CN115782327A - Upper surface layer, double-layer composite ethylene propylene diene monomer waterproof roll and preparation method and application thereof - Google Patents
Upper surface layer, double-layer composite ethylene propylene diene monomer waterproof roll and preparation method and application thereof Download PDFInfo
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- CN115782327A CN115782327A CN202211512070.6A CN202211512070A CN115782327A CN 115782327 A CN115782327 A CN 115782327A CN 202211512070 A CN202211512070 A CN 202211512070A CN 115782327 A CN115782327 A CN 115782327A
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- 239000002344 surface layer Substances 0.000 title claims abstract description 67
- 229920002943 EPDM rubber Polymers 0.000 title claims abstract description 52
- 239000010410 layer Substances 0.000 title claims abstract description 51
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 238000005096 rolling process Methods 0.000 title claims description 6
- 238000002360 preparation method Methods 0.000 title abstract description 49
- 239000000463 material Substances 0.000 claims abstract description 56
- -1 polypropylene Polymers 0.000 claims abstract description 42
- 239000004743 Polypropylene Substances 0.000 claims abstract description 38
- 229920001971 elastomer Polymers 0.000 claims abstract description 38
- 239000000806 elastomer Substances 0.000 claims abstract description 38
- 229920001155 polypropylene Polymers 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 239000004611 light stabiliser Substances 0.000 claims abstract description 24
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 22
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 15
- 238000004078 waterproofing Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims description 28
- 239000003921 oil Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 13
- 239000004712 Metallocene polyethylene (PE-MC) Substances 0.000 claims description 12
- 239000003963 antioxidant agent Substances 0.000 claims description 12
- 230000003078 antioxidant effect Effects 0.000 claims description 12
- 238000005469 granulation Methods 0.000 claims description 12
- 230000003179 granulation Effects 0.000 claims description 12
- 238000003490 calendering Methods 0.000 claims description 10
- 239000000049 pigment Substances 0.000 claims description 10
- 229920002397 thermoplastic olefin Polymers 0.000 claims description 10
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 8
- 239000000155 melt Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 6
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 6
- 239000006229 carbon black Substances 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 4
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 3
- OUBMGJOQLXMSNT-UHFFFAOYSA-N N-isopropyl-N'-phenyl-p-phenylenediamine Chemical compound C1=CC(NC(C)C)=CC=C1NC1=CC=CC=C1 OUBMGJOQLXMSNT-UHFFFAOYSA-N 0.000 claims description 2
- 239000005662 Paraffin oil Substances 0.000 claims description 2
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000010692 aromatic oil Substances 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 239000003086 colorant Substances 0.000 claims description 2
- 229920001903 high density polyethylene Polymers 0.000 claims description 2
- 239000004700 high-density polyethylene Substances 0.000 claims description 2
- 229920001684 low density polyethylene Polymers 0.000 claims description 2
- 239000004702 low-density polyethylene Substances 0.000 claims description 2
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims 2
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- 238000010276 construction Methods 0.000 description 9
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- 238000005453 pelletization Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- ZRMMVODKVLXCBB-UHFFFAOYSA-N 1-n-cyclohexyl-4-n-phenylbenzene-1,4-diamine Chemical compound C1CCCCC1NC(C=C1)=CC=C1NC1=CC=CC=C1 ZRMMVODKVLXCBB-UHFFFAOYSA-N 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
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- 229920005549 butyl rubber Polymers 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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- 230000007774 longterm Effects 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention relates to the field of building waterproofing, and discloses an upper surface layer, a double-layer composite ethylene propylene diene monomer waterproof coiled material, and a preparation method and application thereof. The upper surface layer is formed by an ethylene propylene diene monomer waterproof layer, and the ethylene propylene diene monomer waterproof layer contains the following components: ethylene propylene diene monomer, polypropylene elastomer, TPO-g- (GMA-co-St), softening oil, reinforcing filler, vulcanizing agent, accelerator, anti-aging agent and light stabilizer. The waterproof coiled material provided by the invention can be welded, has the advantages of simple process, excellent physical properties, tight adhesion of a double-layer structure, good toughness, high strength and good weather resistance, and is suitable for the field of building waterproofing.
Description
Technical Field
The invention relates to the field of building waterproofing, in particular to an upper surface layer, a double-layer composite ethylene propylene diene monomer waterproof coiled material, and a preparation method and application thereof.
Background
The Ethylene Propylene Diene Monomer (EPDM) rubber waterproof coiled material is prepared by adding a proper amount of butyl rubber, a vulcanizing agent, an accelerant, a softening agent, a reinforcing agent and the like into EPDM rubber, and carrying out banburying, pulling sheet filtration, extrusion molding and other working procedures.
