asphalt waterproof coiled material heat resistance.
Low-temperature bendability: according to GB/T328.15-2007 test method for waterproof coiled materials for buildings part 15: and (4) detecting the low-temperature bending property of the asphalt waterproof coiled material.
Tear performance: according to GB/T328.18-2007 test method part 19 of waterproof roll materials for buildings: testing tearing performance (nail-rod method) of asphalt waterproof coiled materials.
Hardness: the measurement is carried out according to GB/T2411-2008 "hardness of plastic and hard rubber measured by using a durometer in indentation hardness (Shore hardness)".
Examples 1 to 5 and comparative example 1
The formulation of the polymer waterproof sheets of examples 1 to 5 and comparative example 1 is shown in table 3, and the performance test results of the polymer waterproof sheets of examples 1 to 5 and comparative example 1 are shown in table 4.
TABLE 3 formulation of Polymer Water-repellent sheets of examples 1 to 5 and comparative example 1
Table 4 results of testing the properties of the polymeric water repellent sheets of examples 1 to 5 and comparative example 1
As can be seen from table 4, the addition of the thermoplastic plastic and the thermoplastic elastomer can improve the tensile property, the low-temperature bending property and the tear resistance of the polymer waterproof sheet, and reduce the hardness of the polymer waterproof sheet.
The crystallinity of the thermoplastic plastics (low density polyethylene, ultra-low density polyethylene and ethylene-vinyl acetate copolymer) and the thermoplastic elastomer (polyethylene octene co-elastomer) is low, so that the flexibility of the high-molecular waterproof sheet is improved, and the molding processing of the high-molecular waterproof sheet is ensured; however, the hardness of the polymer waterproof sheet is reduced.
Examples 6 to 10 and comparative examples 4 to 7
Examples 6 to 10 and comparative examples 4 to 7: compared with example 2, examples 6 to 10 and comparative examples 4 to 7 differ only in that a polymer containing a phenolic hydroxyl group is further added. The source and the amount of the polymer having phenolic hydroxyl groups in the waterproof polymer sheets of examples 6 to 10 and comparative examples 4 to 7 are shown in table 5, and the performance test results of the waterproof polymer sheets of examples 6 to 10 and comparative examples 4 to 7 are shown in table 6.
TABLE 5 Source and amount of phenolic hydroxyl group-containing Polymer in examples 6 to 10 and comparative examples 4 to 7 of Polymer waterproofing sheets
| Polymers containing phenolic hydroxyl groups | Source | Dosage of |
| Example 6 | Preparation example 1 | 8kg |
| Example 7 | Preparation example 2 | 5kg |
| Example 8 | Preparation example 2 | 8kg |
| Example 9 | Preparation example 2 | 10kg |
| Example 10 | Preparation example 3 | 8kg |
| Comparative example 4 | Preparation of comparative example 1 | 8kg |
| Comparative example 5 | Preparation of comparative example 2 | 8kg |
| Comparative example 6 | Preparation of comparative example 3 | 8kg |
| Comparative example 7 | Preparation of comparative example 4 | 8kg |
TABLE 6 results of testing the properties of the polymeric water-repellent sheets of examples 6 to 10 and comparative examples 4 to 7
As can be seen from tables 4 and 6, the tensile property, tear resistance and hardness of the polymeric waterproof sheet can be further improved by adding the phenolic hydroxyl group-containing polymer provided by the present application. The polymer containing phenolic hydroxyl can be subjected to coupling reaction with a titanate coupling agent through carbon-carbon double bonds and phenolic hydroxyl contained in the polymer, and the alkyl long chain of cardanol is inserted into the high-molecular waterproof sheet, so that the polymer containing phenolic hydroxyl is prevented from migrating in the high-molecular waterproof sheet; the long alkyl chain contained in the polymer containing phenolic hydroxyl can further improve the tensile property and the tearing property of the high-molecular waterproof sheet; benzene rings contained in the polymer containing phenolic hydroxyl groups can improve the hardness of the high-molecular waterproof sheet, so that the problem of deformation of the high-molecular waterproof sheet in the using process is solved.