Ethylene propylene diene monomer is a high molecular polymer copolymerized from ethylene, propylene and non-conjugated diene, and has high chemical stability due to the characteristic of a saturated structure of a main chain.
The ethylene propylene diene monomer waterproof coiled material has good aging resistance and long service life. Because the main chain of the ethylene propylene diene monomer rubber molecular structure has no double bonds, when the ethylene propylene diene monomer rubber waterproof coiled material is subjected to the action of ozone, ultraviolet rays and damp heat, the main chain is not easy to break, so that the ethylene propylene diene monomer rubber waterproof coiled material has excellent weather resistance and aging resistance, and the service life can reach more than 50 years.
However, the existing ethylene propylene diene monomer waterproof coiled material body cannot be welded, a construction mode that solvent type glue is adopted for bonding the overlapping edges is adopted, the construction time is long, the construction process is complex, the reliability of bonding parts is not high, the bonding parts fail after long-term use, and water seepage and leakage occur.
Therefore, the weldability and the anti-seepage performance of the bonding part of the ethylene propylene diene monomer rubber waterproof coiled material are improved, the construction process is simplified, the construction time is shortened, and the method has important significance.
Disclosure of Invention
The invention aims to solve the problems that an ethylene propylene diene monomer waterproof coiled material in the prior art cannot be welded, the construction time is long, the construction process is complex, the bonding part is easy to lose efficacy, and water seepage and water leakage occur.
In order to achieve the above object, a first aspect of the present invention provides an upper surface layer applied in a waterproof roll, where the upper surface layer is formed by an epdm waterproof layer, and the epdm waterproof layer contains the following components: ethylene propylene diene monomer, polypropylene-based elastomer, TPO-g- (GMA-co-St), softening oil, reinforcing filler, vulcanizing agent, accelerator, anti-aging agent and light stabilizer;
in the upper surface layer, the total weight of the ethylene propylene diene monomer waterproof layer is 100 parts by weight, the content of the ethylene propylene diene monomer is 30-70 parts by weight, the content of the polypropylene-based elastomer is 40-80 parts by weight, the content of TPO-g- (GMA-co-St) is 1-10 parts by weight, the content of the softening oil is 2-10 parts by weight, the content of the reinforcing filler is 10-20 parts by weight, the content of the vulcanizing agent is 0.1-1 part by weight, the content of the accelerator is 0.1-1 part by weight, the content of the anti-aging agent is 1-4.5 parts by weight, and the content of the light stabilizer is 1-5 parts by weight.
The invention provides a double-layer composite ethylene propylene diene monomer rubber waterproof coiled material, which comprises an upper surface layer and a lower surface layer which are sequentially stacked;
the upper surface layer is the upper surface layer described in the first aspect, and
the lower surface layer is formed of a thermoplastic polyolefin elastomer waterproof layer, and
the ratio of the thickness of the thinnest part of the upper surface layer to the thickness of the thinnest part of the lower surface layer is 1:1-1.8.
The third aspect of the invention provides a method for preparing the double-layer composite ethylene propylene diene monomer rubber waterproof coiled material of the second aspect, which is carried out by applying the components of the waterproof coiled material of the second aspect, and comprises the following steps:
(1) Mixing and contacting: mixing ethylene propylene diene monomer, polypropylene-based elastomer, TPO-g- (GMA-co-St), softening oil, filler, anti-aging agent and light stabilizer to contact I to obtain premix 1;
mixing polypropylene-based elastomer, TPO-g- (GMA-co-St), metallocene polyethylene, filler, antioxidant and pigment to contact II to obtain premix 2;
(2) And (3) granulation: granulating the premix 1 to obtain a granulated material 1;
(3) Plasticizing and rolling: extruding and plasticizing the granulating material 1 and the premix 2, introducing into a three-roll calender for calendering to obtain the double-layer composite ethylene propylene diene monomer waterproof coiled material.
The fourth aspect of the invention provides an application of the double-layer composite ethylene propylene diene monomer waterproof coiled material in the third aspect in the field of building waterproofing.
The double-layer composite ethylene propylene diene monomer waterproof coiled material provided by the invention has the advantages of reliable welding performance, tight adhesion, good waterproofness and simple production process and construction process.
Drawings
Fig. 1 is a schematic structural diagram of a double-layer composite ethylene propylene diene monomer waterproof roll.
Description of the reference numerals
1: upper surface layer 2: lower surface layer
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For numerical ranges, each range between its endpoints and individual point values, and each individual point value can be combined with each other to give one or more new numerical ranges, and such numerical ranges should be construed as specifically disclosed herein.
It is to be noted that, in various aspects of the present invention, the present invention is described only once in one aspect thereof with respect to the same components or terms in the aspects without repeated descriptions, and those skilled in the art should not be construed as limiting the present invention.
As described above, in a first aspect of the present invention, an upper surface layer applied in a waterproof roll is provided, where the upper surface layer is formed by an epdm waterproof layer, and the epdm waterproof layer contains the following components: ethylene propylene diene monomer, polypropylene-based elastomer, TPO-g- (GMA-co-St), softening oil, reinforcing filler, vulcanizing agent, accelerator, anti-aging agent and light stabilizer;
in the upper surface layer, the total weight of the ethylene propylene diene monomer waterproof layer is 100 parts by weight, the content of the ethylene propylene diene monomer is 30-70 parts by weight, the content of the polypropylene-based elastomer is 40-80 parts by weight, the content of TPO-g- (GMA-co-St) is 1-10 parts by weight, the content of the softening oil is 2-10 parts by weight, the content of the reinforcing filler is 10-20 parts by weight, the content of the vulcanizing agent is 0.1-1 part by weight, the content of the accelerator is 0.1-1 part by weight, the content of the anti-aging agent is 1-4.5 parts by weight, and the content of the light stabilizer is 1-5 parts by weight.
According to a preferred embodiment, in the ethylene propylene diene monomer waterproof layer, the softening oil is at least one selected from naphthenic oil, paraffin oil and aromatic oil.
Preferably, the vulcanizing agent is at least one selected from sulfur and dicumyl peroxide.
Preferably, the accelerator is selected from at least one of accelerator DM, accelerator TMTD, accelerator BZ.
Preferably, the antioxidant is selected from at least one of antioxidant 4010NA, antioxidant 4010 and antioxidant RD.
Preferably, the polypropylene-based elastomer is selected from the group consisting of Riandbacel CA10A, riandbacel CA60A, and VERSIFY 2300.
Preferably, the reinforcing filler is selected from at least one of carbon black, white carbon, and calcium carbonate.
Preferably, the light stabilizer is at least one selected from the group consisting of a light stabilizer UV-2020, an ultraviolet absorber UV-326 and an ultraviolet absorber UV-531.
According to a preferred embodiment, said TPO-g- (GMA-co-St) is a product obtained by the following process:
s1, mixing raw materials for preparing TPO-g- (GMA-co-St) to obtain a mixture I;
s2, carrying out melt grafting on the mixture I at the temperature of 180-230 ℃ to obtain the TPO-g- (GMA-co-St), wherein the melt grafting time is 8-15min;
wherein, the raw materials for preparing TPO-g- (GMA-co-St) comprise: polypropylene-based elastomer, glycidyl methacrylate, styrene, dicumyl peroxide and antioxidant 1010.
According to a preferred embodiment, the method further comprises: the mixing at least satisfies: under the condition of stirring, the rotating speed is 300-800r/min, the temperature is 70-90 ℃, and the time is 8-15min.
It is to be noted that the present invention does not specifically require the apparatus for the mixing, and the mixing can be carried out by the conventional apparatus and means, for example, a high-speed mixer.
It should be noted that, in the present invention, the melt grafting equipment is not particularly required, and the melt grafting can be carried out by the conventional equipment and means, for example, a twin-screw extrusion granulator.
Preferably, in the raw material for preparing TPO-g- (GMA-co-St), the glycidyl methacrylate is used in an amount of 1 to 5 parts by weight, relative to 100 parts by weight of the polypropylene-based elastomer; the dosage of the styrene is 0.5 to 4 weight parts; the dosage of the dicumyl peroxide is 0.1 to 0.8 weight part; the antioxidant 1010 is used in an amount of 0.1 to 1 part by weight, wherein the polypropylene-based elastomer is the same as the polypropylene-based elastomer in the upper surface layer.
As described above, a second aspect of the present invention provides a double-layer composite ethylene propylene diene monomer waterproof roll, which includes an upper surface layer and a lower surface layer that are sequentially stacked;
the upper surface layer is the upper surface layer described in the first aspect, and
the lower surface layer is formed of a water-repellent layer of a thermoplastic polyolefin elastomer, and
the ratio of the thickness of the thinnest part of the upper surface layer to the thickness of the thinnest part of the lower surface layer is 1:1-1.8.
According to a preferred embodiment, the following provides a double-layer structure of the double-layer composite ethylene propylene diene monomer rubber waterproof coiled material, in particular to the following, with reference to fig. 1:
the lower surface layer 2 is provided with a groove structure, and the upper surface layer 1 is positioned in the groove structure of the lower surface layer 2; the double-layer structure is provided with a welding edge which is formed by the thermoplastic polyolefin elastomer waterproof layer in the lower surface layer 2. The inventors found that the physical properties of the waterproof roll prepared in this preferred case are more excellent.