Comparing example 8 with comparative examples 4 to 5, it can be seen that the tensile property, tear resistance and hardness of example 8 are significantly better than those of comparative examples 4 to 5, and thus it can be seen that the tensile property, tear resistance and hardness of the polymer waterproof sheet are improved by the synergistic cooperation of cardanol and hydroquinone in the polymer containing phenolic hydroxyl groups.
It is understood by comparing example 8 with comparative examples 6 to 7 that the tensile property, tear property and hardness of example 8 are significantly superior to those of comparative examples 6 to 7, and thus it is understood that the presence of catechol and resorcinol in the polymer containing phenolic hydroxyl groups reduces the tensile property, tear property and hardness of the polymer waterproof sheet. The reason for this is that catechol, resorcinol, and hydroquinone have different active sites, which may affect the network structure formed by the polymer containing phenolic hydroxyl group in the polymer waterproof sheet, and further affect the tensile property, tearing property, hardness, and other properties of the polymer waterproof sheet.
In view of the above analysis, the polymeric waterproofing sheet of the present application is provided with a plurality of hydrophobic grooves arranged along the width direction thereof, and the polymeric waterproofing sheet of the present application also has excellent flexibility and rigidity.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. The polymer waterproof sheet is characterized by comprising the following raw materials in parts by weight: 30 to 70 parts of high-density polyethylene, 10 to 20 parts of thermoplastic plastics, 10 to 20 parts of thermoplastic elastomer, 0.01 to 0.5 part of coupling agent, 1 to 5 parts of compatilizer, 0.01 to 0.5 part of age resister, 1 to 5 parts of flame retardant, 5 to 10 parts of filler, 0 to 10 parts of white oil and 5 to 10 parts of polymer containing phenolic hydroxyl;
wherein the polymer containing phenolic hydroxyl is obtained by polymerization reaction of cardanol, hydroquinone and formaldehyde under an acid catalyst; 7-9 parts of cardanol, 1-3 parts of hydroquinone, 2-4 parts of formaldehyde and 0.01-0.1 part of acidic catalyst by weight;
the thermoplastic is selected from low density polyethylene, ultra-low density polyethylene and ethylene-vinyl acetate copolymer;
the thermoplastic elastomer is a polyethylene octene co-elastomer.
2. The polymeric waterproofing sheet according to claim 1, wherein the coupling agent is selected from titanate coupling agents and silane coupling agents.
3. The polymeric waterproofing sheet according to claim 1 wherein the compatibilizer is selected from the group consisting of maleic anhydride grafted polyethylene wax, high density oxidized polyethylene wax, and AClyn low relative molecular mass ionomer.
4. The polymeric water repellent sheet according to claim 1, wherein said acidic catalyst is selected from the group consisting of oxalic acid, hydrochloric acid and sulfuric acid.
5. The polymer waterproof sheet according to claim 1, wherein the reaction temperature of the polymerization reaction is 90 to 100 ℃.
6. The polymeric water repellent sheet according to claim 1, wherein said phenolic hydroxyl group-containing polymer has a weight average molecular weight of 5000 to 10000.
7. The method for preparing the polymer waterproof sheet according to any one of claims 1 to 6, comprising the steps of:
(1) Firstly, uniformly mixing a coupling agent and a filler, then adding a polymer containing phenolic hydroxyl, uniformly mixing, and finally adding a compatilizer, an anti-aging agent, a flame retardant and white oil, and uniformly mixing to obtain powder;
(2) Uniformly mixing high-density polyethylene, thermoplastic plastics and thermoplastic elastomer to obtain granules;
(3) And (3) performing blending extrusion molding, cooling and shaping on the powder and the granules to obtain the macromolecular waterproof sheet.
8. A waterproof roll of polymer material, comprising the waterproof sheet according to any one of claims 1 to 6.
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| CN115707752A (en) * | 2022-07-21 | 2023-02-21 | 北新禹王防水科技集团有限公司 | Pre-laid high-polymer waterproof roll with permeation crystallization function and preparation method thereof |
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