According to a preferred embodiment, in the thermoplastic polyolefin elastomer waterproofing layer, the following components are contained: TPO-g- (GMA-co-St), polypropylene-based elastomer, metallocene polyethylene, reinforcing filler, antioxidant, light stabilizer, pigment, wherein in the lower surface layer, the TPO-g- (GMA-co-St) is the same as the TPO-g- (GMA-co-St) in the upper surface layer described in the first aspect.
Preferably, in the thermoplastic polyolefin elastomer waterproof layer, the TPO-g- (GMA-co-St) content is 1 to 10 parts by weight, the metallocene polyethylene content is 10 to 40 parts by weight, the reinforcing filler content is 10 to 30 parts by weight, the antioxidant content is 0.1 to 1 part by weight, the light stabilizer content is 1 to 5 parts by weight, and the pigment content is 0.5 to 2 parts by weight, with respect to 100 parts by weight of the polypropylene-based elastomer, the reinforcing filler, and the light stabilizer being the same as the polypropylene-based elastomer, the reinforcing filler, and the light stabilizer of the first aspect, respectively.
Preferably, in the thermoplastic polyolefin elastomer waterproof layer, the antioxidant is at least one selected from the group consisting of antioxidant 1010, antioxidant 168 and antioxidant 1076.
Preferably, the pigment is selected from at least one of titanium dioxide, carbon black and a colorant.
Preferably, the metallocene polyethylene is at least one selected from metallocene high density polyethylene and metallocene low density polyethylene.
As described above, the third aspect of the present invention provides a method for preparing the double-layer composite ethylene propylene diene monomer rubber waterproof roll material of the second aspect, which is performed by using the components of the waterproof roll material of the second aspect, and comprises the following steps:
(1) Mixing and contacting: mixing ethylene propylene diene monomer, polypropylene-based elastomer, TPO-g- (GMA-co-St), softening oil, filler, anti-aging agent and light stabilizer to contact I to obtain premix 1;
mixing and contacting polypropylene-based elastomer, TPO-g- (GMA-co-St), metallocene polyethylene, a filler, an antioxidant and a pigment II to obtain a premix 2;
(2) And (3) granulation: granulating the premix 1 to obtain a granulated material 1;
(3) Plasticizing and rolling: extruding and plasticizing the granulating material 1 and the premix 2, introducing into a three-roll calender for calendering to obtain the double-layer composite ethylene propylene diene monomer waterproof coiled material.
In the present invention, the equipment for carrying out the mixing contact I is not particularly limited, and may be carried out by equipment commonly used in the art, for example, by using a high-speed kneader.
According to a preferred embodiment, in the process of the invention, said granulation in step (2) is carried out in a screw extruder.
According to a preferred embodiment, the method of the invention further comprises: before the material is introduced into a three-roll calender, firstly adopting two extruders to carry out extrusion plasticization, and specifically, introducing the granulating material 1 into the extruder 1 to carry out extrusion plasticization to obtain a material I; introducing the premix 2 into an extruder 2 for extrusion and plasticization to obtain a material II; and co-extruding the material I and the material II into a double-layer co-extrusion die for discharging to obtain a co-extrusion material to be applied to the three-roll calender for calendering.
According to a preferred embodiment, the method of the invention further comprises: before the pelletizing material 1 obtained in the step (2) is subjected to extrusion plasticization, dynamically vulcanizing the pelletizing material 1 by using a vulcanizing agent and an accelerator to obtain a vulcanized pelletizing material 1 to be applied to the extrusion plasticization.
It should be noted that the present invention has no specific requirements on the operating conditions of the granulation, extrusion plasticizing, dynamic vulcanization and calendering, and can be carried out by using the technical means and parameters commonly used in the art, and the following provides an exemplary operating condition, including:
the granulation and dynamic vulcanization conditions are as follows: under the condition of stirring, the rotating speed is 400-600rpm, and the temperature is 180-230 ℃;
the extrusion plasticizing conditions are as follows: under the condition of stirring, the temperature is 180-230 ℃, and the rotating speed is 200-500rpm;
the conditions of the calendering are as follows: the temperature is 30-70 ℃;
wherein, the temperature of the granulation and the dynamic vulcanization refers to the temperature of a die of a screw extruder.
According to a preferred embodiment, the mixing contact I is at least such that: under the condition of stirring, the rotating speed is 300-800r/min, the temperature is 70-90 ℃, and the time is 5-10min.
Preferably, said mixing contact II at least satisfies: under the condition of stirring, the rotating speed is 300-800r/min, the temperature is 70-90 ℃, and the time is 5-10min.
As mentioned above, the fourth aspect of the present invention provides the application of the double-layer composite ethylene propylene diene monomer waterproof roll material of the third aspect in the field of building waterproofing.
Compared with the prior art, the waterproof roll provided by the invention at least has the following advantages:
(1) The waterproof coiled material provided by the invention has the characteristics of simple production process, high production efficiency, excellent physical properties and simple and rapid construction.
(2) The double-layer structure of the waterproof coiled material provided by the invention is tightly bonded, has good waterproofness, and has the characteristics of low oil charge, good toughness, high strength, good weather resistance and weldability.
The present invention will be described in detail below by way of examples. In the following examples, the raw materials used are all common commercial products unless otherwise specified.
Some of the starting materials and sources used in the following examples are shown in table 1 below:
TABLE 1
A high-speed mixer: model number SHR-800A, available from Zhengxing mechanical Co., ltd;
a double-screw extrusion granulator: model JWE-75 available from gold weft machine manufacturing, inc.;
an extruder 1: model CJWH75-44D, available from jin Yuan machinery manufacturing Co., ltd;
an extruder 2: model CJWH95-44D, available from jin Yuan machinery manufacturing Co., ltd;
three-roller calender: model number 600 × 2400 from underwriters laboratories, inc.;
and (3) testing the physical properties of the waterproof roll: testing according to GB/T18173.1-2012 'sheet of part 1 of high molecular waterproof material' JL 1;
the seam peel strength of the waterproof coiled material is carried out according to 6.11 in GB 27789-2011.
Unless otherwise specified, the following examples represent 10g per part by weight.
Preparation example A-1
The raw material formula for preparing TPO-g- (GMA-co-St) in the preparation example is as follows:
this preparation example illustrates TPO-g- (GMA-co-St) prepared as follows:
s1, mixing raw materials for preparing TPO-g- (GMA-co-St) to obtain a mixture I;
wherein, in the step S1, the mixing is carried out under the condition of stirring, the rotating speed is 500r/min, the temperature is 85 ℃, and the time is 8min;
s2, carrying out melt grafting on the mixture I in a double-screw extrusion granulator at the temperature of 200 ℃ to obtain the TPO-g- (GMA-co-St), wherein the melt grafting time is 10min;
TPO-g- (GMA-co-St) was obtained and designated as T1.
Preparation example A-2
The formulation of the raw materials for preparing TPO-g- (GMA-co-St) in this preparation example was the same as that in preparation example A-1.
This preparation was carried out in a similar manner to preparation A-1, except that: in the present preparation example, the reaction mixture was,
the mixing time in the step S1 is 14min;
the temperature of the melt grafting in the step S2 is 220 ℃, and the time of the melt grafting is 15min;
TPO-g- (GMA-co-St) was obtained and designated as T2.
Preparation example B-1
This preparation example is intended to illustrate the preparation of premix 1 (i.e. the upper surface layer according to the invention).
Specifically, ethylene propylene diene monomer, polypropylene-based elastomer, TPO-g- (GMA-co-St) (T1), softening oil I, reinforcing filler, anti-aging agent, and light stabilizer were mixed in a high-speed mixer to contact I, as shown in Table 2.
Wherein, the mixing contact I is carried out under stirring, and the conditions of the mixing contact I are as follows: the rotation speed is 500rpm, the temperature is 85 ℃, and the time is 8min.
Preparation example B-2
This preparation example prepared premix 1 in a similar manner to preparation example B-1, except that:
in this preparation, the same parts by weight of softening oil II were used in place of softening oil I in preparation B-1 to carry out mixing contact I, and TPO-g- (GMA-co-St) used was T2, see Table 2 specifically;
Preparation example B-3
This preparation example prepared premix 1 in a similar manner to preparation example B-1, except that:
in this preparation, the same parts by weight of PP-g-MAH was used in place of TPO-g- (GMA-co-St) in preparation B-1 for mixed contact I, see Table 2;
Preparation example B-4
This preparation example prepared premix 1 in a similar manner to preparation example B-1, except that: mixing contact I was performed using PEg-MAH instead of TPO-g- (GMA-co-St), see in particular Table 2;
Preparation example B-5
This preparation example prepared premix 1 in a similar manner to preparation example B-1, except that: mixed contact I was carried out without addition of TPO-g- (GMA-co-St), see in particular table 2;
TABLE 2
Preparation example C-1
This preparation example is intended to illustrate the preparation of premix 2 (i.e., the lower surface layer according to the present invention).
Specifically, the preparation method comprises the following steps: mixing polypropylene-based elastomer, TPO-g- (GMA-co-St) (T1), metallocene polyethylene, reinforcing filler, antioxidant and pigment to contact II, specifically referring to Table 3, wherein the conditions of the mixing contact II are as follows: stirring at 500r/min and 85 deg.C for 8min;
Preparation example C-2
This preparation was carried out in a similar manner to preparation C-1, except that: mixing contact II with metallocene polyethylene II instead of metallocene polyethylene I and using TPO-g- (GMA-co-St) as T2, see Table 3 for details;
Preparation example C-3
This preparation was carried out in a similar manner to preparation C-1, except that: mixed contact II was performed using PP-g-MAH instead of TPO-g- (GMA-co-St), see in particular Table 3;
Preparation example C-4
This preparation was carried out in a similar manner to preparation C-1, except that: mixing contact II using PE-g-MAH instead of TPO-g- (GMA-co-St), see in particular Table 3;
Preparation example C-5
This preparation was carried out in a similar manner to preparation C-1, except that: mixed contact II without TPO-g- (GMA-co-St) addition, see table 3 for details;
TABLE 3
Example 1
This example is used to illustrate that the preparation of the double-layer composite ethylene propylene diene monomer waterproof roll provided by the present invention is performed according to the following parameters, and includes the following steps:
SS1, granulation:
adding the premix 1 into a screw extruder for granulation to obtain a granulation material 1;
SS2, dynamic vulcanization:
before the pelleting material 1 is extruded and plasticized, dynamically vulcanizing the pelleting material 1 by adopting a vulcanizing agent and an accelerant to obtain a vulcanized pelleting material 1 to be applied to extrusion and plasticization;
SS3, extrusion plasticizing:
extruding and plasticizing by adopting two extruders, specifically, introducing the granulating material 1 into the extruder 1 for extruding and plasticizing to obtain a material I; introducing the premix 2 into an extruder 2 for extrusion and plasticization to obtain a material II; co-extruding the material I and the material II into a double-layer co-extrusion die for discharging to obtain a co-extruded material to be applied to the three-roll calender for calendering;
SS4, rolling:
introducing the co-extruded material into a three-roll calender for calendering to obtain a double-layer composite ethylene propylene diene monomer waterproof roll;
wherein premix 1 used was premix 1-a in total parts by weight obtained by the method in production example B-1, and premix 2 was premix 2-a in total parts by weight obtained by the method in production example C-1;
the granulation and dynamic vulcanization conditions are as follows: under the condition of stirring, the rotating speed is 500rpm, and the temperature of a die of a screw extruder is 225 ℃;
the extrusion plasticizing conditions are as follows: under the condition of stirring, the temperature is 225 ℃, and the rotating speed is 365rpm;
the calendering conditions are as follows: the temperature is 45 ℃ for the upper roller, 45 ℃ for the middle roller and 45 ℃ for the lower roller;
the waterproof roll is named as P1, the thickness of the thinnest part of the upper surface layer is 0.5cm, and the thickness of the thinnest part of the lower surface layer is 0.7cm.
Example 1-a
This example was carried out in a similar manner to example 1 and under the same operating conditions, except that: the addition amount of the raw materials is changed:
wherein, in the process of preparing the premix 1-a, the addition amount of the polypropylene-based elastomer is 50 parts by weight;
in the process of preparing premix 2-a, the polypropylene-based elastomer was added in an amount of 80 parts by weight.
The waterproof roll is obtained and named as P1-a, the thickness of the thinnest part of the upper surface layer is 0.5cm, and the thickness of the thinnest part of the lower surface layer is 0.5cm.
Example 1 b
This example was carried out in a similar manner to example 1, except that: the addition amount of raw materials and the operation conditions are changed:
wherein, in the process of preparing the premix 1-a, the addition amount of the polypropylene-based elastomer is 60 parts by weight, the addition amount of TPO-g- (GMA-co-St) is 5 parts by weight, the addition amount of the reinforcing filler is 15 parts by weight, and the addition amount of the light stabilizer is 2 parts by weight;
in the process of preparing the premix 2-a, the addition amount of the polypropylene-based elastomer is 80 parts by weight, the addition amount of the polypropylene-based elastomer is 5 parts by weight, and the addition amount of the reinforcing filler is 15 parts by weight;
in the process of preparing the waterproof roll, the granulation and dynamic vulcanization conditions in the steps SS1 and SS2 are as follows: under the condition of stirring, the rotating speed is 500rpm, and the temperature of a die of a screw extruder is 200 ℃;
in step SS3, the extrusion plasticizing conditions are: under the condition of stirring, the temperature is 200 ℃, and the rotating speed is 450rpm;
in step SS4, the conditions of the calendering are: the temperature is 55 ℃ of the upper roller, 55 ℃ of the middle roller and 55 ℃ of the lower roller;
the waterproof roll is obtained and named as P1-b, the thickness of the thinnest part of the upper surface layer is 0.5cm, and the thickness of the thinnest part of the lower surface layer is 0.8cm.
Examples 1 to c
This example was carried out in a similar manner to example 1, except that: the addition amount of the raw materials is changed:
wherein, in the process of preparing the premix 1-a, the addition amount of the polypropylene-based elastomer is 70 parts by weight, the addition amount of TPO-g- (GMA-co-St) is 5 parts by weight, the addition amount of the reinforcing filler is 15 parts by weight, and the addition amount of the light stabilizer is 2 parts by weight;
in the process of preparing premix 2-a, the polypropylene-based elastomer is added in an amount of 100 parts by weight, the polypropylene-based elastomer is added in an amount of 5 parts by weight, and the reinforcing filler is added in an amount of 15 parts by weight.
The waterproof roll is obtained and named as P1-c, the thickness of the thinnest part of the upper surface layer is 0.5cm, and the thickness of the thinnest part of the lower surface layer is 0.6cm.
Example 2
This example was carried out in a similar manner to example 1, except that: the premix 1 is premix 1-b, and the premix 2 is premix 2-b;
the waterproof roll is named as P2, the thickness of the thinnest part of the upper surface layer is 0.5cm, and the thickness of the thinnest part of the lower surface layer is 0.9cm.
Comparative example 1
This comparative example was carried out in a similar manner to example 1, except that: premix 1 used was the total parts by weight of premix 1-C obtained by the method in production example B-3, and premix 2 was the total parts by weight of premix 2-C obtained by the method in production example C-3;
the waterproof roll was obtained, which was designated as DP1, and had an upper surface layer with a thinnest point of 0.5cm and a lower surface layer with a thinnest point of 0.7cm.
Comparative example 2
This comparative example was carried out in a similar manner to example 1, except that: premix 1 used was premix 1-d of the total parts by weight obtained by the method in production example B-4, and premix 2 was premix 2-d of the total parts by weight obtained by the method in production example C-4;
the waterproof roll was obtained, designated as DP2, with a thickness of 0.5cm at the thinnest point of the upper surface layer and 0.7cm at the thinnest point of the lower surface layer.
Comparative example 3
This comparative example was carried out in a similar manner to example 1, except that: premix 1 used was premix 1-e of the total parts by weight obtained by the method in production example B-5, and premix 2 was premix 2-e of the total parts by weight obtained by the method in production example C-5;
the waterproof roll was obtained, designated as DP3, with a thickness of 0.5cm at the thinnest point of the upper surface layer and 0.7cm at the thinnest point of the lower surface layer.
Test example 1
The waterproof roll prepared above was lapped by welding, and physical properties and seam peel strength were measured, and the results are shown in table 4.
TABLE 4
TABLE 4 continuation of the table
From the results, the waterproof coiled material provided by the invention can be welded, has the advantages of simple process, excellent physical properties, tight adhesion of a double-layer structure, good toughness, high strength and good weather resistance, and is suitable for the field of building waterproofing.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (11)
1. The upper surface layer applied to the waterproof coiled material is characterized in that the upper surface layer is formed by an ethylene propylene diene monomer waterproof layer, and the ethylene propylene diene monomer waterproof layer contains the following components: ethylene propylene diene monomer, polypropylene-based elastomer, TPO-g- (GMA-co-St), softening oil, reinforcing filler, vulcanizing agent, accelerator, anti-aging agent and light stabilizer;
in the upper surface layer, the total weight of the ethylene propylene diene monomer waterproof layer is 100 parts by weight, the content of the ethylene propylene diene monomer is 30-70 parts by weight, the content of the polypropylene-based elastomer is 40-80 parts by weight, the content of TPO-g- (GMA-co-St) is 1-10 parts by weight, the content of the softening oil is 2-10 parts by weight, the content of the reinforcing filler is 10-20 parts by weight, the content of the vulcanizing agent is 0.1-1 part by weight, the content of the accelerator is 0.1-1 part by weight, the content of the anti-aging agent is 1-4.5 parts by weight, and the content of the light stabilizer is 1-5 parts by weight.
2. The upper surface layer according to claim 1, wherein in the ethylene propylene diene monomer waterproof layer, the softening oil is at least one selected from naphthenic oil, paraffin oil and aromatic oil; and/or
The vulcanizing agent is selected from at least one of sulfur and dicumyl peroxide; and/or
The accelerator is at least one of accelerator DM, accelerator TMTD and accelerator BZ; and/or
The anti-aging agent is selected from at least one of anti-aging agent 4010NA, anti-aging agent 4010 and anti-aging agent RD; and/or
The polypropylene-based elastomer is selected from the group consisting of Riandbasel CA10A, riandbasel CA60A, VERSIFY 2300, dow; and/or
The reinforcing filler is selected from at least one of carbon black, white carbon black and calcium carbonate; and/or
The light stabilizer is at least one selected from the group consisting of a light stabilizer UV-2020, an ultraviolet absorber UV-326 and an ultraviolet absorber UV-531.
3. The upper surface layer according to claim 1 or 2, wherein the TPO-g- (GMA-co-St) is a product prepared by the following method:
s1, mixing raw materials for preparing TPO-g- (GMA-co-St) to obtain a mixture I;
s2, carrying out melt grafting on the mixture I at the temperature of 180-230 ℃ to obtain TPO-g- (GMA-co-St), wherein the melt grafting time is 8-15min;
wherein, the raw materials for preparing TPO-g- (GMA-co-St) comprise: polypropylene-based elastomer, glycidyl methacrylate, styrene, dicumyl peroxide and an antioxidant 1010.
4. The upper surface layer according to claim 3, wherein the glycidyl methacrylate is used in an amount of 1 to 5 parts by weight with respect to 100 parts by weight of the polypropylene-based elastomer in the raw material for preparing TPO-g- (GMA-co-St); the dosage of the styrene is 0.5 to 4 weight parts; the dosage of the dicumyl peroxide is 0.1 to 0.8 weight part; the antioxidant 1010 is used in an amount of 0.1 to 1 part by weight, wherein the polypropylene-based elastomer is the same as the polypropylene-based elastomer described in claim 1 or 2.
5. A double-layer composite ethylene propylene diene monomer waterproof coiled material is characterized by comprising an upper surface layer and a lower surface layer which are sequentially stacked;
the upper surface layer is the upper surface layer of any one of claims 1 to 4, and
the lower surface layer is formed of a thermoplastic polyolefin elastomer waterproof layer, and
the ratio of the thickness of the thinnest part of the upper surface layer to the thickness of the thinnest part of the lower surface layer is 1:1-1.8.
6. A sheet for waterproofing according to claim 5, wherein in the thermoplastic polyolefin elastomer waterproofing layer, the following components are contained: TPO-g- (GMA-co-St), polypropylene-based elastomer, metallocene polyethylene, reinforcing filler, antioxidant, light stabilizer, pigment, wherein in the lower surface layer, the TPO-g- (GMA-co-St) is the same as the TPO-g- (GMA-co-St) in the upper surface layer of any one of claims 1 to 4.
7. The waterproofing membrane according to claim 6, wherein in the thermoplastic polyolefin elastomer waterproofing layer, the TPO-g- (GMA-co-St) is contained in an amount of 1 to 10 parts by weight, the metallocene polyethylene is contained in an amount of 10 to 40 parts by weight, the reinforcing filler is contained in an amount of 10 to 30 parts by weight, the antioxidant is contained in an amount of 0.1 to 1 part by weight, the light stabilizer is contained in an amount of 1 to 5 parts by weight, and the pigment is contained in an amount of 0.5 to 2 parts by weight, with respect to 100 parts by weight of the polypropylene-based elastomer, the reinforcing filler and the light stabilizer being the same as those in claim 1 or 2, respectively.
8. The waterproofing membrane according to any one of claims 5 to 7, wherein in the thermoplastic polyolefin elastomer waterproofing layer, the antioxidant is at least one selected from the group consisting of antioxidant 1010, antioxidant 168, antioxidant 1076; and/or
The pigment is selected from at least one of titanium dioxide, carbon black and a colorant; and/or
The metallocene polyethylene is at least one selected from metallocene high density polyethylene and metallocene low density polyethylene.
9. A method for preparing the double-layer composite ethylene propylene diene monomer waterproof coiled material as claimed in any one of claims 5 to 8, which is carried out by applying the components of the waterproof coiled material as claimed in any one of claims 5 to 8, and comprises the following steps:
(1) Mixing and contacting: mixing ethylene propylene diene monomer, polypropylene-based elastomer, TPO-g- (GMA-co-St), softening oil, filler, anti-aging agent and light stabilizer to contact I to obtain premix 1;
mixing and contacting polypropylene-based elastomer, TPO-g- (GMA-co-St), metallocene polyethylene, a filler, an antioxidant and a pigment II to obtain a premix 2;
(2) And (3) granulation: granulating the premix 1 to obtain a granulated material 1;
(3) Plasticizing and rolling: and extruding and plasticizing the granulating material 1 and the premix 2, and introducing into a three-roll calender for calendering to obtain the double-layer composite ethylene propylene diene monomer waterproof coiled material.
10. The method of claim 9, wherein the mixed contact I at least satisfies: stirring at 300-800r/min at 70-90 deg.C for 5-10min; and/or
Said mixed contact II being at least: under the condition of stirring, the rotating speed is 300-800r/min, the temperature is 70-90 ℃, and the time is 5-10min.
11. The use of the double-layer composite ethylene propylene diene monomer rubber waterproof roll material of claims 5 to 8 in the field of building waterproofing.
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